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Showing papers on "Thin-layer chromatography published in 2016"


Journal ArticleDOI
TL;DR: N nanoparticle synthesis by a hitherto unreported actinomycete culture is highlighted, the biomolecule involved in the process is identified and the associated antioxidant activity is described.

64 citations


Journal ArticleDOI
TL;DR: The identification of a novel metabolite N-(1-(2,2-dimethyl-5-undecyl-1,3-dioxolan-4-yl)-2-hydroxyethyl)stearamide by spectral studies can be exploited for pest management in future.

42 citations


Journal ArticleDOI
TL;DR: The chemical structure of astaxanthin was confirmed by thin layer chromatography (TLC), UV spectroscopy scanning, high performance liquid chromatography with a ZORBAX SB-C18 column and a Waters Nova-pak C18 column, and ESI/MS/MS.

27 citations


Journal ArticleDOI
TL;DR: TLC is used to completely separate acetaminophen and its internal standard from other components and to form a single spot/zone containing them at the solvent front position (after the final stage of the thin-layer chromatogram development).

26 citations


Journal ArticleDOI
TL;DR: This protocol provides useful information regarding the preparation and characterization of drug-loaded micelles and thus will facilitate the research and development of novel micelle-based cancer nanomedicines.
Abstract: Micelles have been successfully used for the delivery of anticancer drugs. Amphiphilic polymers form core-shell structured micelles in an aqueous environment through self-assembly. The hydrophobic core of micelles functions as a drug reservoir and encapsulates hydrophobic drugs. The hydrophilic shell prevents the aggregation of micelles and also prolongs their systemic circulation in vivo. In this protocol, we describe a method to synthesize a doxorubicin lipophilic pro-drug, doxorubicin-palmitic acid (DOX-PA), which will enhance drug loading into micelles. A pH-sensitive hydrazone linker was used to conjugate doxorubicin with the lipid, which facilitates the release of free doxorubicin inside cancer cells. Synthesized DOX-PA was purified with a silica gel column using dichloromethane/methanol as the eluent. Purified DOX-PA was analyzed with thin layer chromatography (TLC) and (1)H-Nuclear Magnetic Resonance Spectroscopy ((1)H-NMR). A film dispersion method was used to prepare DOX-PA loaded DSPE-PEG micelles. In addition, several methods for characterizing micelle formulations are described, including determination of DOX-PA concentration and encapsulation efficiency, measurement of particle size and distribution, and assessment of in vitro anticancer activities. This protocol provides useful information regarding the preparation and characterization of drug-loaded micelles and thus will facilitate the research and development of novel micelle-based cancer nanomedicines.

26 citations


Journal ArticleDOI
TL;DR: In this paper, an oil sample was fractionated into five fractions, referred to as saturate, aro1, a ro2, polar1, and polar2; these fractions were completely characterized by thin-layer chromatography-flame ionization detection (TLC-FID), field desorption (FD) and (+) atmospheric pressure photoionization (APPI) high-resolution mass spectrometry (HR-MS), and gas chromatography with an atomic emission detector (GC-AED).
Abstract: In this study, a preparatory-scale fractionation method was developed. To verify the effectiveness of this method, an oil sample was fractionated into five fractions, referred to as saturate, aro1, aro2, polar1, and polar2; these fractions were completely characterized by thin-layer chromatography–flame ionization detection (TLC–FID), field desorption (FD) and (+) atmospheric pressure photoionization (APPI) high-resolution mass spectrometry (HR-MS), and gas chromatography with an atomic emission detector (GC–AED). TLC–FID analysis was used to compare the results obtained by the fractionation method to those obtained from the conventional saturates, aromatics, resins, and asphaltenes (SARA) method. FD–MS was employed to characterize the hydrocarbon class compounds in the saturate and aro1 fractions. As observed from the FD–MS spectra, non-aromatic hydrocarbon compounds were abundant in saturates, while mono- and diaromatic compounds were abundant in the aro1 fraction. This result is in good agreement with ...

25 citations


Journal ArticleDOI
TL;DR: The dichloromethane extract of A. mirheydari Iranshar, an endemic plant from Iran, was investigated for its cytotoxic properties and chemical constituents and was the most active one among the tested material.
Abstract: Context The genus Anthemis L. (Asteraceae) comprises about 195 species which are widely used in the pharmaceutical, cosmetic and food industries. Objective Anthemis mirheydari Iranshar, an endemic plant from Iran, was investigated for its cytotoxic properties and chemical constituents. Materials and methods The whole parts of the plant (320 g) were extracted by dichloromethane and methanol for four days, successively. The cytotoxic activity of both dichloromethane and methanol extracts were assayed by 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide colorimetric methods against three human cancer cell lines including LS180, MCF-7 and MOLT-4. Different concentrations (10-100 μg/mL) of the plant extracts were tested to obtain IC50 values. The dichloromethane extract of A. mirheydari was subjected to silica gel-column and thin layer chromatography for purification of its chemical constituents and the isolated compounds were further tested against MOLT-4 cells. The structures of the pure compounds were elucidated using different spectral data including nuclear magnetic resonance and electron impact mass spectra. Results The IC50 values of the dichloromethane extract were 30.8 ± 6.7, 25.2 ± 6.5 and 8.6 ± 1.1 μg/mL (means ± standard error) for the above-mentioned cell lines, respectively. Two triterpenoids, taraxasterol (1) and pseudotaraxasterol (2), one sterol, β-sitosterol (3) and one coumarin, 7-methoxycoumarin (4) were isolated from the extract. The IC50 of the mixture of compounds 1 and 2 as well as compounds 3 and 4 were higher (>100 μM) than that reported for the dichloromethane extract against MOLT-4 cells. Conclusion The dichloromethane extract was the most active one among the tested material.

21 citations


Journal ArticleDOI
TL;DR: The research findings have supported the claims that extracts of Allium cepa possess glucose lowering properties in experimental diabetic animals.
Abstract: BACKGROUND Allium cepa has been in use in traditional medicine in the treatment of diabetes mellitus. The aqueous and ethanolic extracts have been found effective in lowering blood glucose levels in experimental diabetic rats and guinea pigs. METHODS The study was carried out to isolate the active principle responsible for the observed hypoglycaemic effect in experimental animals. Freeze-dried aqueous extract of Allium cepa was separated into various fractions using column chromatography with silica gel as a stationary phase. The column was eluted with various ratios of mixtures of hexane, chloroform, ethyl acetate and methanol. These column fractions obtained were tested for hypoglycaemic effects in alloxan-induced diabetic male rats. The identified active fraction was further separated by means of preparative thin layer chromatography (P-TLC) using silica gel as stationary phase and mixture of solvents chloroform, ethyl acetate, and methanol in the ratio of 10: 4: 1 respectively as the mobile phase. Pre-coated P-TLC plates were used and the fraction bands were identified under u.v. lamp and by spraying with concentrated sulphuric acidvanillin reagent. The isolated bands (Rf 0.438) were scrapped off from the P-TLC plates, redissolved in absolute methanol, filtered and concentrated to dryness. RESULTS The isolated compound's structure was determined be means of one and two dimensional nuclear magnetic resonance spectroscopy as well as comparison with literature data. The isolated compound given at 25 mg/kg dose reduced blood glucose in diabetic rats in manner which was comparable to the effect obtained with 2 mg/kg of glibenclamide (p < 0.05). The structure of the compound was found to be that of kaempferol- 3-O-β - D 6{P-coumaroyl} glucopyranoside. CONCLUSION The research findings have supported the claims that extracts of Allium cepa possess glucose lowering properties in experimental diabetic animals.

19 citations


Journal ArticleDOI
TL;DR: The results of this study could lead to the development of novel therapeutic agents capable of dealing with specific diseases that either have weakened reaction or are currently not responsive to existing drugs.
Abstract: This study isolated and identified the antimicrobial compounds of Philippine Piper betle L. leaf ethanol extracts by thin layer chromatography- (TLC-) bioautography and gas chromatography-mass spectrometry (GC-MS). Initially, TLC separation of the leaf ethanol extracts provided a maximum of eight compounds with values of 0.92, 0.86, 0.76, 0.53, 0.40, 0.25, 0.13, and 0.013, best visualized when inspected under UV 366 nm. Agar-overlay bioautography of the isolated compounds demonstrated two spots with values of 0.86 and 0.13 showing inhibitory activities against two Gram-positive multidrug-resistant (MDR) bacteria, namely, methicillin-resistant Staphylococcus aureus and vancomycin-resistant Enterococcus. The compound with an value of 0.86 also possessed inhibitory activity against Gram-negative MDR bacteria, namely, carbapenem-resistant Enterobacteriaceae-Klebsiella pneumoniae and metallo-β-lactamase-producing Acinetobacter baumannii. GC-MS was performed to identify the semivolatile and volatile compounds present in the leaf ethanol extracts. Six compounds were identified, four of which are new compounds that have not been mentioned in the medical literature. The chemical compounds isolated include ethyl diazoacetate, tris(trifluoromethyl)phosphine, heptafluorobutyrate, 3-fluoro-2-propynenitrite, 4-(2-propenyl)phenol, and eugenol. The results of this study could lead to the development of novel therapeutic agents capable of dealing with specific diseases that either have weakened reaction or are currently not responsive to existing drugs.

19 citations


Journal ArticleDOI
TL;DR: DAPPI-MS was found to be a simple, rapid, and efficient approach for detecting lipids separated by TLC.
Abstract: Desorption atmospheric pressure photoionization (DAPPI) allows surface analysis in the open atmosphere and is thus an appropriate method for the direct coupling of thin-layer chromatography (TLC) and mass spectrometry (MS). Here, the capability of DAPPI-MS for ionizing and detecting lipids, namely, cholesterol, triacylglycerols, 1,2-diol diesters, wax esters, cholesteryl esters, and hydrocarbons, from TLC and high-performance thin-layer chromatography (HPTLC) plates in MS and MS2 modes was tested. Limits of detection for lipid standards separated using normal-phase (NP)-TLC and NP-HPTLC were established. TLC/DAPPI-MS was applied for lipids of vernix caseosa, a white creamy proteolipid biofilm that progressively coats the fetus during the last trimester of the pregnancy, and plant oils including caraway, parsley, safflower, and jojoba oils. Various lipids were identified by means of high resolution/accurate mass measurement of Orbitrap and comparison of the retardation factors with standards. Lipid class s...

16 citations


Journal ArticleDOI
TL;DR: It is shown, that the system type inversion results in significant change of selectivity of separation, which may be especially useful in 2D separation of complex samples of basic/amphoteric compounds such as peptides.

Journal ArticleDOI
TL;DR: It is shown that the colloid content can be measured by TLC and that solid phase extraction and HPLC completely remove 68Ga-colloid from 68 Ga-labeled tracer preparations, resulting in very low liver and spleen uptake.
Abstract: Ga-labeled radiotracers are increasingly used for PET imaging. During the labeling procedure, formation of 68Ga-colloid may occur. Upon i.v. injection, 68Ga-colloid will accumulate rapidly in the liver, spleen, and bone marrow, resulting in reduced target-to-background ratios. In this study, we applied a thin layer chromatography (TLC) method to measure colloid content and we studied the effect of the purification method on the in vivo characteristics of 68Ga-labeled DOTA-exendin-3. DOTA-exendin-3 was labeled with 68Ga, and the colloid content was measured by TLC on silica gel ITLC with two mobile phases. The labeling mixture was purified by gel filtration on a 5-ml G25M column, by reversed-phase high-performance liquid chromatography (RP-HPLC) using a C8 column or by solid phase extraction (SPE) on an HLB cartridge. The in vivo characteristics of the preparations were determined in BALB/c nude mice, and PET images were acquired 1 h p.i. using a microPET scanner. In these studies, unpurified 68Ga-DOTA-exendin-3 and 111In-DOTA-exendin-3 were used as a reference. The colloid content of 111In-DOTA-exendin-3 and unpurified, gel filtration, RP-HPLC- and SPE-purified 68Ga-DOTA exendin-3 was <3, 7, 9, <3, and <3 %, respectively. Unpurified 68Ga-DOTA exendin-3 showed high liver and spleen uptake. Gel filtration partly removed 68Ga-colloid from the preparation, resulting in moderate liver and spleen SPE-purified 68Ga-DOTA exendin-3 showed very low liver and spleen uptake, that was similar to that of RP-HPLC purified 68Ga-DOTA exendin-3. We showed that the colloid content can be measured by TLC and that solid phase extraction and HPLC completely remove 68Ga-colloid from 68Ga-labeled tracer preparations, resulting in very low liver and spleen uptake. This study clearly shows the importance of removal of 68Ga-colloid from preparations.

Journal ArticleDOI
TL;DR: This novel addition to the isolation protocol increased the purity of fucoxanthin and allowed for concentration of diadinoxanth in and diatoxanthin before HPLC separation, and the enhanced protocol is useful for obtaining high purity pigments for biochemical studies.
Abstract: Fucoxanthin, diadinoxanthin and diatoxanthin are carotenoids found in brown algae and most other heterokonts. These pigments are involved in photosynthetic and photoprotective reactions, and they have many potential health benefits. They can be extracted from diatom Phaeodactylum tricornutum by sonication, extraction with chloroform : methanol and preparative thin layer chromatography. We assessed the utility of an additional column chromatography step in purification of these pigments. This novel addition to the isolation protocol increased the purity of fucoxanthin and allowed for concentration of diadinoxanthin and diatoxanthin before HPLC separation. The enhanced protocol is useful for obtaining high purity pigments for biochemical studies.

Journal ArticleDOI
TL;DR: Five phenolic acids identified from SC extracts demonstrated analgesic activity, facilitating the mechanistic studies of SC in the treatment of neurasthenia.

Journal ArticleDOI
TL;DR: The result shows that recrystallization method could apply to extract and purify lycopene from watermelon that would also be used as a natural colorant as well as value-added product.
Abstract: Lycopene was extraction, isolation and purification using recrystallization, column chromatography, and preparative thin layer chromatography (TLC) methods as well as degradation kinetics of lycopene were studied at refrigerated temperature and room temperature for 3 wk from watermelon. Higher lycopene degradation was observed at refrigerated temperature as compared to ambient temperature throughout the storage periods. The highest amount of lycopene retained in recrystallization (101.69 μg/g) followed by column chromatography (18.20 μg/g) and preparative TLC (15.57 μg/g). Color parameters, half-life time (t1/2 ), and color retention (%R) were dependent on extraction, isolation, and purification methods and storage life. Recrystallization and preparative TLC were followed by first order reaction model. Preparative TLC exhibited higher activation energy than did the recrystallization and column chromatography. Therefore, the result shows that recrystallization method could apply to extract and purify lycopene from watermelon that would also be used as a natural colorant as well as value-added product.

Journal ArticleDOI
TL;DR: L-Trp proved to be a good ligand using a common mobile phase in each case and the issue of involvement of the Cu(II) cation for the best performance of the two methods has been discussed with respect to the same mobile phase.
Abstract: A new chromatographic method has been developed for direct enantioresolution of (RS)-baclofen by ligand-exchange thin-layer chromatography (TLC) adopting two different approaches; (A) TLC plates were prepared by mixing the ligand exchange reagents (LER) with silica gel slurry and the chromatograms were developed with different achiral solvents or solvents having no chiral additive, and (B) the LER consisting of Cu(II)-L-amino acid complex was used as chiral mobile phase additive and the plain plates of silica gel having no chiral selector were used. Cu(II) acetate and four L-amino acids (namely, L-tryptophan, L-histidine, L-proline and L-phenylalanine) were used for the preparation of LERs. Spots were located by the use of iodine vapor. Effect of temperature and the mole ratio of Cu(II)-to-amino acid on enantioresolution were also studied. The results for the two methods have been compared, and the issue of involvement of the Cu(II) cation for the best performance of the two methods has been discussed with respect to the same mobile phase. L-Trp proved to be a good ligand using a common mobile phase in each case.

Journal ArticleDOI
TL;DR: The proposed HPTLC method showed good linearity, precision, accuracy, and high sensitivity, and may be applied in a routine quantification of RA, SIN, TMF, and EUP found in ethanol, 50% of ethanol and water extract of O. stamineus leaves.
Abstract: Context: Orthosiphon stamineus is a medicinal herb widely grown in Southeast Asia and tropical countries. It has been used traditionally as a diuretic, abdominal pain, kidney and bladder inflammation, gout, and hypertension. Aims: This study aims to develop and validate the high-performance thin layer chromatography (HPTLC) method for quantification of rosmarinic acid (RA), 3'-hydroxy-5,6,7,4'-tetramethoxyflavone (TMF), sinensitin (SIN) and eupatorin (EUP) found in ethanol, 50% ethanol and water extract of O. stamineus leaves. Materials and Methods: HPTLC method was conducted using an HPTLC system with a developed mobile phase system of toluene: ethyl acetate: formic acid (3:7:0.1) performed on precoated silica gel 60 F254 TLC plates. The method was validated based on linearity, accuracy, precision, limit of detection, limit of quantification (LOQ), and specificity, respectively. The detection of spots was observed at ultraviolet 254 nm and 366 nm. Results: The linearity of RA, TMF, SIN, and EUP were obtained between 10 and 100 ng/spot with high correlation coefficient value (R2) of more than 0.986. The limit of detection was found to be 122.47 ± 3.95 (RA), 43.38 ± 0.79 (SIN), 17.26 ± 1.16 (TMF), and 46.80 ± 1.33 ng/spot (EUP), respectively. Whereas the LOQ was found to be 376.44 ± 6.70 (RA), 131.45 ± 2.39 (SIN), 52.30 ± 2.01 (TMF), and 141.82 ± 1.58 ng/spot (EUP), respectively. Conclusion: The proposed method showed good linearity, precision, accuracy, and high sensitivity. Hence, it may be applied in a routine quantification of RA, SIN, TMF, and EUP found in ethanol, 50% of ethanol and water extract of O. stamineus leaves.

Journal ArticleDOI
TL;DR: An efficient, fast, and reliable reversed phase high-performance liquid chromatography based method was developed to detect specific adulterant in premium and pure ghee (clarified butterfat) samples as discussed by the authors.
Abstract: An efficient, fast, and reliable reversed phase high-performance liquid chromatography based method was developed to detect specific adulterant in premium and pure ghee (clarified butterfat) samples. The method is based on the detection of cholesterol and β-sitosterol as markers in the unsaponifiable matter of pure ghee and adulterated ghee samples, respectively. The reversed phase high-performance liquid chromatography method resolved cholesterol, stigmasterol, campasterol, and β-sitosterol at Rt values of 17.681 ± 0.122, 19.7 ± 0.2, 20.2 ± 0.2, and 22.7 ± 0.2 min., respectively. β-sitosterol served as an indicator for the adulteration in ghee by plant and specific adulterant oil at dose dependent manner (1–5 g/100 g of ghee). Validation of the method revealed that it was fast, economical, highly reliable, and comparable with the reversed-phase thin layer chromatography method with no false negatives.

Journal ArticleDOI
TL;DR: In this paper, a simple two-step silica gel column chromatography was employed to separate the DON mycotoxin from wheat culture, combined with preparative high performance liquid chromatography (preparative HPLC) to purify the compound.

Journal ArticleDOI
TL;DR: Thin-layer chromatography (TLC) method for the separation and quantitative determination of seven related compounds has been developed and the applicability of the method was checked by screening of extracts of green, black, oolong, white tea and tea cultivars leaves.

Journal ArticleDOI
TL;DR: The described approach increases the desorption/ionization efficiencies of analytes separated by TLC, prevent spot blurring, simplifies and decrease time for sample preparation.

Journal ArticleDOI
TL;DR: The new mode of two-dimensional gradient thin layer chromatography (MGD-2D TLC) has been presented and it has been observed that application of the latter mode leads to almost triplicated number of zones in comparison with the former one.
Abstract: The new mode of two-dimensional gradient thin layer chromatography (MGD-2D TLC) has been presented. Short distance development of sample in the first dimension leads to formation of the preconcentrated narrow zones. They are consecutively separated in the second dimension with the mobile phase gradient in several steps of development until the eluent reaches the further end of the chromatographic plate. The use of the above-mentioned technique allows isolating and then identifying the compounds of various polarity from the multicomponent mixture. The practical application of two-dimensional gradient thin layer chromatography has been performed for isolation of the two plant (Juniperus and Thymus) oils components as the examples of test mixtures. The experiments have been carried out with the use of silica gel plates as well as a normal phase condition. The results of solute separation with isocratic one-dimensional thin layer chromatography system have been compared with those of two-dimensional gradient system. It has been observed that application of the latter mode leads to almost triplicated number of zones in comparison with the former one. It is purposeful to apply the proposed mode to control the purity of the dominant component or components of the mixture.

Journal ArticleDOI
TL;DR: In this paper, seven Scutellaria species were analyzed using the extraction procedure (Soxhlet apparatus, dichloromethane, and methanol as solvents) and thin-layer chromatography method.
Abstract: Seven different Scutellaria species were analyzed using the extraction procedure (Soxhlet apparatus, dichloromethane, and methanol as solvents) and thin-layer chromatography method. Selected standards of flavonoids and phenolic acids (caffeic acid, chlorogenic acid, ferulic acid, baicalein, wogonin, baicalin, chrysin, quercetin, scutellarin, hesperetin, hesperidin, apigenin, luteolin, rutin, and kaempferol) were separated using silica gel thin-layer chromatography (TLC) plates with the mobile phase consisting of ethyl acetate—toluene—formic acid (5:4.9:0.1, v/v) for dichloromethane and methanolic extracts. Dichloromethane extracts were also developed using cyanopropyl-bonded silica gel with the following mobile phases: propan-2-ol—n-heptane—formic acid (5:4.9:0.1, v/v) and methanol—water—formic acid (6:3.9:0.1, v/v), and after drying, they were sprayed using the anisaldehyde reagent. In the case of methanolic extracts, the same non-aqueous eluent was used and the aqueous eluent consisting of methanol—wate...

Journal ArticleDOI
TL;DR: This TLC@UV method is shown to be suitable for the refined kinetic analysis of different reactions related to the hydrolysis of sugars and validated according to ICH guidelines Q2(R1) in terms of specificity, limits of detection and quantification, precision and robustness.

Journal ArticleDOI
TL;DR: Two stability-indicating chromatographic methods have been developed and validated for determination of flecainide acetate in the presence of its degradation products (flecainides impurities; B and D) and applied for bulk powder and dosage form.
Abstract: In this work, two stability-indicating chromatographic methods have been developed and validated for determination of flecainide acetate (an antiarrhythmic drug) in the presence of its degradation products (flecainide impurities; B and D). Flecainide acetate was subjected to a stress stability study including acid, alkali, oxidative, photolytic and thermal degradation. The suggested chromatographic methods included the use of thin layer chromatography (TLC-densitometry) and high-performance liquid chromatography (HPLC). The TLC method employed aluminum TLC plates precoated with silica gel G.F254 as the stationary phase and methanol-ethyl acetate-33% ammonia (3:7:0.3, by volume) as the mobile phase. The chromatograms were scanned at 290 nm and visualized in daylight by the aid of iodine vapor. The developed HPLC method used a RP-C18 column with isocratic elution. Separation was achieved using a mobile phase composed of phosphate buffer pH 3.3-acetonitrile-triethylamine (53:47:0.03, by volume) at a flow rate of 1.0 mL/min and UV detection at 292 nm. Factors affecting the efficiency of HPLC method have been studied carefully to reach the optimum conditions for separation. The developed methods were validated according to the International Conference on Harmonization guidelines and were applied for bulk powder and dosage form. Copyright © 2016 John Wiley & Sons, Ltd.

Journal ArticleDOI
TL;DR: Combination of TLC with LD-IMS technique offers additional separation dimension, allowing separation of overlapping TLC analytes, and fast and effective analysis of the mixtures is possible with the proposed method.

Journal ArticleDOI
TL;DR: In this article, a chiral inducing reagent (CIR) was used in thin-layer chromatography (TLC) for enantioresolution of (±)-etodolac.
Abstract: Direct enantioresolution of (±)-etodolac has been achieved by adopting a new conceptual approach involving both achiral phases in thin-layer chromatography (TLC). Enantiomerically pure l-tryptophan, l-phenyl alanine, l-histidine, and l-arginine were used as chiral inducing reagents (CIR); none of these was impregnated with silica gel (while making TLC plates) or mixed with the mobile phase. The solvent system MeCN—CH2Cl2—MeOH, in different proportions, was found to be successful for enantioresolution. Spots were located in iodine chamber. Effect of concentration of chiral inducing reagent and temperature on enantioresolution was studied.

Journal ArticleDOI
TL;DR: It is proved, that due to different characteristic of adsorbents used in both techniques (RP HPLC and HPTLC), influence of ion-pairing reagents on retention of basic and/or amphoteric compounds also may be quite different.

Journal ArticleDOI
TL;DR: In this paper, a core consisting of hyperbranched poly(ethyleneimine) core surrounded by oligosaccharide shell (PEI-OS) was used as a component of the stationary phase in HPTLC for the separation of water-soluble vitamins, amino acids, and chiral β-blocker enantiomers.
Abstract: Impregnation of a stationary phase by organic and inorganic agents in high-performance thin-layer chromatography (HPTLC) may result in higher separation selectivity and resolution. This work is devoted to the application of novel core—shell polymers consisting of hyperbranched (poly(ethyleneimine)) core surrounded by oligosaccharide shell (PEI-OS) as a component of silica stationary phase in HPTLC for the separation of water-soluble vitamins, amino acids, and chiral β-blocker enantiomers. The influence of polymer structure (degree of substitution of PEI terminal amino groups with oligosaccharides and molecular weight of dendritic core [5 or 25 kDa]) as well as the content of PEI-OS in the stationary phase and a method of modification of the stationary phase on the efficiency of vitamin and amino acid determination and on the enantioselectivity factors of β-blockers separation were investigated. It was established that such polymers can be used as modifying agents of HPTLC systems for on-line preconcentration of vitamins (B2) and amino acids (lysine, tryptophan, and glutamic acids). These polymers can also be recommended as chiral selectors for the effective TLC separation of β-blockers.

Journal ArticleDOI
TL;DR: In this paper, different solvent extracts of Dichotomaria obtusata (J. Ellis & Solander) Lamark, a red algae collected from the coast of Bushehr in the Persain Gulf, were investigated for its cytotoxic properties and chemical constituents.
Abstract: Different solvent extracts of Dichotomaria obtusata (J. Ellis & Solander) Lamark, Galaxauraceae, a red algae collected from the coast of Bushehr in the Persain Gulf, was investigated for its cytotoxic properties and chemical constituents. The fresh alga, after extraction with methanol and dichloromethane were combined and partitioned between water, dichloromethane and ethyl acetate. The above fractions were then tested against MOLT-4 (human lymphoblastic leukemia) cancer cell line. The IC 50 values of the dichloromethane and ethyl acetate layers of the crude extract were 29.8 ± 3.1 and 30.6 ± 7.9 μg/ml against MOLT-4 cells, respectively, while the water layer showed a week activity with IC 50 > 50 μg/ml. After fractionation of the active extracts using open column chromatography over silica gel and preparative thin layer chromatography purification, two terpenoid derived compounds, trans -phytol palmitate and γ-tocopherol were isolated from the dichloromethane and ethyl acetate extracts. The structures of the compounds were elucidated using different spectral data including 1 H NMR, 13 C NMR, HSQC, HMBC and EI-MS. The IC 50 values of compounds trans -phytol palmitate, γ-tocopherol and an undetermined mixture of compounds (F-13-14) were determined as 43.4 ± 1.6, – and 20.3 ± 6.2 μg/ml against LS180 (human colon adenocarcinoma); 53.2 ± 9.3, >100 and 27.6 ± 6.9 μg/ml against MCF-7 (human breast adenocarcinoma) and 40.0 ± 4.1, 48.8 ± 1.8 and 15.9 ± 0.3 μg/ml against MOLT-4 cell lines, respectively, which were comparable to the IC 50 values of standard anticancer agent, cisplatin against the same cell lines. The red algae collected from the Persian Gulf contained substances that could inhibit the growth of human cancer cell lines and may represent a natural source for the discovery of novel anticancer agents.