牡丹与芍药中活性成分的动态研究

前文报道了芍药甙类和丹皮酚类成分在芍药科植物中的存在,本文在此工作的基础上又测定了不同时间采集的牡丹Paeonia suffrutieosa和芍药P.lactiflora根中芍药甙(paeonif-     

Box-Behnken supported validation of stability-indicating high performance thin-layer chromatography (HPTLC) method: An application in degradation kinetic profiling of ropinirole

Stability-indicating high-performance thin-layer chromatographic (HPTLC) method for the analysis of ropinirole HCl was developed and validated as per the ICH guidelines. The method employed the mobile phase and toluene-ethyl acetate-6 M ammonia solution (5:6:0.5, v/v/v) was optimized with the help of a design expert. Densitometric analysis of ropinirole HCl was carried out in the absorbance mode at 250 and 254 nm. Compact spots for ropinirole HCl were found at R_f value of 0.58 ± 0.02. The linear regression analysis data for the calibration plots showed R² = 0.9989 ± 0.0053 with a concentration range of 100–3000 ng spot⁻¹. The method was validated for precision, accuracy, ruggedness, robustness, specificity, recovery, limit of detection (LOD) and limit of quantitation (LOQ). The LOD and LOQ were 12.95 and 39.25 ng spot⁻¹ respectively. Drug was subjected to acidic, alkaline, oxidative, dry heat, wet heat and photo degradation stress. All the peaks of degradation products were well resolved from the standard drug peak with significant difference of R_f. The acidic and alkaline stress degradation kinetics of ropinirole, were found to be in first order, showing high stability (t_1/2, 146.37 h⁻¹; t_0.9, 39.11 h⁻¹) in the acidic medium and low stability (t_1/2, 97.67 h⁻¹; t_0.9, 14.87 h⁻¹) in the alkaline environment.     

Integrative approaches for unmasking hidden species in herbal dietary supplement products: What is in the capsule?

Herbal dietary supplement products are often marketed as herbal mixtures, which makes quality control processes difficult. Herein, paired-end next-generation sequencing (NGS), microscopic examination and high-performance thin layer chromatography (HPTLC) were integrated to unveil herbal ingredient compositions in a selected herbal dietary supplement product. The product was labeled as containing capsicum, cactus, wheat, white bean, Garcinia cambogia, psyllium husk and black pepper in each capsule. A laboratory-made sample was prepared as a reference sample according to the product label. NGS indicated that six out of the seven herbal species were detected in the laboratory-made sample, while 97.02 ± 0.15% of sequencing reads from the commercial product belonged to Senna alexandrina. Microscopic examination also confirmed the presence of Senna. Similar chemical constituents of the product and Senna powder were observed by HPTLC patterns. Surprisingly, there was a distinct band difference between samples. After extraction and LC-MS/MS analysis, oleamide was found as an adulterant in the product. None of the plants listed on the commercial product label were detected by any of the methods. Therefore, the integrative approaches successfully unmasked nonlisted herbal species in a selected herbal dietary supplement product. These approaches should be applied to other dietary supplement products for registration and regulation processes.     

固定化介导提高苦味叶下珠中的海冰叶下珠脂素和叶下珠次素的含量(英文)

Phyllanthus amarus plant is used in the traditional system of medicine as a hepatoprotective drug for which the majorlignans phyllanthin and hypophyllanthin are responsible.So far,no significant work has been done on the culture of this plant.Realizingthe hepatoprotective potential,the present investigation was undertaken.A cost effective process was developed for enhancingphyllanthin and hypophyllanthin utilizing the immobilization technique.HPTLC was used to compare the phyllanthin and hypophyllanthincontents in calcium alginate immobilized cells obtained from fresh grown plants and MS medium was supplemented withdifferent abiotic elicitors,under aseptic conditions for the treatment with chitosan,copper sulphate,phenylalanine and silver nitratesolution to make the whole process commercially viable.It was revealed that silver nitrate and phenylalanine at low concentrationenhances phyllanthin and hypophyllanthin yield as compared to control immobilized cell culture.The study revealed that an increase inthe content of phyllanthin and hypophyllanthin was elicitor concentration dependent and silver nitrate treatment gave a maximum yieldof hepatoprotective bioactives as compared to the other abiotic elicitors used.     

四级杆飞行时间串联质谱(QTofMS)辅助高效薄层色谱(HPTLC)鉴别乳香中乳香酸

 目的 建立薄层色谱法鉴别乳香中乳香酸类成分。方法 样品经甲醇超声提取,C₁₈固相萃取柱净化后,点样于硅胶GF₂₅₄高效预制薄层板上,以甲苯-乙酸乙酯-庚烷-无水甲酸（8∶2∶1∶0.3）为展开剂展开,先置紫外灯（254 nm）下检视,再喷以10%硫酸乙醇溶液,并于105 ℃加热至条斑清晰,置紫外灯（365 nm）下检视。条斑借助QTofMS进行成分识别。结果 紫外灯（254 nm）下,埃塞俄比亚乳香和索马里乳香的色谱均可见2个明显的暗条斑,紫外灯（365 nm）下,均可见8个荧光条斑,其特征图谱与其他常见树脂类药材（洋乳香、天然没药、胶质没药、安息香、松香和达玛树脂）区别明显。结论 该法简便、专属、准确,适用于乳香的快速鉴别和质量控制。     

Effective separation and analysis of E- and Z-guggulsterones in Commiphora mukul resin, guggulipid and their pharmaceutical product by high performance thin-layer chromatography-densitometric method

A high performance thin-layer chromatographic (HPTLC) method for the simultaneous determination of the hypolipidemic agents, E- and Z-isomers of guggulsterone in Commiphora mukul resin, guggulipid (ethyl acetate extract of resin), and its pharmaceutical formulation, was developed. The developed system was efficient enough to separate both isomers from their conger, 17,20-dihydroguggulsterone (3). HPTLC glass plates, pre-coated with silica gel 60F-254, were used as a stationary phase. The mobile phase consisted of toluene:acetone (9.3:0.7, v/v) which gave well resolved spots for E- and Z-guggulsterones (R_f: 0.52 ± 0.01, and 0.67 ± 0.01, respectively) following double development of chromatoplate with the same mobile phase under unsaturated conditions. The analyte stability towards the developed chromatographic procedure was also investigated by two-dimensional (2D) HPTLC analysis. 17,20-Dihydroguggulsterone (3) was identified by the electrospray ionization quadrupole time-of-flight tandem mass spectrometry (ESI-QTOF-MS/MS) analysis.     

Isolation and Characterization of Antineoplastic Alkaloids from Catharanthus Roseus L. Don. Cultivated in Egypt

Vinblastine and vincristine (the antileukemic agents) were isolated, in a pure form, from Catharanthus roseus L. Don., cultivated in Egypt, by several chromatographic techniques. Five modified methods for the preparation of total alkaloids were carried out. All the isolated mixtures were evaluated by HPLC and HPTLC analyses. The antineoplastic alkaloids; vinblastine and vincristine, were isolated by the use of vacuum liquid chromatographic column on silica gel : aluminium oxide (1:1) mixed bed vacuum liquid chromatography (VLC), Charcoal column, and finally purified by centrifugally accelerated radial chromatography (Chromatotrone).     

Pharmacokinetic Study of a Novel Antihyperlipidemic Agent LM-13765- A Prodrug

A sensitive and specific high performance thin layer chromatographic method has been developed for estimation of a novel antihyperlipidemic agent LM 13765 in rabbit plasma and its use for pharmacokinetic study has been evaluated. The proposed method was employed to study pharmacokinetics of LM 13765 in rabbits. It was observed that LM 13765 metabolized immediately after oral administration. The metabolite of LM 13765 was identified and characterized as LM 13765-C. A sensitive and specific HPTLC method was developed for estimation of LM 13765-C in plasma after oral administration of LM 13765 and pharmacokinetic parameters were determined. Biological screening of LM 13765-C on hyperlipidemic rats indicated that it is less potent than the parent compound which is indicative of biotransformation of LM 13765 to active form LM 13765-C.     

高效薄层荧光光密度法测定生物样品中的小檗碱含量

建立了高效薄层荧光光密度法测定生物样品中小檗碱的含量,并比较了口服小檗碱(100mg/kg)及含等量小檗碱的黄连粉(2 g/kg)后的血药浓度、降血糖效应和组织分布。     

HPTLC method for simultaneous determination of ascorbic acid and gallic acid biomarker from freeze dry pomegranate juice and herbal formulation

A new rapid, simple, sensitive and high performance thin layer chromatography (HPTLC) has been established for the simultaneous determination of ascorbic acid and gallic acid in the freeze-dried pomegranate fruit juice and herbal formulation. HPTLC method was carried out using ethyl acetate: acetone: water: formic acid, 10:6:2:2 (%, v/v/v/v)) on 20 × 10 cm glass coated silica gel 60 F₂₅₄ plates and scanned at 254 nm for ascorbic acid and gallic acid. Ascorbic acid and gallic acid in the freeze-dried pomegranate fruit juice were identified by comparing their single spot at R_f = 0.54 ± 0.02 and R_f = 0.83 ± 0.01 respectively. The value of regression equation (r² ≥ 0.9992) revealed a good linear relationship between peak area and amount of ascorbic acid and gallic acid in the range of 100–800 ng/band. The method was validated for precision, accuracy, robustness LOD and LOQ. The method proposed can be useful for routine determination of ascorbic acid and gallic acid in various crude as well as herbal formulations as a quality control tool.