1 Updating the research on the chemopreventive and therapeutic role of

2 peptide lunasin

3 Running title: Chemopreventive and therapeutic properties of peptide lunasin

4 Chia-Chien Hsieh1, Cristina Martínez-Villaluenga2, Ben O. de Lumen3, Blanca Hernández-

5 Ledesma4*

6

7 1 Department of Human Development and Family Studies (Nutritional Science & Education),

8 National Taiwan Normal University, No. 162, Heping East Road, Section 1, Taipei 10610,

9 Taiwan

10 2 Institute of Food Science, Technology and Nutrition (ICTAN-CSIC), Juan de la Cierva 3,

11 28006 Madrid

12 3 Department of Nutritional Science and Toxicology, University of California at Berkeley,

13 119 Morgan Hall, Berkeley, CA 94720-3104, USA

14 4 Instituto de Investigación en Ciencias de la Alimentación (CIAL, CSIC-UAM, CEI

15 UAM+CSIC). Nicolás Cabrera, 9. 28049 Madrid, Spain

16 17 * Corresponding author: B. Hernández-Ledesma

18 Nicolás Cabrera, 9. 28049 Madrid, Spain

19 Phone: +34 910017970

20 Fax: +34 910017905

21 e-mail: [email protected]

22 1

23 Abstract

24 Chronic diseases have become the medical challenge of the 21st century because of their high

25 incidence and mortality rates. Modulation of diet and lifestyle habits is considered as the best

26 strategy for the prevention of these disorders. Health promoting benefits beyond their

27 nutritional effects have been described for multiple dietary compounds. Among these

28 compounds, peptide lunasin is considered as one of the most promising. Naturally present in

29 , lunasin has been extensively studied in the last two decades because of its potential

30 against chronic diseases, such as , cardiovascular and immunological disorders. The

31 purpose of this article is to summarize the evidence on the presence of lunasin in soybean and

32 derived foods, and its bioavailability once it is orally ingested. The protective and therapeutic

33 effects of this peptide against cancer, oxidative stress, , and high

34 levels as well as the molecular mechanisms of action involved in these effects are also

35 described in this review.

36

37 Keywords: lunasin; bioactive peptide; chemopreventive and therapeutic properties; cancer;

38 chronic diseases

39

2

40 INTRODUCTION

41 Twenty-year history of peptide lunasin

42 Lunasin (from the Tagalog word “lunas” for cure) is a peptide identified in the

43 soybean cotyledon twenty years ago.1 It corresponds to a small subunit peptide encoded

44 within the soybean 2S albumin Gm2S-1 gene that also codes for a methionine-rich protein, a

45 signal peptide, and a linker peptide.2 Early studies carried out with the chimeric gene

46 encoding lunasin and tagged with the green fluorescent protein demonstrated that its

47 transiently transfection into murine embryo fibroblast C3H 10T1/2, hepatoma Hepa1c1c7

48 cells, and human breast cancer MCF-7 cells resulted in cell division arrest causing abnormal

49 spindle fiber elongation, chromosomal fragmentation, and cell lysis.3 These results suggested

50 that the binding of lunasin to chromatin prevented the normal formation of the kinetochore

51 complex in the centromere, thus leading to the disruption of mitosis, and eventually to cell

52 death. According to the first reports, lunasin identified in soybean contains 43 amino acids. Its

53 sequence (SKWQHQQDSCRKQLQGVNLTPCEKHIMEKIQGRGDDDDDDDDD, National

54 Center for Biotechnology Information, NCBI, accession number AAP62458) presents nine

55 aspartic acid (D) residues at the C-terminal end responsible for lunasin’s colocalization with

56 hypoacetylated chromatin through ionic interactions and for inhibition of histone H3

57 acetylation, the 33RGD35 cell adhesion motif responsible for lunasin adhesion and

58 internalization into cells, a predicted helical region (23E-I30) with homology to a conserved

59 region in chromatin-binding proteins, and twenty two residues at N-terminal facilitating the

60 binding to deacetylated N-terminal tail of histone H4.4 A molecular dynamics study was

61 carried out to characterize the exact three-dimensional structure of lunasin.5 It was revealed

62 that this peptide exhibits three separate α-helical bundles in its structure supported by residues

63 5H-C10, 22C-I30 and 35D-D41. Moreover, the last residues present in both N- and C-terminus

64 remain extended or unstructured, and the motif RGD plays a key role of hinge winding and 3

65 unwinding the central and C-terminus helical regions of the peptide. This study suggested that

66 the α-helix associated with aspartic acid (D) residues at C-terminal of lunasin plays a

67 recognition role in its binding with the chromatin residue and, could thus be responsible for its

68 anti-mitotic action in mammalian cell lines. Later on, a structural analysis by circular

69 dichroism at 25°C has concluded that lunasin contains 29% α-helix, 28% β-strands, 23%

70 turns, and 20% unordered.6 More recently, nuclear magnetic resonance and circular dichroism

71 have revealed that lunasin can adopt a reduced form with thiols or an oxidized form with

72 intramolecular disulphide bonds, both containing two helical segments (3W-K12 and 21P-I30)

73 and a single region with and extended β-sheet conformation corresponding to C-terminal

74 poly-D tail.7 Additionally, these authors found that these secondary structures are in

75 equilibrium with unstructured conformations.

76 Although the first studies characterized lunasin as a 43 amino acid peptide, the

77 analysis carried out in the last five years show controversial results. Seber and coworkers

78 purified lunasin from soybean white flake by anion exchange chromatography followed by

79 reversed-phase chromatography.8 The purified ≈14 kDa protein complex containing lunasin

80 was analyzed by electrospray ionization (ESI) mass spectrometry (MS) revealing that the

81 major peptide in this preparation had a monoisotopic mass of 5139.25, which is 114.02 Da

82 higher than the expected mass of 5025.23 Da for the 43 amino-acid form of lunasin described

83 in the literature. The mass difference suggested that the predominant form of purified lunasin

84 from soybean flake contained 44 amino acids with an additional asparagine (N) residue at C-

85 terminal. This fact was confirmed by the analysis of tryptic peptides derived from purified

86 lunasin by liquid chromatography (LC) coupled to tandem MS (LC-MS/MS). Also, a weak

87 signal with a monoisotopic mass 5025.23 Da was observed suggesting that a minor amount of

88 the 43 amino-acid form of lunasin may be present. Similar results have been recently obtained

89 by Serra et al. for lunasin purified from a commercial soybean beverage powder and 4

90 characterized by top-down proteomics.9 In addition to the unmodified 44-amino acids lunasin,

91 these authors found different post-translationally modified proteoforms resulting from diverse

92 degrees of glycation mainly at residue lysine (24K and 29K) as well the occurrence of

93 alternative side chain modifications, including oxidation (M), dihydroxy (K), dehydration

94 (D/N), deamidation (N/Q), methyl esterification (D), carbamylation (K), acetylation (K) and

95 pyro-glutamate conversion (N). All these modifications may have an important repercussion

96 on lunasin’s bioactive effects and its epigenetic regulatory capacity.9

97

98 Presence of lunasin in plants: what is its origin?

99 Since its discovery in soybean, studies have focused on purifying and quantifying

100 lunasin from different soybean varieties, reporting concentration values ranged from 1,100 to

101 14,000 g lunasin/g extracted protein or 500-810 g lunasin/g seed.10,11 The results obtained

102 from these studies demonstrate that the soybean genotype is the main affecting factor on

103 lunasin’s quantity in soybean seeds, indicating the possibility of selecting and breeding

104 varieties of soybean with higher content of this peptide.10 Environmental factors, mainly

105 temperature and soil moisture, have also been reported to affect lunasin’s concentration in

106 soybean seeds, whereas light and dark conditions do not seem to have any effect.12 Other

107 factors such as the stages of seed development and maturation have also a notable influence

108 on lunasin’s content in soybean. Seed maturation resulted in an important increase of this

109 content while sprouting leads to a continuing decrease of lunasin with soaking time.11

110 Germination time and temperature have significant influences on the composition and

111 concentration of nutrients and bioactive compounds such as lunasin in germinated soybean

112 flour from several Brazilian soybean cultivars.13-15

113 Once the biological activity of soybean lunasin was reported for the first time, a

114 number of studies focused on the search of this peptide in other plants. Its presence was 5

115 detected in both cereals and non-cereal plants with variable content. In cereals, this content

116 ranged from 13-99 μg g-1 seed in ,16 200-300 μg g-1 seed in ,17 45-150 μg g-1 seed

117 in ,18 429-6,458 μg g-1 grain in triticale,19 and 34-197 μg g-1 grain in oat.20 The content was

118 reported to be mainly influenced by the genotype.21 These authors found that the broad-sense

119 heritability for the lunasin content in this cereal was 70.4%. Lunasin production is also

120 dependent on the interaction of genotype and organic farming systems. Legzdina et al. found

121 that average amount of lunasin in barley was significantly higher in organically grown plants;

122 however, it is worth noting that some barley genotypes displayed the opposite effect.21 These

123 results provide the idea that it is possible to select genotypes that are appropriate for organic

124 farming and lunasin accumulation such as barley variety Rubiola. Lunasin has also been

125 detected in other plant sources, such as the black nightshade (Solanum nigrum L.)22 and the

126 pseudocereal amaranth (Amaranthus hypochondriacus L.)23 In amaranth, the lunasin peptide

127 is encrypted in a 22 kDa precursor protein, and the primary structure of the native precursor

128 protein differs from that of soybean lunasin.24 The sequence of amaranth lunasin-like peptide

129 (SKWQHQQDSCRKQLQGFKMTATPPCEKHITRAFRRAPIQQRGRGISTRRGDDDDDD-

130 DDD) showed high homology with the soybean peptide.

131 In the last years, studies have brought into question the origin of lunasin and its actual

132 presence in other plants than soybean. Mitchell and coworkers carried out an exhaustive

133 proteomic and transcriptomic analysis of wheat and other cereals, as well as a deeply search

134 in different DNA sequences databases that failed to identify sequences similar to those known

135 to encode peptide lunasin in soybean. 25 Similarly, Dinelly and co-workers, using chemical

136 (LC-MS) and molecular (polymerase chain reaction, PCR) analyses, reported the complete

137 absence of lunasin in the investigated wheat genotypes.26 These findings have been recently

138 supported by Alaswad and Krishman who conducted immunological analysis in cereals and

139 other plant species using polyclonal antibodies specific to the first 20 amino acid N-terminal 6

140 peptide and the 15 amino acid C-terminal peptide of lunasin.27 Results from this study

141 demonstrated that peptides identical to lunasin are absent in the studied plant species.

142 However, other proteins with higher molecular weight were recognized by soybean lunasin

143 antibodies providing the hypothesis that lunasin-like peptides could be released from

144 precursor proteins by the action of proteases from gastrointestinal or microbial origin. This

145 hypothesis is in line with the study of Rizzello and co-workers who investigated the presence

146 of lunasin-like polypeptides in nineteen traditional Italian legumes after sourdough

147 fermentation with Lactobacillus plantarum C48 and Lactobacillus brevis AM7, expressing

148 different peptidases.28 These authors confirmed the absence of lunasin in legume flours

149 although different lunasin-like polypeptides were found in bean and lentil varieties. After

150 lactic acid fermentation, legume sourdoughs showed increased number and intensities of

151 lunasin-like polypeptides, suggesting that endogenous legume proteases and microbial

152 peptidases were responsible for the release of lunasin-like fragments. Rizzello and co-workers

153 have additionally suggested a possible microbial origin for lunasin.29 According to these

154 authors, lunasin might be synthesized and secreted by microorganisms, either as a mature

155 peptide or a precursor which is further processed by a microbial or endogenous plant

156 proteinase. Further studies should be needed to elucidate the real origin of this peptide.

157

158 Lunasin in plant-derived products: extraction, identification, structure diversity and

159 production

160 Lunasin has been quantified in a variety of soybean derived products, foods and

161 beverages by using Western blot and ELISA assays.30,31 The concentration of this peptide in

162 those products is shown in Table 1. These methods require the use of antibodies that only

163 recognize the sequence corresponding to fragment 23EKHIMEKIQGRGDDDDD39, and thus,

164 they can suffer from cross-reactivity. Therefore, two dimensional analytical methods have 7

165 been applied combining an isoelectrofocusing separation with LC-MS and a time-of-flight

166 (TOF) analyzer for the selective and sensitive determination of lunasin in soybean-derived

167 products, such as textured soybean and soybean flour (Table 1).32 Recently, top-down

168 proteomic strategy was used to identify and characterize novel proteoforms of lunasin in

169 commercial soybean food products derived from food processing and natural chemical

170 reactions.9 Four different lunasin derived advanced glycation end products containing mainly

171 Nε-carboxy-methyl-lysine and Nε-carboxy-ethyl-lysine at 24K and 29K were detected.

172 In addition to the natural presence of lunasin in plant derived-foods, some processing

173 methodologies have been demonstrated to augment its concentration. Rizzello and others

174 revealed the potential role of microbial proteolytic system for increasing the lunasin

175 concentration in food matrices by sourdough fermentation.29 This study suggests new

176 alternatives of cost effective bio-production of lunasin over chemical synthesis as well as new

177 developments of functional fermented products containing this peptide.

178 In spite of the different beneficial properties that have been demonstrated for lunasin,

179 production of this peptide for commercial or research applications is very costly. In the last

180 years, efforts have been made to obtain lunasin in a higher concentrated or purified form.

181 Cavazos and others developed a method resulting in >90% purity of lunasin from defatted soy

182 flour.31 Simultaneously, Seber and others applied more advanced techniques, namely, anion-

183 exchange chromatography, ultrafiltration, and reversed-phase chromatography to purify

184 lunasin, resulting in >99% purity of lunasin from defatted soy flour.8 A recent work has been

185 published reporting the development of a novel method involving extraction of soybean flour

186 with 30% ethanol followed by preferential precipitation of lunasin and protease inhibitors by

187 calcium.33 This simple procedure yielded 3.2 g of lunasin-protease inhibitor concentrate from

188 100 g of soybean flour, and the entire isolation procedure was completed in less than 2 h. The

189 concentrate obtained by this methodology was demonstrated to be active suppressing 8

190 lipopolysaccharide (LPS)-stimulated cytokine expression, thus it might be considered a

191 promising starting material for further lunasin purification. Another efficient and cheap

192 alternative to plant peptide-purification or chemical synthesis is recombinant production of

193 lunasin by transgenic organisms.34 The obtained yield of recombinant production was 75 mg/l

194 and 210 mg/l in Escherichia coli and Clostridium thermocellum, respectively.34,35 Lunasin

195 was successfully expressed as recombinant his-tagged gene in E. coli and was found to have

196 identically biological activity than that demonstrated for synthetic lunasin.36 Recently, a

197 patent has been granted to prepare lunasin from plants through expressing a fusion protein

198 comprising lunasin and cleaving it from given protein.37

199 Lunasin is currently commercialized as a dietary supplement with different health

200 claims.38 LunasSoyTM (protein complex) and LunasinXP® (peptide extract) are two powder

201 supplements (Soy Labs®, LLC, USA) with beneficial properties on heart and skin health,

202 immunomodulatory, anti-inflammatory and anti-aging effects. A drink mix

203 (Carefast FSP100, Carefast Products, Inc.) enriched with LunasinXP® has been developed. As

204 indicated by the manufacturer, this beverage delivers 13 g of heart-healthy soy protein and 30

205 mg of soy isoflavones per serving. LunaRich® is a product commercialized by Reliv

206 International (USA) that provides (in one 125 mg capsule) the same quantity of lunasin found

207 in 25 g of high-quality soy protein, the daily amount identified by the Food and Drug

208 Administration (FDA) to help reduce the risk of heart disease. LunaSmartTM Blend

209 (LunaSmart, USA) is also a capsule supplement that contains 600 ng of lunasin by serving

210 (two capsules). Recently, a new product has been launched by Simplesa® (USA), known as

211 LunaCellTM and defined as a new generation of lunasin products because of the effective and

212 potent combination of this peptide and protease inhibitors, which together deliver bioavailable

213 lunasin to the body.

214 9

215 BIOAVAILABILITY OF LUNASIN

216 One of the most important characteristics of any food-derived compound with

217 demonstrated biological properties is its ability to remain intact and bioactive after absorption,

218 distribution and metabolism, termed as bioavailability. This term refers to the portion of the

219 ingested compound that reaches circulation. In vitro bioavailability studies have reported that

220 isolated lunasin, either synthetic or soybean-purified, is easily digested after 2 minutes

221 incubation with simulated gastric or intestinal fluids.39 However, lunasin survives, at least

222 partially, the attack of digestive enzymes when is present in crude protein extracts purified

223 from soybean, remaining 60% and 80% of initial lunasin after proteolysis by pepsin and

224 pancreatin for 120 min, respectively.39 Results from these studies suggested the protective

225 role that naturally-occurring protease inhibitors, such as Bowman-Birk inhibitor (BBI) or

226 Kunitz-trypsin inhibitor might exert against lunasin’s proteolysis by digestive enzymes.

227 Hernández-Ledesma et al. observed the protection exerted by BBI when lunasin present in

228 soybean-derived foods was subjected to a sequential digestion with pepsin and pancreatin,

229 suggesting the importance of the lunasin:BBI ratio on this protection.30 This hypothesis has

230 been confirmed by Cruz-Huerta and co-workers that described the protective effect of the

231 major isoinhibitor of the Bowman-Birk family (IBB1) on the in vitro digestion of synthetic

232 lunasin simulating physiological conditions.40 In absence of IBB1, lunasin is completely

233 hydrolyzed by the action of digestive enzymes whereas partial hydrolysis of lunasin is

234 observed when the isoinhibitor is present. Peptides released from lunasin during simulated

235 digestive process have been recently identified.41 These authors also studied the

236 bioavailability of lunasin and released fragments by using Caco-2 cell monolayers, indicating

237 that both lunasin and fragment 11RKQLQGVN18 were absorbed intact across the intestinal

238 epithelium through a mechanism involving paracellular passive diffusion. The role of Kunitz-

10

239 trypsin inhibitor on the stability of lunasin present in soybean products against pepsin-

240 pancreatin hydrolysis has also been recently demonstrated.42

241 In vivo bioavailability studies carried out in animals and humans have confirmed

242 above in vitro findings. Hsieh et al. demonstrated that lunasin was bioavailable when orally

243 ingested by mice and rats.43 Synthetic 3H-labeled lunasin was absorbed in CD-1 mice and

244 distributed in various tissues including lung, mammary gland, prostate, and brain. In addition,

245 these authors also reported that lunasin extracted from the blood and liver of lunasin-enriched

246 soy flour-fed rats was able to suppress foci formation as effectively as equimolar amount of

247 synthetic lunasin. A previous study had also found an intact and active form of this peptide in

248 blood and liver of rats fed soybean lunasin-enriched diets.44 Interestingly, detection of lunasin

249 in plasma of healthy male volunteers after consumption of soy protein has been reported.45 In

250 these studies, subjects were fed 50 g of soy protein for 5 days after a one-week washout

251 period. Thirty and sixty minutes after soy protein ingestion, blood samples were collected and

252 analyzed for lunasin that appeared at concentrations between 50.2 and 110.6 ng ml-1 of

253 plasma. This amount represents 4.5% absorption of lunasin from 50 g of soy protein.

254 Recently, a method for the direct isolation and quantification of lunasin from plasma using an

255 ion-exchange microspin column and a validated immunoassay protocol has been optimized.6

256 The promising bioavailability results as well as the development of new technologies to detect

257 and quantify lunasin content in human samples are important in supporting clinical trials

258 confirming the chemoprevention evidence for this peptide by cell culture and animal studies.

259

260 CANCER CHEMOPREVENTIVE AND THERAPEUTIC PROPERTIES OF

261 LUNASIN

262 The promising chemopreventive properties of peptide lunasin have been demonstrated

263 in both cell culture experiments and animal models. Cell culture has demonstrated that while 11

264 lunasin’s treatment does affect neither normal cells proliferation nor morphology, it is capable

265 to prevent mammalian cells transformation induced by chemical carcinogens, viral oncogene

266 E1A, and ras-oncogene.46-48 Thus, a significant reduction of foci formation induced by

267 chemical carcinogens 7,12-dimethylbenz[a]-anthracene (DMBA) and 3-methylcholanthrene

268 (MCA) in mouse C3H 10T1/2 cells was reported after lunasin treatment.46 This peptide was

269 also able to increase p21 protein level, and to suppress foci formation in NIH/3T3 cells stably

270 transfected cells with the viral oncogene E1A and ras-oncogene.47,48 Differences between the

271 effect of lunasin in non-tumorigenic and tumorigenic cell lines have also been described.

272 Galvez et al. confirmed the selective capacity of this peptide to act on tumorigenic prostate

273 RWPE-1 cancer cells without affecting non-tumorigenic RWPE-2 prostate epithelial cells.49

274 The study also demonstrated that HIF1A, PRKAR1A, TOB1, and THBS1 genes expression

275 was up-regulated by lunasin in RWPE-1 cells, but not in RWPE-2 cells. In addition, a recent

276 study has reported that treatment of highly purified soybean-derived lunasin caused inhibition

277 of cell-line specific proliferation on anchorage-dependent growth of non-small lung cancer

278 cells, whereas it did not exert any effect on two normal bronchial epithelial cell lines.50

279

280 Lunasin modulates cell growth and apoptosis

281 Disruption of the normal regulation of cell cycle progression and division are

282 important events in the development of cancer. Therefore, inhibition of deregulated cell cycle

283 progress in cancer cells is being considered an effective strategy to delay or halt tumor

284 growth. Cell cycle is highly regulated by internal checkpoints molecules, such as the protein

285 kinases cyclin-dependent complexes (CDKs) after binding to their related cyclin regulatory

286 subunits.51 A significant arrest of breast cancer MDA-MB-231 cell cycle was observed when

287 these cells were treated with lunasin. This effect was accompanied of a decrease in the

288 expression of CDC25A, caspase-8, Ets2, Myc, Erbb2, PIK3R1 and Jun genes52,53 as well as in 12

289 the protein levels of cyclin D1, D3, CDK4 and CDK6.54 The increase of retinoblastoma (Rb)

290 gene expression and the inhibition of Rb phosphorylation might also contribute to the breast

291 cancer cell cycle arresting effect.17,52 Recently, lunasin has been shown to inhibit cell cycle

292 progression at the G1/S phase through alteration of the expression of CDK complex

293 components cyclin D1, CDK4, and CDK6, increase of p27Kip1 levels, reduction of Akt

294 phosphorylation, and inhibition of Rb phosphorylation in non-small lung cancer cells.50 These

295 authors showed that the in vitro effects of lunasin on this type of cells was significantly higher

296 in anchorage-independent assays and correlate significantly with its in vivo effects in a non-

297 small lung cancer cells mouse xenograft model. Inaba and coworkers compared the effects of

298 lunasin treatment on lunasin-sensitive (H661) and lunasin-insensitive (H1299) non-small cell

299 lung cancer cells with respect to lunasin uptake, histone acetylation and integrin signaling.55

300 These authors reported changes in histone acetylation in both cell lines, with H661 cells

301 showing a unique increase in H4K16 acetylation. Moreover, they demonstrated that the

302 lunasin´s ability to block the G1/S phase transition in H661 cells was also due to its ability to

303 bind αv-containing integrins (αvβ3 and αvβ1), and consequently act as an integrin signaling

304 antagonist.55 Integrins are heterodimeric cell-surface proteins involved in cell adhesion to

305 extracellular matrix and cell signaling that affect cell migration, survival and proliferation.

306 Therefore, the dual mechanism of action demonstrated for lunasin on non-small cell lung

307 cancer cells may be responsible for the potential therapeutic effects attributed to this peptide.

308 In colon cancer cells, lunasin caused a cell cycle arrest at G2/M phase and a

309 mitochondrial-mediated apoptosis induction accompanied of an increase of p21 protein

310 expression in HT-29 cells, and an increase of both p21 and p27 proteins in KM12L4 cells.56,57

311 In addition, lunasin’s treatment to KM12L4 cells affected the Bax:Bcl-2 ratio by up-

312 regulating anti-apoptotic Bax protein and down-regulating pro-apoptotic Bcl-2 protein,

313 resulting in the cytochrome c release involved in the mitochondrial-dependent apoptosis 13

314 pathway.56 Lunasin has also been demonstrated to exert cytotoxic effect against L12120

315 leukemia cells through arresting cell cycle at G2/M phase and inducing apoptosis.58 These

316 authors found that the increase of apoptotic cell number was due to the augment of caspases -

317 3, -8 and -9 expression. In human MCF-7 breast cancer cells, treatment of lunasin induced

318 tumor suppressor phosphatase and tensin homolog (PTEN)-mediated apoptosis after

319 increasing the expression of this protein and enhancing its nuclear localization.59 Moreover,

320 lunasin can act as co-adjuvant in breast cancer chemoprevention strategies because of the

321 synergistic effects were observed on cell cycle arrest and apoptosis induction, when combined

322 with natural and synthetic compounds, such as anacardic acid and aspirin, respectively.52,53,60

323 The angiogenesis and metastasis abilities of cancer cells are often associated to

324 deregulation and degradation of the extracellular matrix, and alteration in the integrin

325 receptors.61,62 These receptors can recognize peptides with RGD-motif in their sequences that

326 bind integrins to block their signaling pathways.63 The presence of this motif within lunasin’s

327 sequence could be responsible for its cell growth suppressive effects. Preliminary results in

328 colon cancer KM12L4 cells have demonstrated that lunasin’s treatment modulates the

329 expression of 62 genes involved in cell adhesion and extracellular matrix.57 In addition,

330 decreases in gene expression of collagen type VII α1, integrin β2, matrix metalloproteinase

331 10, selectin E and integrin α5, and increases in collagen type XIV α1 genes expression were

332 observed in lunasin-treated colon cancer cells compared with untreated cells.64 Similar effects

333 have been reported in breast cancer cells lines in which lunasin treatment suppresses cell

334 migration and invasion by inhibiting matrix metalloproteinases.65 Moreover, this anti-

335 metastasis property of lunasin has also been demonstrated to modestly inhibit the

336 angiogenesis-mediator vascular endothelial growth factor (VEGF) in 4T1 breast cancer cell.66

337 These results suggested the ability of lunasin to act as an anti-metastatic agent contributing on

338 its chemopreventive effects. 14

339 Increasing evidence confirms that colorectal cancer (CRC) could be initiated due to

340 metabolic dysregulation. Several studies pointed out an association between colonic cell

341 proliferation and insulin secretion,67,68 which led to other investigations on the potential role

342 of the antidiabetic drug metmorfin as an anticancer agent in both diabetic and non diabetic

343 patients, and animal models.69-71 Results from these studies showed positive effects of

344 metmorfin on CRC incidence, colon epithelial cell proliferation and number of aberrant foci.

345 A recent study showed that lunasin enhances drug efficacy of metmorfin in an in vitro model

346 of aggressive colon cancer (HCT116) in a hyperinsulinemic environment.72 Molecular

347 mechanisms for these effects include down-regulation of the tumor suppressor PTEN and the

348 lipid biosynthesis-associated enzyme fatty acid synthase (FASN), further blocking the self-

349 renewal and expansion of colon-like stem cells epithelial subpopulations. These findings

350 suggest the potential value of lunasin inhibiting CRC progression and conceivably, metastasis

351 and recurrence.

352 Melanoma is a type of skin cancer which major cause of morbidity and mortality is

353 associated with recurrence of this disease. It is initiated and maintained by a small population

354 of malignant cells called cancer-initiating cells that exhibit stem-cell-like properties and are

355 resistant to and radiation, suggesting their implication in invasion, metastasis,

356 and ultimately relapse.73 A recent study has demonstrated that treatment with lunasin reduced

357 the size of a subpopulation of melanoma cells expressing aldehyde dehydrogenase, a cancer-

358 initiating cells marker, associated with a reduction in the capacity to form colonies in soft agar

359 assays.74 Moreover, the mechanistic model revealed that lunasin, added to isolated melanoma

360 cancer-initiating cells, induced expression of the melanocyte-associated differentiation

361 markers tyrosinase and microphthalmia-associated transcription factor concomitant with

362 reduced expression of the stem-cell-associated marker NANOG. A subsequent study of these

363 authors demonstrated robust antimetastatic properties of lunasin through alterating histone 15

364 acetylation patterns and modulating integrin signaling through FAK and PI3K/AKT

365 pathways.75 Lunasin is shown as a complex and multifaceted peptide with potential

366 therapeutic efficacy against malignant diseases in which recurrence resulting from cancer-

367 initiating cells is expected.

368

369 Lunasin exerts an epigenetic mechanism of action

370 Epigenetic changes (i.e., variation in phenotype or patterns of gene expression without

371 a change in the underlying DNA sequence) are crucial for the regulation and expression of

372 genes involved in the normal growth and development, and in the maintenance of cellular

373 function, but also, they play a key role in cancer initiation and development.76 Three distinct

374 mechanisms are well known to regulate the epigenome: DNA methylation, histone

375 modifications, and small-interfering RNAs. Although a number of histone modifications

376 certainly play important roles in epigenetic regulation, the acetylation has been clinically

377 associated with pathological epigenetic disruptions in cancer cells.77 In addition to its ability

378 to neutralize the charge of histones altering the chromatin structure and accessibility, histone

379 acetylation of lysine residues is a mechanism associated with binding of various

380 transcriptional activators and repressors.78 Under steady-state conditions, the core H3 and H4

381 histones are mostly in a deacetylated (repressed) state. Evidence has shown that after treating

382 mammalian cells with lunasin and histone deacetylation inhibitor sodium butyrate, lunasin

383 translocates to cellular nucleus and tightly binds to deacetylate core histones inhibiting

384 histone acetylation, which is perceived by the cell as an abnormal cell growth, resulting in

385 programmed cell death.46,48,79 Lunasin either synthetic,46,54 or extracted from natural seeds

386 16,17,24,44 has been shown to inhibit core histone H3 and H4 acetylation seeds. Moreover,

387 lunasin has demonstrated to compete with different histone acetyltransferases (HATs), such as

388 yGCN5 and PCAF, inhibiting the acetylation and repressing the cell cycle progression.44 On 16

389 the basis of these findings, lunasin has been suggested as the first natural peptide with an

390 epigenetic mechanism of action, although further studies should be carried out to completely

391 elucidate the nature of this mechanism.

392

393 In vivo cancer preventive properties of lunasin peptide

394 The promising chemopreventive role of lunasin has also been demonstrated in several

395 animal models. The first model using SENCAR mice showed that topical administration of

396 this peptide reduced chemical carcinogen-induced skin carcinoma incidence and delayed the

397 tumor development. A posterior carcinogen-induced mouse model also reported lunasin’s

398 ability to delay the appearance of papilloma by slowing epidermal cell proliferation.80 Studies

399 carried out in the last years have revealed that lunasin also exerts chemopreventive effects

400 against other types of cancer, such as breast, colon, and lung . This peptide was found

401 to reduce the generation and incidence of chemical-induced mammary tumors in SENCAR

402 mice fed lunasin-enriched diet.81 A similar preventive effect was demonstrated in a chemical-

403 induced mammary tumor rat model after administration of an isoflavone-deprived soy peptide,

404 although the specific contribution of lunasin to the observed effects has not clarified yet.82

405 Intraperitoneal administration of lunasin has also been found to reduce tumor incidence,

406 generation and weight in a xenograft breast cancer MDA-MB-231 mouse model.43 The

407 analysis of histological tumor sections carried out by these authors also revealed the

408 capability of the peptide to inhibit cell proliferation through reducing Ki-67 biomarker, and

409 inducing cell death. Similarly, a decrease of proliferation cell nuclear antigen (PCNA) levels

410 in liver tumor and an increase of Bax:Bcl-2 ratio was observed after intraperitoneal

411 administration of lunasin to colorectal KM12L4 metastasis mice.57 These authors also showed

412 that oral administration of lunasin could significantly reduce the incidence of liver metastasis

413 in this animal model; however, no effects on PCNA levels were found.83 These discrepancies 17

414 suggest that the route of lunasin’s administration can be determinant on its chemopreventive

415 activity, thus further studies determining the route and optimal dose should be performed in

416 order to achieve the best effects.

417 A recent study has been reported the tumor growth and size reducing properties of

418 lunasin after its intraperitoneal administration to the xenograft lung cancer H1299 mice when

419 compared to untreated animals.50 In a melanoma xenograft mouse model, it has been shown

420 that the in vivo tumor growth initiated by the cancer-initiating cells population was

421 significantly impaired by treatment with lunasin.74 Also, when C57Bl/6 mice were subjected

422 to an experimental metastasis model of melanoma using B16-F10 cells, lunasin significantly

423 suppressed the ability of these cells to invade and proliferate in the lungs.75 Since several mice

424 in the lunasin-treated group did not display any macrometastasis sign, the authors suggested

425 the efficacy of lunasin to reduce or abolish metastatic burden. The lunasin’s ability to inhibit

426 subcutaneous tumor growth of murine models of melanoma and non-small cell lung cancer

427 has been also demonstrated.84

428

429 OTHER BIOACTIVITIES OF LUNASIN

430 In the past several years, accumulating evidence has shown that lunasin not only exerts

431 chemopreventive properties but also acts modulating inflammation and oxidative stress,

432 cardiovascular, central nervous, and immune systems (Figure 1). The detailed information of

433 these lunasin’s effects was described below in this section.

434

435 Antioxidant and anti-inflammatory activities

436 A growing body of evidence has revealed that chronic inflammation and/or oxidative

437 stress are involved in the development of cancer as well as different degenerative disorders,

438 including cardiovascular and neurodegenerative diseases.85,86 Therefore, antioxidant and anti- 18

439 inflammatory compounds are being considered as promising candidates to exert

440 chemopreventive effects against cancer and a number of diseases. Lunasin has demonstrated

441 to exert in vitro antioxidant activity through different mechanisms, including free radical and

442 iron scavenging capacity.87

443 Lunasin extracted from Solanum nigrum L. was showed to chelate ferrous ions, and

444 protect DNA from oxidative damage via blocking fenton reaction to suppress hydroxyl radical

445 generation.88 At cellular level, lunasin acts as a free radical scavenger and inhibitor of reactive

446 oxygen species production in murine RAW264.7 macrophages stimulated with LPS, and

447 intestinal epithelial Caco-2 cells challenged by chemicals hydrogen peroxide and tert-

448 butylhydroperoxide.87,89 Recently, the ability of lunasin to protect human liver HepG2 cells

449 from oxidative stress stimulated by tert-butylhydroperoxide through modulation of associated

450 biomarkers has been reported.90 Oxidative damage in the eye lens has been reported as a

451 major mechanism in the initiation and development of cataracts. Interestingly, Dai et al.

452 demonstrated that lunasin administration markedly inhibited the progression of d-galactose-

453 induced cataract in rats.91 The mechanisms of action responsible for lunasin´s protection from

454 lipid peroxidation were mediated through up-regulation of antioxidant enzymes and inhibition

455 of the activation of polyol pathway by decreasing aldose reductase activity.

456 Lunasin has also been demonstrated to exert anti-inflammatory properties. In LPS-

457 induced RAW264.7 cells, lunasin inhibited secretion of pro-inflammatory mediators

85 458 interleukine (IL)-6, tumor necrosis factor (TNF)-α, and prostaglandin E2 (PGE2). Moreover,

459 inflammation-associated genes expression profile was affected by this peptide in LPS-treated

460 RAW264.7 cells.92 The possible mechanisms of these effects could involve the modulation of

461 cyclooxygenase-2 (COX-2), inducible nitric oxide synthase (iNOS), and nuclear factor (NF)-

462 κB pathways.93,94 Lunasin presents in natural quinoa has also been found to inhibit the

463 secretion of nitric oxide, TNF-α and IL-6 in RAW264.7 cells activated by LPS.95 Recently, it 19

464 has been revealed that lunasin acts as a potential anti-inflammatory agent not only in

465 macrophages but also in adipocytes, disrupting the crosstalk between these two cells,

466 suggested that auxiliary prevention or therapy in obesity-related inflammatory applications.96

467 Moreover, lunasin’s anti-inflammatory activity possibly benefits its chempreventive activity

468 in 4T1 breast cancer cell cultured in the condition of inflammatory adipocyte.66

469 The inhibition of NF-κB-dependent inflammatory mediators through down-regulation

470 of Akt phosphorylation and p65 protein expression was observed after treating human LPS-

471 challenged THP-1 macrophages with lunasin.97 Peptide interacted with αVβ3 integrin receptor

472 being internalized by cells where it exerts its anti-inflammatory effects.

473

474 Effects of lunasin on cardiovascular system

475 Cardiovascular disease is one of the most serious public health problems worldwide.

476 Daily consumption of 25 g of soy protein was approved by the Food and Drug Administration

477 as a health claim to reduce the risk of this disease.98 Lunasin, as one of the components of soy

478 protein, could contribute on this preventive effect due to its demonstrated activity decreasing

479 the biosynthesis of hepatic cholesterol in HepG2 cells by inhibiting 3-hydroxy-3-methyl-

480 glutaryl (HMG) CoA reductase gene expression, and augmenting cholesterol clearance by

481 increasing the low density lipoprotein (LDL) receptor levels.99,100 This hypocholesterolemic

482 effect was confirmed in LDL-receptor mutant pigs, whose LDL cholesterol levels decreased

483 after supplementation of their casein diets with lunasin-enriched soy extract.99 A posterior

484 study carried out with the same pig model has exposed that administration of a lunasin-

485 enriched food supplement in combination with a lunasin-enriched soy extract reduced free

486 fatty acid by increasing leptin and adiponectin levels in the plasma of the animals.100 A human

487 trial was designed to evaluate the effects of the previously reported supplement on blood

488 cholesterol, LDL, triglycerides and uric acid levels, revealing an important decrease after 60 20

489 days consumption of the supplement.101 Interestingly, these reducing effects were greater

490 among the diabetic and overweight individuals, suggesting lunasin´s ability for the control of

491 cardiovascular diseases associated with adjustment lipid imbalances.

492 Recently, in a nonalcoholic steatohepatitis model, C57BL/6 mice were fed a high fat

493 diet and CardioAid and lunasin was orally administered for 25 weeks. The serum of mice was

494 analyzed, the population of CD4+CD25+ lymphocytes and transforming growth factor beta

495 secretion were showed a significant increased, and the IL1- production was decreased.102 It

496 indicated that dietary treatment associated with blunting the liver damage resulting to improve

497 the histological nonalcoholic fatty liver disease activity score. Moreover, the biological

498 markers like serum triglyceride and glucose levels were observed in mice fed lunasin,

499 showing that lunasin exerts protective properties in mice fed the high fat diet.102 In addition,

500 the antioxidant and anti-inflammatory properties of lunasin could contribute on its potential

501 protective role against cardiovascular disorders. Specifically, lunasin has been shown to

502 interact with endocytosis pathways in human macrophages THP-1 which are associated with

503 integrin signaling, clathrin-coated vesicles and macropinosomes,103 thus contributing to the

504 control of cardiovascular disease.

505

506 Effects of lunasin on central nervous system

507 In animal studies, it was shown that lunasin, once orally ingested, is absorbed and

508 distributed through various tissues, included the brain after crossing blood-brain barrier.43,45

509 The central (motionless/neuroleptic/cataleptic) effects of this peptide have been recently

510 assessed by Dzirkale et al. that found local intracisternal administration of synthetic lunasin

511 into male C57BL/6 mice to cause a marked neuroleptic/cataleptic effect even at small doses

512 (0.1 nmol/mouse). Lunasin decreased the hyperlocomotor activity of amphetamine (a

513 dopamine releaser), and slightly affected apomorphine (a dopamine receptor agonist)-induced 21

514 climbing behavior.104 In contrast, lunasin did not affect ketamine (a N-methyl-D-Aspartate

515 (NMDA) receptor agonist) and bicuculline (an antagonist of GABAA receptor)-induced

516 effects. These findings confirmed that glutamate and GABAergic systems did not play an

517 essential role in lunasin’s central effects while affinity of this peptide for dopamine D1

518 receptors could have an important contribution. Further studies aimed to confirming this

519 hypothesis should be needed because there is a necessity for novel types of antipsychotic

520 drugs without serious side-effects.

521

522 Effects of lunasin on the immune system

523 Cytokine immunotherapy is a recent therapeutic strategy used to control the immune

524 surveillance to eliminate cancer cells, and to regulate imbalance immune responses. A recent

525 work has reported, by the first time, the immunomodulatory properties of peptide lunasin.105

526 These authors demonstrated robust synergistic effects of lunasin, and cytokines IL-2 and IL-

527 12 combination on increasing IFN-γ production and granzyme B expression by natural killer

528 cells in post-transplant lymphoma patients who are immune compromised. A simultaneous

529 study carried out with human dendritic cells showed that lunasin-treated cells not only

530 expressed elevated levels of co-stimulatory molecules CD86 and CD49, but also exhibited up-

531 regulation of IL-1, IL-6, and chemokines CCL3 and CCL4.106 Using a prophylactic mouse

532 model, these authors also demonstrated the adjuvant activity of lunasin when mixed with a

533 soluble antigen (ovalbumin) to protect animals against subsequent challenge. Therefore, the

534 results of the study suggest the promising application of lunasin as vaccine adjuvant inducing

535 dendritic cells maturation, which in turn improves the development of protective immune

536 responses to the vaccine antigens.

537 Rheumatoid arthritis is characterized by inflammatory changes of synovial tissues and

538 the formation of rheumatoid pannus. The first study carried out with synovial fibroblasts from 22

539 rheumatoid arthritis patients suggests the promising role of lunasin. After cells treatment with

540 this peptide, a significant decrease of IL-6, IL-8, and matrix metalloproteinase-3 productions

541 were observed, causing suppression of NF-B activation.107

542 Asthma is other immune hypersensitive disease associated with dysregulated T helper

543 type-II immunity leading to chronic eosinophilic inflammation in the airways. A recent study

544 conducted with an ovalbumin plus intranasal LPS-induced mouse model found that

545 intraperitoneal injection of peptide lunasin effectively suppressed allergic airway

546 inflammation through reduction of total cells, especially eosinophils, in bronchoalveolar

547 lavage fluid, and IL-4 secretion from mediastinal lymph nodes.108 In addition, an important

548 decrease of inflammatory Fizz1 gene expression and increase of regulatory T cells

549 accumulation were observed in the lunasin-treated mice group. All these recent findings

550 suggest an immunomodulatory role for lunasin through multiple mechanisms of action

551 making it as a promising agent to be potentially used in therapy of hypersensitive immune

552 disorders or as an adjuvant to enhance vaccination response. Human trials are needed to

553 confirm these effects to have an effective and safe application.

554

555 CONCLUDING REMARKS

556 After nineteen years from its discovery in soybean, lunasin has become one of the

557 most studied plant peptides because of its beneficial properties against chronic diseases. Cell

558 culture and animal models have demonstrated the chemopreventive role of lunasin against

559 skin, breast, colorectal cancers and lymphoma. In addition, studies carried out in the last years

560 have suggested a promising effect of this peptide against hypercholesterolemia, obesity,

561 metabolic syndrome and associated-cardiovascular diseases as well as protective effects in

562 inflammatory and immune regulated-diseases. Findings obtained from bioavailability and

563 bioactivity studies support the inclusion of lunasin-containing food products in the human diet. 23

564 However, clinical trials confirming the already evidential properties are limited. Genomics,

565 proteomics, epigenetics and metabolomics tools should be used as new disciplines to

566 elucidate the complete mechanism of action of this peptide. Other aspects, such as the search

567 of new lunasin’s sources, the optimization of techniques to enrich products with this peptide,

568 study of lunasin’s interactions with other food constituents affecting its activity and

569 bioavailability should be also designed to increase the value of this peptide and its preventive

570 and therapeutic potential against cancer, cardiovascular and immunological diseases.

571

572 Conflict of Interest

573 B.O. de Lumen is one of the co-inventors of patent on lunasin owned by the

574 University of California, Berkeley, and owner of the company Narra Biosciences that is

575 currently developing lunasin-based products.

576

577 Acknowledgements

578 C.-C. H. acknowledges funding from Ministry of Science and Technology, Taiwan

579 (MOST 103-2320-B-003-003-MY3). C. M.-V. and B. H.-L. acknowledge funding from

580 Ministry of Economy and Competitiveness (MINECO, Spain) (grants AGL2013-43247-R and

581 AGL2015-66886-R).

582

583

584

585

24

586 REFERENCES

587 1. Galvez AF, Revilleza MJR and de Lumen BO, A nove1 methionine-rich protein from

588 soybean cotyledon: cloning and characterization of cDNA (Accession No. AF005030).

589 Plant Physiol 114:1567-1597 (1997).

590 2. Odani S, Koide T and Ono T, Amino acid sequence of a soybean (Glycine max) seed

591 polypeptide having a poly(L-aspartic acid) structure. J Biol Chem 262:10502-10505

592 (1987).

593 3. Galvez AF and de Lumen BO, A soybean cDNA encoding a chromatin-binding peptide

594 inhibits mitosis of mammalian cells. Nat Biotechnol 17:495-500 (1999).

595 4. Hernández-Ledesma B, Hsieh CC and de Lumen BO, Lunasin, a novel seed peptide for

596 cancer prevention. Peptides 30:426-430 (2009)

597 5. Singh P and Bisetty K, A molecular dynamics study of lunasin. South Afric J Chem

598 65:115-124 (2012).

599 6. Dia VP, Frankland-Searby S, Laso del Hierro F, Garcia G and de Mejia EG, Structural

600 property of soybean lunasin and development of a method to quantify lunasin in plasma

601 using an optimized immunoassay protocol. Food Chem 138:334-341 (2013).

602 7. Aleksis R, Jaudzems K, Muceniece R and Liepinsh E, Lunasin is a redox sensitive

603 intrinsically disordered peptide with two transiently populated α-helical regions. Peptides

604 85:56-62 (2016).

605 8. Seber LE, Barnett BW, McConnell EJ, Hume SD, Cai J, Boles K, et al., Scalable

606 purification and characterization of the anticancer lunasin peptide from soybean. PLoS

607 ONE 7:e35409 (2012).

608 9. Serra A, Gallart-Palau X, See-Toh RSE, Hemu X, Tam JP and Sze SK, Commercial

609 processed soy-based food product contains glycated and glycoxidated lunasin proteoforms.

610 Sci Rep 6:1-11 (2016). 25

611 10. de Mejia EG, Vasconez M, de Lumen BO and Nelson R, Lunasin concentration in

612 different soybean genotypes, commercial soy protein, and isoflavone products. J Agric

613 Food Chem 52:5882-5887 (2004).

614 11. Park JH, Jeong HJ and de Lumen BO, Contents and bioactivities of lunasin, Bowman-

615 Birk inhibitor, and isoflavones in soybean seed. J Agric Food Chem 53:7686-7690 (2005).

616 12. Wang WY, Dia VP, Vasconez M, de Mejia EG and Nelson RL, Analysis of soybean

617 protein-derived peptides and the effect of cultivar, environmental conditions, and

618 processing on lunasin concentration in soybean and soy products. J AOAC Int 91:936-946

619 (2008).

620 13. Paucar-Menacho LM, Berhow MA, Mandarino JMG, de Mejia EG and Chang YK,

621 Optimisation of germination time and temperature on the concentration of bioactive

622 compounds in Brazilian soybean cultivar BRS 133 using response surface methodology.

623 Food Chem 119:636-642 (2010).

624 14. Paucar-Menacho LM, Berhow MA, Mandarino JMG, Chang YK and de Mejia EG, Effect

625 of time and temperature on bioactive compounds in germinated Brazilian soybean cultivar

626 BRS 258. Food Res Int 43:1856-1865 (2010).

627 15. Paucar-Menacho LM, Amaya-Farfan J, Berhow MA, Mandarino JMG, de Mejia EG and

628 Chang YK, A high-protein soybean cultivar contains lower isoflavones and saponins but

629 higher minerals and bioactive peptides than a low-protein cultivar. Food Chem 120:15-21

630 (2010).

631 16. Jeong HJ, Lam Y and de Lumen BO, Barley lunasin suppresses ras-induced colony

632 formation and inhibits core histone acetylation in mammalian cells. J Agric Food Chem

633 50:791-794 (2002).

634 17. Jeong H, Jeong JB, Kim DS, Park JH, Lee JB, Kweon DH, et al., The cancer preventive

635 lunasin from wheat inhibits core histone acetylation. Cancer Lett 255:42-48 (2007). 26

636 18. Jeong HJ, Lee JR, Jeong JB, Park JH, Cheong YK and de Lumen BO, The cancer

637 preventive seed peptide lunasin from rye is bioavailable and bioactive. Nutr Cancer

638 61:680-686 (2009).

639 19. Nakurte I, Klavins K, Kirhnere I, Namniece J, Adlere L, Matvejevs Jet al., Discovery of

640 lunasin peptide in triticale (X Triticosecale Wittmack). J Cereal Sci 56:510-514 (2012).

641 20. Nakurte I, Kirhnere I, Namniece J, Saleniece K, Krigere L, Mekssb P, et al., Detection of

642 the lunasin peptide in oats (Avena sativa L.). J Cereal Sci 57:319-324 (2013).

643 21. Legzdina L, Nakurte I, Kirhnere I, Namniece J, Krigere L, Saleniece K, et al., Up to 92%

644 increase of cancer-preventing lunasin in organic spring barley. Agron Sustain Dev 34:783-

645 791 (2014).

646 22. Jeong JB, Jeong HJ, Park JH, Lee SH, Lee JR, Lee HK,et al., Cancer preventive peptide

647 lunasin from Solanum nigrum L. inhibits acetylation of core histones H3 and H4 and

648 phosphorylation of retinoblastoma protein (Rb). J Agric Food Chem 55:10707-10713

649 (2007).

650 23. Silva-Sánchez C, Barba de la Rosa AP, León-Galván MF, de Lumen BO, de León-

651 Rodríguez A and de Mejia EG, Bioactive peptides in amaranth (Amaranthus

652 hypochondriacus) seed. J Agric Food Chem 56:1233-1240 (2008).

653 24. Maldonado-Cervantes E, Jeong HJ, León-Galván F, Barrera-Pacheco A, de León-

654 Rodríguez A, de Mejia EG et al., Amaranth lunasin-like peptide internalizes into the cell

655 nucleus and inhibits chemical carcinogen-induced transformation of NIH-3T3 cells.

656 Peptides 31:1635-1642 (2010).

657 25. Mitchell RAC, Lovegrove A and Shewry PR, Lunasin in cereal seeds: What is the origin?

658 J Cereal Sci 57:267-269 (2013).

659 26. Dinelli G, Bregola V, Bosi S, Fiori J, Gotti R, et al., Lunasin in wheat: A chemical and

660 molecular study on its presence or absence. Food Chem 151:520-525 (2014). 27

661 27. Alaswad AA and Krishnan HB, Immunological investigation for the presence of lunasin, a

662 chemopreventive soybean peptide, in the seeds of diverse plants. J Agric Food Chem

663 64:2901-2909 (2016).

664 28. Rizzello CG, Hernández-Ledesma B, Fernández-Tome S, Curiel JA, Pinto D, Marzani, B,

665 et al., Italian legumes: effect of sourdough fermentation on lunasin-like polypeptides.

666 Microb. Cell Fact 14:1-20 (2015).

667 29. Rizzello CG, Nionelli L, Coda R and Gobbetti M, Synthesis of the cancer preventive

668 peptide lunasin by lactic acid bacteria during sourdough fermentation. Nutr Cancer

669 64:111-120 (2012).

670 30. Hernández-Ledesma B, Hsieh CC and de Lumen BO, Lunasin and Bowman-Birk protease

671 inhibitor (BBI) in US commercial soy foods. Food Chem 115:574-580 (2009).

672 31. Cavazos A, Morales E, Dia VP and de Mejia EG, Analysis of lunasin in commercial and

673 pilot plant produced soybean products and an improved method of lunasin purification. J

674 Food Sci 77:C539-C545 (2012).

675 32. Guijarro-Díez M, García MC, Crego AL and Marina ML, Off-line two dimensional

676 isoelectrofocusing-liquid chromatography/mass spectrometry (time of flight) for the

677 determination of the bioactive peptide lunasin. J Chromatog A 1371:117-124 (2014).

678 33. Krishnan HB and Wang TTY, An effective and simple procedure to isolate abundant

679 quantities of biologically active chemopreventive lunasin protease inhibitor Concentrate

680 (LPIC) from soybean. Food Chem 177:120-126 (2015).

681 34. Setrerrahmane S, Zhang Y, Dai G, Lv J and Tan S, Efficient production of native lunasin

682 with correct N-terminal processing by using the pH-induced self-cleavable Ssp dnab mini-

683 intein system in Escherichia coli. Appl Biochem Biotechnol 174:612-622 (2014).

684 35. Kyle S, James KA and McPherson MJ, Recombinant production of the therapeutic peptide

685 lunasin. Microb Cell Fact 11:1-8 (2012). 28

686 36. Liu CF and Pan TM, Recombinant expression of bioactive peptide lunasin in Escherichia

687 coli. Appl Biochem Biotechnol 88:177-186 (2010).

688 37. Davis KR, Barnett B and Seber L, Method of producing a lunasin polypeptide in plants.

689 U.S. Patent 8,759,613, June 24 (2014).

690 38. Lule VK, Garg S, Pophaly SD, Hitesh S and Tomar SK, Potential health benefits of

691 lunasin: a multifaceted soy-derived bioactive peptide. J Food Sci 80:R485-R494 (2015).

692 39. Park JH, Jeong HJ and de Lumen BO, In vitro digestibility of the cancer-preventive soy

693 peptides lunasin and BBI. J Agric Food Chem 55:10703-10706 (2007).

694 40. Cruz-Huerta E, Fernández-Tomé S, Arques MC, Amigo L, Recio I, Clemente A, et al.,

695 The protective role of the Bowman-Birk protease inhibitor in soybean lunasin digestion:

696 the effect of released peptides on colon cancer growth. Food Funct 6:2626-2635 (2015).

697 41. Fernández-Tomé S, Sanchón J, Recio I and Hernández-Ledesma B, Transepithelial

698 transport of lunasin and derived peptides: inhibitory effects on the gastrointestinal cancer

699 cells viability. J Food Comp Anal (in press) DOI: 10.1016/j.jfca.2017.01.011 (2017).

700 42. Price SJ, Pangloli P, Krishnan HB and Dia VP, Kunitz trypsin inhibitor in addition to

701 Bowman-Birk inhibitor influence stability of lunasin against pepsin-pancreatin hydrolysis.

702 Food Res Int 90:205-215 (2016).

703 43. Hsieh CC, Hernández-Ledesma B, Jeong HJ, Park JH and de Lumen BO, Complementary

704 roles in cancer prevention: protease inhibitor makes the cancer preventive peptide lunasin

705 bioavailable. PLoS One 5:e8890 (2010).

706 44. Jeong HJ, Jeong JB, Kim DS and de Lumen BO, Inhibition of core hystone acetylation by

707 the cancer preventive peptide lunasin. J Agric Food Chem 55:632-637 (2007).

708 45. Dia VP, Torres S, de Lumen BO, Erdman JW and de Mejia EG, Presence of lunasin in

709 plasma of men after soy protein consumption. J Agric Food Chem 57:1260-1266 (2009).

29

710 46. Galvez AF, Chen N, Macasieb J and de Lumen BO, Chemopreventive property of a

711 soybean peptide (lunasin) that binds to deacetylated histones and inhibits acetylation.

712 Cancer Res 61:7473-7478 (2001).

713 47. Lam Y, Galvez A and de Lumen BO, Lunasin suppresses E1A-mediated transformation of

714 mammalian cells but does not inhibit growth of immortalized and established cancer cell

715 lines. Nutr Cancer 47:88-94 (2003).

716 48. Jeong HJ, Park JH, Lam Y and de Lumen BO, Characterization of lunasin isolated from

717 soybean. J Agric Food Chem 51:7901-7906 (2003).

718 49. Galvez AF, Huang L, Magbanua MMJ, Dawson K and Rodriguez RL, Differential

719 expression of thrombospondin (THBS1) in tumorigenic and nontumorigenic prostate

720 epithelial cells in response to a chromatin-binding soy peptide. Nutr Cancer 63:623-636

721 (2011).

722 50. McConnell EJ, Devapatla B, Yaddanapudi K and Davis KR, The soybean-derived peptide

723 lunasin inhibits non-small cell lung cancer cell proliferation by suppressing

724 phosphorylation of the retinoblastoma protein. Oncotarget 6:4649-4662 (2015).

725 51. Malumbres M and Barbacid M, Cell cycle, CDKs and cancer: a changing paradigm. Nat

726 Rev Cancer 9:156-166 (2009).

727 52. Hsieh CC, Hernández-Ledesma B and de Lumen BO, Lunasin, a novel seed peptide,

728 sensitizes human breast cancer MDA-MB-231 cells to aspirin-arrested cell cycle and

729 induced apoptosis. Chem Biol Interact 186:127-134 (2010).

730 53. Hsieh CC, Hernández-Ledesma B and de Lumen BO, Cell proliferation inhibitory and

731 apoptosis-inducing properties of anacardic acid and lunasin in human breast cancer MDA-

732 MB-231 cells. Food Chem 125:630-636 (2011).

30

733 54. Hernández-Ledesma B, Hsieh CC and de Lumen BO, Relationship between lunasin’s

734 sequence and its inhibitory activity of histones H3 and H4 acetylation. Mol Nutr Food Res

735 55:989-998 (2011).

736 55. Inaba J, McConnell EJ and Davis KR, Lunasin sensitivity in non-small cell lung cancer

737 cells is linked to suppression of integrin signaling and changes in histone acetylation. Int J

738 Mol Sci 15:23705-23724 (2014).

739 56. Dia VP and de Mejia EG Lunasin promotes apoptosis in human colon cancer cells by

740 mitochondrial pathway activation and induction of nuclear clusterin expression. Cancer

741 Lett 295:44-53 (2010).

742 57. Dia VP and de Mejia EG, Lunasin induces apoptosis and modifies the expression of genes

743 associated with extracellular matrix and cell adhesion in human metastatic colon cancer

744 cells. Mol Nutr Food Res 55:623-634 (2011).

745 58. de Mejia EG, Wang W and Dia VP, Lunasin, with an arginine-glycine-aspartic acid motif,

746 causes apoptosis to L1210 leukemia cells by activation of caspase-3. Mol Nutr Food Res

747 54:406-414 (2010).

748 59. Pabona JMP, Dave B, Su Y, Montales MTE, de Lumen BO, de Mejia EG, et al., The

749 soybean peptide lunasin promotes apoptosis of mammary epithelial cells via induction of

750 tumor suppressor PTEN: similarities and distinct actions from soy isoflavone .

751 Genes Nutr 8:79-90 (2013).

752 60. Hsieh CC, Hernández-Ledesma B and de Lumen BO, Lunasin-aspirin combination

753 against NIH/3T3 cells transformation induced by chemical carcinogens. Plant Foods

754 Human Nutr 66:107-113 (2011).

755 61. Parise LV, Lee JW and Juliano RL, New aspects of integrin signaling in cancer. Sem

756 Cancer Biol 10:407-414 (2000).

31

757 62. Westermarck J and Kahari VM, Regulation of matrix metalloproteinase expression in

758 tumor invasion. FASEB J 13:781-792 (1999).

759 63. Ruoslahti E and Pierchbacher MD, New perspectives in cell adhesion RGD and integrins.

760 Science 238:491-497 (1987).

761 64. Dia VP and de Mejia EG, Lunasin potentiates the effect of oxaliplatin preventing

762 outgrowth of colon cancer metastasis, bind to α5β1 integrin and suppresses

763 FAK/ERK/NF-kB signaling. Cancer Lett 313:167-180 (2011).

764 65. Jiang Q, Lunasin suppresses the migration and invasion of breast cancer cells by

765 inhibiting matrix metalloproteinases. Onc Rep 36:253-262 (2016).

766 66. Hsieh CC, Wang CH and Huang YS, Lunasin attenuates obesity-associated metastasis of

767 4T1 breast cancer cell through anti-inflammatory property. Int J Mol Sci 17:2109 (2016).

768 67. Al-Dwairi A, Pabona JM, Simmen RC and Simmen FA, Cystolic malic enzyme 1 (ME1)

769 mediates high fat diet-induced adiposity, endocrine profile, and gastrointesintal tract

770 prolifration-associated biomarkers in male mice. PLoS One 7:e46716 (2012).

771 68. Al-Dwairi A, Bron AR, Wight PA, Simmen RC and Simmen FA, Enhanced

772 gastrointestinal expression of cytosolic malic enzyme (ME1) induces intestinal and liver

773 lipogenic gene expression and intestinal cell proliferation in mice. PLoS One 9:e113058

774 (2014).

775 69. Dowling RJ, Goodwin P and Stambolic V, Understanding the benefit of metformin use in

776 cancer treatment. BMC Med 9:33 (2011).

777 70. Sehdev A, Shih YC, Vekhter B, Bissonnette MB, Olopade OI and Polite BN, Metformin

778 for primary colorectal cancer prevention in patients with diabetes: a case-control study in

779 a US population. Cancer 121:1071-1078 (2015).

32

780 71. Nangia-Makker P, Yu Y, Vasudevan A, Farhana L, Rajendara SG, Levi E, et al.,

781 Metformin: a potential therapeutic agent for recurrent colon cancer. PLoS One 9:e84369

782 (2014).

783 72. Montales MT, Simmen RCM, Ferreira ES, Neves VA and Simmen FA, Metformin and

784 soybean-derived bioactive molecules attenuate the expansion of stem cell-like epithelial

785 subpopulation and confer apoptotic sensitivity in human colon cancer cells. Genes Nutr

786 10:1-14 (2015).

787 73. Yu Y, Ramena G and Elble RC, The role of cancer stem cells in relapse of solid tumors.

788 Front Biosci 4:1528-1541 (2012).

789 74. Shidal C, Al-Rayyan N, Yaddanapudi K and Davis KR, Lunasin is a novel therapeutic

790 agent for targeting melanoma cancer stem cells. Oncotarget 7:84128-84141 (2016).

791 75. Shidal C, Inaba J-I, Yaddanapudi K and Davis KR, The soy-derived peptide Lunasin

792 inhibits invasive potential of melanoma initiating cells. Oncotarget 8:25525-25541 (2017).

793 76. Bassett SA and Barnett MPG, The role of dietary histone deacetylases (HDACs)

794 inhibitors in health and disease. Nutrients 6:4273-4301 (2014).

795 77. Lee HS and Herceg Z, The epigenome and cancer prevention: A complex story of dietary

796 supplementation. Cancer Lett 342:275-284 (2014).

797 78. Marmorstein R, Protein modules that manipulate histone tails for chromatin regulation.

798 Nat Rev Mol Cell Biol 2:422-432 (2001).

799 79. de Lumen BO, Lunasin: a cancer-preventive soy peptide. Nutr Rev 63:16-21 (2005).

800 80. Hsieh EA, Chai CM, de Lumen BO, Neese RA and Hellerstein MK, Dynamics of

2 801 keratinocytes in vivo using H2O labeling: A sensitive marker of epidermal proliferation

802 state. J Inv Dermatol 123:530-536 (2004).

33

803 81. Hsieh CC, Hernández-Ledesma B and de Lumen BO, Soybean peptide lunasin suppresses

804 in vitro and in vivo 7,12-dimethylbenz[a]anthracene-induced tumorigenesis. J Food Sci

805 75:H311-H316 (2010).

806 82. Park K, Choi K, Kim H, Kim K, Lee MH, Lee JH, et al., Isoflavone-deprived soy peptide

807 suppresses mammary tumorigenesis by inducing apoptosis. Exp Mol Med 41:371-380

808 (2009).

809 83. Dia VP and de Mejia EG, Potential of lunasin-orally administered in comparison to

810 intraperitoneal injection to inhibit colon cancer metastasis in vivo. J Cancer Ther 4:34-43

811 (2013).

812 84. Devapatla B, Shidal C, Yaddanapudi K and Davis KR, Validation of syngeneic mouse

813 models of melanoma and non-small cell lung cancer for investigating the anticancer

814 effects of the soy-derived peptide Lunasin. F1000 Res 5:2432 (2016).

815 85. Allavena P, Garlanda C, Borrello MG, Sica A and Mantovani A, Pathways connecting

816 inflammation and cancer. Curr Opin Gen Devel 18:3-10 (2008).

817 86. Khan N, Afaq F and Mukhtar H, Cancer chemoprevention through dietary antioxidants:

818 progress and promise. Antiox Redox Sign 10:475-510 (2008).

819 87. García-Nebot MJ, Recio I and Hernández-Ledesma B, Antioxidant activity and protective

820 effects of peptide lunasin against oxidative stress in intestinal Caco-2 cells. Food Chem

821 Toxicol 65:155-161 (2014).

822 88. Jeong JB, de Lumen BO and Jeong HJ, Lunasin peptide purified from Solanum nigrum L.

823 protects DNA from oxidative damage by suppressing the generation of hydroxyl radical

824 via blocking fenton reaction. Cancer Lett 293:58-64 (2010).

825 89. Hernández-Ledesma B, Hsieh CC and de Lumen BO, Antioxidant and anti-inflammatory

826 properties of cancer preventive peptide lunasin in RAW 264.7 macrophages. Biochem

827 Biophys Res Comm 390:803-808 (2009). 34

828 90. Fernández-Tomé S, Ramos S, Cordero-Herrera I, Recio I, Goya L and Hernández-

829 Ledesma B, In vitro chemo-protective effect of bioactive peptide lunasin against oxidative

830 stress in human HepG2 cells. Food Res Int 62:793-800 (2014).

831 91. Dai G, Zhang P, Ye P, Zhang M, Han N, Shuai H, et al., The chemopreventive peptide

832 lunasin inhibits d-galactose- induced experimental cataract in rats. Prot Pept Lett 23:619-

833 625 (2016).

834 92. Dia VP and de Mejia EG, Differential gene expression of RAW 264.7 macrophages in

835 response to the RGD peptide lunasin with and without lipopolysaccharide stimulation.

836 Peptides 32:1979-1988 (2011).

837 93. de Mejia EG and Dia P, Lunasin and lunasin-like peptides inhibit inflammation through

838 suppression of NF-kB pathway in the marcrophage. Peptides 30:2388-2398 (2009).

839 94. Dia VP, Wang W, Oh VL, de Lumen BO and de Mejia EG, Isolation, purification and

840 characterization of lunasin from defatted soybean flour and in vitro evaluation of its anti-

841 inflammatory activity. Food Chem 114:108-115 (2009).

842 95. Ren G, Zhu Y, Shi Z and Li J. Detection of lunasin in quinoa (Chenopodium quinoa

843 Willd.) and the in vitro evaluation of its antioxidant and anti-inflammatory activities. J Sci

844 Food Agric 97:4110-4116 (2017).

845 96. Hsieh CC, Chou MJ and Wang CH, Lunasin attenuates obesity-related inflammation in

846 RAW264.7 cells and 3T3-L1 adipocytes by inhibiting inflammatory cytokine production.

847 PLoS One 12:e0171969 (2017).

848 97. Cam A and de Mejia EG, RGD-peptide lunasin inhibits Akt-mediated NF-kB activation in

849 human macrophages through interaction with the αVβ3 integrin. Mol Nutr Food Res

850 56:1569-1581 (2012).

851 98. FDA Talk Paper, United States Department of Health and Human Services. 1999, October

852 26. Washington, DC: United States Government Printing Office. 35

853 99. Galvez AF, Abstract 10693: Identification of lunasin as the active component in soy

854 protein responsible for reducing LDL cholesterol and risk of cardiovascular disease.

855 Circulation, 2012, 126, A10693.

856 100. Galvez AF, Matel H, Ivey J and Bowles D, Lunasin-enriched soy extract (LunaRich

857 X™), in combination with the dietary supplement Reliv Now, reduces free fatty acid by

858 increasing plasma leptin and adiponectin levels in LDL-receptor mutant pigs. PRWEB

859 [Internet].

860 http://www.prweb.com/releases/lunasinlunarichxrelivnow/nutritionalepigenetics/prweb11

861 137975.htm

862 101. Sison J, Aragon J, Maliwat R and Myrna Y, A study on soy-based supplements as

863 medical nutraceutical therapy in reversing lipid abnormalities [dissertation]. Medical

864 Center Manila, Makati Medical Center, Medical City Philippines.

865 102. Drori A, Rotnemer-Golinkin D, Zolotarov L and Ilan Y. Oral administration of

866 CardioAid and lunasin alleviates liver damage in a high-fat diet nonalcoholic

867 steatohepatitis model. Digestion 96:110-118 (2017).

868 103. Cam A, Sivaguru M and de Mejia EG, Endocytic mechanism of internalization of

869 dietary peptide lunasin into macrophages in inflammatory condition associated with

870 cardiovascular disease. PLoS One 8:e72115 (2013).

871 104. Dzirkale Z, Rumaks J, Svirskis S, Mazina O, Allikalt A, Rinken A, et al., Lunasin-

872 induced behavioural effects in mice: focus on the dopaminergic system. Beh Brain Res

873 256, 5-9 (2013).

874 105. Chang HC, Lewis D, Tung CY, Han L, Henriquez SMP, Voiles L, et al., Soypeptide

875 lunasin in cytokine immunotherapy for lymphoma. Cancer Immunol Immunother 63:283-

876 295 (2014).

36

877 106. Tung CY, Lewis DE, Hana L, Jaja M, Yao S, Li F, et al., Activation of dendritic cell

878 function by soypeptide lunasin as a novel vaccine adjuvant. Vaccine 32:5411-5419 (2014).

879 107. Jia S, Zhang S, Yuan H and Chen N, Lunasin inhibits cell proliferation via apoptosis

880 and reduces the production of proinflammatory cytokines in cultured rheumatoid arthritis

881 synovial fibroblasts. BioMed Res Int ID:346839 (2015).

882 108. Yang X, Zhu J, Tung CY, Gardiner G, Wang Q, Chang HC, et al., Lunasin alleviates

883 allergic airway inflammation while increases antigen-specific tregs. PLoS One 3: 1-11

884 (2015).

37

Figure legend

Figure 1. Lunasin, a natural peptide, acts with multiple bioactivities, including cancer prevention, anti-oxidative, anti-inflammatory, cholesterol biosynthesis regulatory, and central nervous system and immune system modulatory activities.

38

Table 1. Methodology of quantification and peptide lunasin concentration (expressed as mg/g of protein and mg/100 g product) of different soybean-derived products

Lunasin concentration Type of food Quantification methodology Reference mg/g protein mg/100 g product Textured soybean LC/MS-TOF analyzer 20.9-22.5 1600.0-1800.0 32

Soybean flour LC/MS-TOF analyzer 14.0-17.1 700.0-800.0 32

Regular soymilk Western-Blot 4.7-5.6 11.8-15.7 30 ELISA 0.5-2.8 1.8-9.3 31 Organic soymilk Western-Blot 4.3-8.3 10.7-18.9 30 ELISA 1.0-2.7 2.9-9.1 31 Regular soy-based formula Western-Blot 7.3 4.1 30 ELISA 4.4-5.5 7.3-8.9 31 Organic soy-based formula Western-Blot 1.7-7.0 1.5-2.8 30 Soy shake ELISA 0.1-0.4 1.3-3.6 31 Regular Western-Blot 40.7-104.8 3.5-14.3 30 Organic tofu Western-Blot 30.9 6.7 30 Processed tofu Western-Blot 48.3-77.3 0.4-5.5 30 Regular Western-Blot n.d. n.d. 30 Organic tempeh Western-Blot 24.3-39.7 6.1-8.2 30 Bean curd Western-Blot 0-165.8 0-9.5 30 Soybean curd Western-Blot 77.3-135.4 1.1-10.7 30 Su Jea Western-Blot n.d. n.d. 30 Natto Western-Blot n.d. n.d. 30 Western-Blot n.d. n.d. 30 Soybean beverage powder Top-down mass spectrometry --- 22-23a 9 2.7-3.9b 9 a : Native lunasin b : Glycated lunasin n.d. not detected

39