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A Novel Stationary Phase of Thin Layer Chromatography RSC Advances View Article Online PAPER View Journal | View Issue Polymerized high internal phase emulsion monolithic material: a novel stationary phase of Cite this: RSC Adv.,2017,7,7303 thin layer chromatography Dezhong Yin,*a Yudong Guan,a Huimin Gu,b Yu Jiaa and Qiuyu zhang*b A polymerized high internal phase emulsion (polyHIPE) was prepared using styrene, divinylbenzene and butyl acrylate as raw material and employed as stationary phase of thin layer chromatography (TLC). SEM, mercury intrusion porosimetry and FT-IR spectrum were employed to characterize the pore structure and chemical composition. To verify the feasibility as stationary phase of TLC, identification of plant extracts, Chinese herbs and traditional Chinese medicine were practiced on the prepared polyHIPE. Relative retardation factor (a), theoretical plate number (Nplate) and resolution (R) were used to evaluate Received 1st December 2016 the performance of TLC. Large difference in a value make it is feasible to optimize the chromatographic Accepted 9th January 2017 condition. The resolution R and Nplate indicates that the introduction of BA in polyHIPE facilitates the DOI: 10.1039/c6ra27609a Creative Commons Attribution-NonCommercial 3.0 Unported Licence. preparation and improves the performance for TLC separation. Our results show that polyHIPE monolith www.rsc.org/advances is a reusable stationary phase of TLC with high performance. 1. Introduction separation and determination of two steroid hormones, namely progesterone and testosterone.10 Validity of the Thin-layer chromatography (TLC), with a thin layer sorbent as method was investigated, and a wide linear range of 1–200 ng separation medium, is mostly used to monitor the progress of per spot, and low detection limits of 0.16 ng and 0.13 ng per organic reactions, to identify compounds in a given mixture, spot, low quantication limits of 0.51 ng and 0.40 ng per spot, This article is licensed under a and to determine product purity. The main advantages of TLC and good precision (expressed as percent relative standard are the use of inexpensive equipment, lower purity of deviation) lower than 3.1% and 2.7% were obtained for consuming solvents, saving a signicant amount of consum- progesterone and testosterone. A DNA/PVA interpenetrating ables.1–3 It is important to select a suitable stationary phase polymer network was used to coat the surface of the porous Open Access Article. Published on 23 January 2017. Downloaded 9/27/2021 10:35:12 PM. 11 when using TLC to separate mixtures. Thin chromatographic silica particles for TLC. layers can be formed from different organic and inorganic Monolith, a single continuous rod of highly porous material sorbents4,5 and different plates are commercially available. The with an interconnected network of pores, is demonstrated to be most commonly used conventional TLC plates consist of an excellent candidate as ideal stationary phase of chromatog- 12,13 sorbent layers formed from irregular ca. 10 mm silica particles raphy. For TLC analysis, several monoliths have been held together by a binder. successfully demonstrated. A poly(butylmethacrylate-co- Recent year, several new stationary phases6–8 have been ethylene dimethacrylate) layer was prepared and used for developed, providing users alternative for more difficult separation of peptides and proteins, followed by MALDI-TOF- 14 chromatographic separations. Hollow silica microspheres MS detection. Two-dimensional thin layer chromatography with different structures have been synthesized and used to of peptides was also carried out on a superhydrophobic separate a model mixture of methyl red and dimethyl yellow.9 monolithic porous polymer layers coupled with desorption 15 A comparison test shows that HSMs as a stationary phase are electrospray ionization mass spectrometer or matrix-assisted 16 advantageous over commercial silica gel in an easy prepara- laser desorption/ionization (MALDI) mass spectrometry. F. tion of homogeneous TLC thin plates. Another kind of silica Svec prepared porous hypercrosslinking styrenics-based gel, gold nanoparticles graed 3-triethoxysilyl propylamine monolithic layers via a Friedel–Cras alkylation reaction then modied silica gel was developed as a stationary phase for formed a multiplicity of mesopores that increased the surface area and enabled separation of small dye molecules.17 Poly- amide was also used in TLC to separate catechins and O- aSchool of Science, Northwestern Polytechnical University, Xi'an 710072, China. methylated (À)-epigallocatechin gallate.18 E-mail: [email protected] High internal phase emulsions (HIPEs), an emulsion with bKey Laboratory of Space Applied Physics and Chemistry, Ministry of Education, Northwestern Polytechnical University, Xi'an, Shaanxi, 710072, China. E-mail: internal phase exceeds 74%, has been found considerable to [email protected] create highly porous polymer monoliths (referred as This journal is © The Royal Society of Chemistry 2017 RSC Adv.,2017,7,7303–7309 | 7303 View Article Online RSC Advances Paper polyHIPE).19,20 By large amount of surfactants,21 a large portion Then viscous HIPE was poured into the mold (Fig. 1b) and of internal phase can be stabilised in the continuous phase to covered with a glass plate to prevent the evaporation of form stable HIPE. Aer the polymerisation, polyHIPE materials monomer during following curing process (Fig. 1c). Aer the with a typical inter-connected porous morphology, consisting of polymerization was completed for 8 hours in 70 Cwater-bath, large primary pores(cavities) and smaller interconnecting pores, the mould was disassembled and a monolithic plate was ob- are obtained. Due to special properties of low density, high tained(Fig.1d).Finally,theplatewaswashedinethanol porosity, interconnected pore structure and high permeability,22 ultrasonically to remove the impurities and a polyHIPE plate polyHIPE is used in as adsorbents,23 catalyst carriers,24 separa- of 2 mm thickness was obtained. tion medium.25 Optical micrographs were collected with an optical micro- It raised signicant interest in the polyHIPE as stationary scope equipped with a digital camera (CAIKON, China). FTIR phase of TLC due to the well-dened monolithic shape and spectrum (Fourier transformation infrared) was obtained interconnected pore structure of polyHIPE. In this paper, using a BRUKER Tensor 27 spectrometer. Morphology was porous polyHIPE monolithic plates were prepared and used as characterized by a JSM-6700 F Scanning electron microscope stationary phase of TLC for identication of Chinese herbal (Japan) equipped with a eld emission electron gun. The total medicinal ingredients. To the best of our knowledge, this is pore area of polyHIPE was characterized by mercury poros- the rst demonstration of polyHIPE as stationary phase of imetry (AUTOPORE IV 9500, Micromeritics, USA). The porosity TLC. of polyHIPE was measured using pyncometry. The foam r density ( f) of polyHIPEs was measured on approximately 3 3 r 2. Experimental cm of broken pieces of each sample. The matrix density ( m) was determined using a pycnometer using approximately 2.1. Chemicals 500 mg of crushed polyHIPEs and ethanol as medium. The Styrene (St, 99 wt%), divinylbenzene (DVB, 80 wt%), benzoyl porosity (P) of polyHIPE was calculated according to the 28 Creative Commons Attribution-NonCommercial 3.0 Unported Licence. peroxide (BPO, 99 wt%) were purchased from Sinopharm following equation: Chemical Reagent Co. (Shanghai, China). Butyl acrylate (BA), r P ¼ 1 À f  100% CaCl2 and sorbitan monooleate (span80) were purchased from (1) rm Fucheng Chemical Reagent Co. (Tianjing, China). Three herb extracts (emodin, chrysophanol, tanshinone), two herbs (Rhi- zoma Chuanxiong and Polygonum Cuspidatum) were 2.3. TLC analysis purchased from National Institute for food and drug Control of For the TLC analysis, solutions preparation and TLC separation China. All the chemicals were of analytical grade and used as were practiced according to the Chinese pharmacopoeia. Herb received. À1 This article is licensed under a extracts were dissolved in ethanol (1 mg mL ). For TLC of herbs, 1.0 g herb or herbs mixture were extracted ultrasonically 2.2. Preparation of polyHIPE plate for 15 minutes in methanol. Then the solution was separated by A water-in-oil HIPE was prepared by mixing oil phase and lter and concentrated to 2 mL. A second lter was practised to Open Access Article. Published on 23 January 2017. Downloaded 9/27/2021 10:35:12 PM. aqueous phase (1.0 wt% CaCl2 solution) and emulsifying by get a clean solution for TLC. 5 mL of solution was spotted at one homogenizer, as reported elsewhere.26,27 As a typical proce- end of polyHIPEs plate by using a glass capillary and developed dure, monomer (including St, BA, DVB), BPO and span80 were in a TLC tank containing mobile phase. The time and the mixed to form oil phase. CaCl2 aqueous solution (1.0 wt%) distance of TLC develop was recorded and the permeability of was added dropwise under constant stirring at 3000 rpm. monolith was calculated by dividing the distance with the time Once all aqueous phase has been added, stirring was of TLC develop. Aer development, the plate was air-dried and continued for a further 5 min to produce a uniform milky W/O visualized under daylight or ultraviolet (365 nm). To make the HIPE. To assemble a rectangle mould for curing the emulsion, monolith plate reusable, polyHIPE was washed by methanol four slides (thickness 2 mm) was put on a glass plate (Fig. 1a). ultrasonically. Relative retardation factor (a), theoretical plate Fig. 1 Schematic illustration of preparation of polyHIPE plate. 7304 | RSC Adv.,2017,7,7303–7309 This journal is © The Royal Society of Chemistry 2017 View Article Online Paper RSC Advances number (Nplate) and resolution (R) were used to evaluate the 3. Results and discussion performance of TLC, according to equations: 3.1. Preparation of HIPE and polyHIPE Rf;2 a2;1 ¼ (2) Rf;1 In this study, we applied a process developed previously in our lab26,29 for the preparation of HIPE. Span80 was developed as the L 2 most efficient stabilizer for styrenics-based HIPE with high Nplate ¼ 16 (3) viscosity.
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