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Water-Soluble Au Ncs for Multiplexed Mass Spectrometry Imaging

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Water-Soluble Au Ncs for Multiplexed Mass Spectrometry Imaging Electronic Supplementary Material (ESI) for ChemComm. This journal is © The Royal Society of Chemistry 2017 Supporting Information Water-soluble Au NCs for Multiplexed Mass Spectrometry Imaging Jinan Li,ac Jing Liu,ad Zheyi Liu,a, Yuan Tan,bc Xiaoyan Liu,b Fangjun Wang*a aCAS Key Laboratory of Separation Sciences for Analytical Chemistry, National Chromatographic R&A Center, Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS), Dalian 116023, China bState Key Laboratory of Catalysis, iChEM, Gold Catalysis Research Center, Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS), Dalian 116023, China cUniversity of Chinese Academy of Science, Beijing 100049, China dCollege of Pharmacy, Dalian Medical University, Dalian 116044, China. *E-mail: [email protected], Tel: +86-411-82464150, Fax: +86-411-84379620 Contents Page Materials and reagents S-1 Synthesis of Au NCs S-1 Experiment Synthesis of Au NPs S-1 details Materials Characterization S-1 Sample Preparation for MALDI-MS S-2 Mass spectrometry imaging. S-2 Fig. S1 (A) Illustration of the synthesis of homogeneous Au NCs; (B) Typical TEM image of Au NCs (Left) and Au NPs (Right) with scale bar of 20 -1 nm; (C) TGA results of Au NCs under N2 atmosphere with increasing temperature at 10 °C min ; (D) UV−vis absorption spectrum for as-prepared S-4 Au NCs and Au NPs. Fig. S2 Optical images of DHB crystal (A), DHB-analyte cocrystal (B), Au NCs (C), Au NCs-analyte cocrystal (D), Au NPs (E), and Au NPs-analyte S-5 cocrystal (F) on the MALDI steel plate. Fig. S3 The MS spectra of glucose with the different concentration of Au NCs as matrix. S-6 Fig. S4 Mass spectra of carbamazepine (A, m/z = 237.9 [M+H]+, 258.8 [M+Na]+, 274.8 [M+K]+ and 280.8 [M+2Na-H]+), cytosine (B, m/z = 111.9 [M+H]+, 133.9 [M+Na]+, 149.9 [M+K]+ and 155.9 [M+2Na-H]+), glutathione (C, m/z = 307.9 [M+H]+ and 329.9 [M+Na]+) and trechalose (D, m/z = S-7 364.9 [M+Na]+) with Au NCs (a), DHB (b), Au NPs (c) as matrix, or without any matrix (d) for MALDI-MS detection in the positive-ion reflector mode. The amount of analyte was 5 nmol. Fig. S5 Mass spectra of xylose (A, m/z = 172.8 [M+Na]+), trechalose (B, m/z = 364.9 [M+Na]+ and 386.9 [M+2Na-H]+), sucrose (C, m/z = 364.9 Supporting [M+Na]+, 380.9 [M+K]+ and 387.0 [M+2Na-H]+ ), ribose (D, m/z = 172.9 [M+Na]+), raffinose (E, m/z = 527.0 [M+Na]+), maltose (F, m/z = 364.9 Figures and [M+Na]+), lactose (G, m/z = 364.9 [M+Na]+ and 381.0 [M+K]+), glucose (H, m/z = 202.9 [M+Na]+), galactose (I, m/z = 202.9 [M+Na]+) and 1- S-8 Tables progargyl-O-maltose (J, m/z = 402.8 [M+Na]+) with Au NCs for MALDI-MS detection in the positive-ion reflector mode. The amount of analyte was 5 nmol. Fig. S6 Mass spectra of cytidine (A, m/z = 243.9 [M+H]+,265.9 [M+Na]+ and 281.9 [M+K]+), cytosine (B, m/z = 111.0 [M+H]+,133.9 [M+Na]+, 149.9 [M+K]+ and 155.9 [M+2Na-H]+), uridine (C, m/z = 266.9 [M+Na]+), triolein (D, m/z = 907.8 [M+Na]+), oleic acid (E, m/z = 305.4 [M+Na]+ and 327.4 [M+2Na-H]+), linoleic acid (F, m/z = 303.8 [M+Na]+ and 325.4 [M+2Na-H]+), linolenic acid (G, m/z = 301.4 [M+Na]+, 323.5 [M+2Na-H]+ and S-9 339.4 [M+Na+K-H]+), palmitic acid (H, m/z = 279.5 [M+Na]+ and 301.5 [M+2Na-H]+) and arachidonic acid (I, m/z = 327.3 [M+Na]+, 349.6 [M+2Na- H]+ and 365.4 [M+Na+K-H]+) with Au NCs for MALDI-MS detection in the positive-ion reflector mode. The amount of analyte was 5 nmol. Fig. S7 Mass spectra of 3-O-tigloylswietenolide (A, m/z = 591.0 [M+Na]+), atropine (B, m/z =290.0 [M+H]+, 311.9 [M+Na]+ and 327.9 [M+K]+), azedarachol (C, m/z = 443.0 [M+Na]+), gastrodin (D, m/z = 309.0 [M+Na]+, 325.0 [M+K]+ and 331.0 [M+2Na-H]+) and carbamazepine (E, m/z = S-10 258.8 [M+Na]+, 274.8 [M+K]+ and 250.8 [M+2Na-H]+) with Au NCs for MALDI-MS detection in the positive-ion reflector mode. The amount of analyte was 5 nmol. Fig. S8 Mass spectra of W-G (A, m/z = 261.9 [M+H]+ and 283.9 [M+Na]+), G-W-G (B, m/z = 318.9 [M+H]+ and 341.0 [M+Na]+), W-L (C, m/z = 318.0 [M+H]+ and 340.1 [M+Na]+ ), F-A (D, m/z = 236.9 [M+H]+ and 250.9 [M+Na]+), F-A-N (E, m/z = 351.0 [M+H]+ and 373.1 [M+Na]+), F-G-G (F, m/z = 280.0 [M+H]+ and 302.0 [M+Na]+), F-E (G, m/z = 295.0 [M+H]+ and 317.0 [M+Na]+), YV (H, m/z = 281.0 [M+H]+ and 303.1 [M+Na]+) S-11 and glutathione (I, m/z = 308.0 [M+H]+ and 330.0 [M+Na]+) with Au NCs for MALDI-MS detection in the positive-ion reflector mode. The amount of analyte was 5 nmol. Fig. S9 Heatmap generated from the relative deviation of MS intensity related to the analytes commonly detected with Au NCs and DHB as matrix. S-12 Relative deviation is the difference between 1 and the ratio of MS intensity experimental value and average value Fig. S10 Mass spectra of 1-propargyl-O-maltose with Au NCs as matrix. The analyte was 5 nmol with different concentration of NaCl (i), NH HCO 4 3 S-13 (ii) and BSA (iii). The solvent is H2O, H2O and 10 mM NH4HCO3, respectively. Fig. S11 Mass spectra of peptide F-E with Au NCs as matrix. The analyte was 5 nmol with different concentration of NaCl (i), NH HCO (ii) and 4 3 S-13 BSA (iii). The solvent is H2O, H2O and 10 mM NH4HCO3, respectively. Fig. S12 Mass spectra of cytosine with Au NCs as matrix. The analyte was 5 nmol with different concentration of NaCl (i), NH HCO (ii) and BSA 4 3 S-14 (iii). The solvent is H2O, H2O and 10 mM NH4HCO3, respectively. Fig. S13 Average MS spectra of Au NCs-assisted MSI of mouse brain slice. S-15 Fig. S14 Average MS spectra of DHB-assisted MSI of mouse brain slice. The peaks signed with × were caused by DHB. S-16 Fig. S15 MS images related to PAs, PCs and other kinds of biomolecules commonly detected by both Au NCs and DHB assisted MSI. S-17 Fig. S16 MS images related to biomolecules detected only by Au NCs assisted MSI. S-18 Fig. S17 MS images related to biomolecules detected only by DHB assisted MSI. S-19 Table S1 The chemical structure, special charge of relative ions, detection RSD (Au NCs and DHB), and LODs (Au NCs) of analytes. S-20 Table S2 MS peak intensities and signal to noise ratios (S/N) of the seven kinds of biomolecules with Au NCs, DHB, and Au NPs as matrix, S-27 respectively. Table S3 List of biomolecules commonly detected in MSI of mouse brain by both Au NCs and DHB. The * represents that the ion was recorded with S-28 high-quality MS images (with clear lateral distribution outlines). Table S4 List of analytes detected in MSI of mouse brain by Au NCs. The * represents that the ion was recorded with high-quality MS images (with S-35 clear lateral distribution outlines). Table S5 List of analytes detected in MSI of mouse brain by DHB. The * represents that the ion was recorded with high-quality MS images (with S-39 clear lateral distribution outlines). 1. Experiment details Materials and reagents Cysteine (Cys), 2,5-dihyroxyl benzoic acid (DHB), sodium borohydride (NaBH4), sugars (glucose, xylose, sucrose, maltose, raffinose, ribose, lactose, trechalose, and galactose), nucleosides (cytosine, cytidine, and uridine), glutathione (GSH), triolein and fatty acid (oleic acid, linoleic acid, linolenic acid, palmitic acid, and arachidonic acid) were purchased from Sigma-Aldrich (St, Louis, MO, USA). Atropine, carbamazepine, azedarachol, gastrodin and 3-O-tigloylswietenolide were obtained from Aladdin (Shanghai, China). Peptides (W-G, G-W-G, W-L, F-A, F-A-N, F-G-G, F-E and Y-V) were obtained from SERVA Electrophoresis GmbH (Heidelberg, Germany). 1- propargyl-O-maltose was synthesized according to previous report.1 Acetonitrile (ACN) was purchased from Merck (Darmstadt, Germany). Chloroauric acid (HAuCl4) was purchased from Shenyang Nonferrous Metal Research Institute (Shenyang, China). Ammonium bicarbonate (NH4HCO3), sodium hydroxide (NaOH), concentration hydrochloric acid (HCl), nitric acid, anhydrous ethanol and methanol were obtained from Tianjin Kermel plant of chemical reagent (Tianjin, China). Pure water was prepared with a Milli-Q system (Millpore, Bedford, MA, USA). Synthesis of Au NCs All of the glassware was cleaned with aqua regia before use. Au NCs were prepared according to previous 2,3 reports. Typically, an aqueous solution of HAuCl4 (40 mM, 3.75 mL) was added into ultrapure water (141.75 mL), followed by the addition of an aqueous Cys solution (50 mM, 4.5 mL) and the pH of the mixture was adjusted to approximately 12 by using a NaOH solution (1 M).
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