[Quality evaluation of Psoraleae Fructus based on QAMS method and TLC identification].

The present study established a determination method of Psoraleae Fructus by quantitative analysis of multi-components by the single marker(QAMS) and further improved the thin-layer chromatography(TLC) method. The QAMS method was established by UPLC with psoralen as the internal marker, and the content of psoralenoside, isopsoralenoside, psoralen, and isopsoralen was simultaneously determined. As revealed by the comparison with results of the external standard method, the QAMS method was accurate and feasible. According to the current quality standards of Psoraleae Fructus, the TLC method was further optimized and improved, and bakuchiol was added for identification based on the original TLC method with psoralen and isopsoralen as indicators. This study provides a reference for improving the quality control method of Psoraleae Fructus.

[Recommendations on quality standards of Andrographis Herba and its processed slices in Chinese Pharmacopoeia (2020 edition)].

To improve and perfect the quality standards and propose recommendations for the revision of quality standards for Andrographis Herba and its processed slices in Chinese Pharmacopoeia(ChP)(2020 edition) based on the problems and limitations in ChP(2015 edition). TLC identification method with andrographolide and control herbs as references was established using silica gel G thin layer plate, with chloroform-methylbenzene-methanol(8∶1∶1) as developing solvent, and 10% sulfuric acid ethanol solution as colour-developing agent. This method has good reproducibility, strong specificity and high sensitivity. As compared with the original method in ChP 2015, this method has better development effect and clearer spots. Based on the previous research, a quantitative analysis of multi-components by single-marker(QAMS) method with andrographolide as the internal reference substance was developed to simultaneously determine the contents of 4 diterpene lactones: andrographolide(S), neoandrographolide(A), 14-deoxyandrographolide(B), and dehydroandrographolide(C). The relative correction factors of f_(A/S), f_(B/S), and f_(C/S) were determined as 1.12, 0.79, and 0.63, respectively. The relative retention time of t_(A/S), t_(B/S), and t_(C/S) was 1.95, 2.18, and 2.25, respectively. According to the content determination results in 46 batches of crude drugs and 38 batches of processed slices, it was stipulated that the total contents of 4 diterpene lactones should not be less than 1.5% and 1.2% in crude drugs and processed slices, respectively. As compared with the original method in ChP 2015, the present QAMS method could not only reduce the detection cost and improve the efficiency, but also can be used to evaluate the quality of Andrographis Herba and its processed slices more comprehensively and objectively. Diterpene lactones are generally recognized as the effective components in Andrographis Herba, and their contents in leaves were much higher than those in stems. However, almost all of the current commercial processed slices are processed from stems, so their quality is gene-rally poor and the efficacy is hard to be guaranteed. Therefore, the weight percentage of leaves should be added into the inspection items of the processed slices and it should not be less than 25%.

[Study on revision of quality standard of Sophorae Flavescentis Radix and its processed slices].

Sophorae Flavescentis Radix is prepared from the root of Sophora flavescens. The comprehensive knowledge of the effective components in S. flavescens makes its quality standard improvement more possible. TLC identification method for main flavonoids and alkaloids in one test was established using GF_(254) thin layer plate and the lower solution of chloroform-methanol-water-formic acid(4∶2∶1∶0.6) as developing solvent. The quantitative method of marker alkaloids was revised including the simplified sample preparation procedure and the chromatographic conditions. The determination of four alkaloids in the samples indicated that 32 batches of tested samples were qualified ones. The total oxymatrine and matrine, total oxysophocarpine and sophocarpine, as well as total amount of four tested components in the different samples were 1.08%-2.55%, 0.369%-0.860%, 1.67%-3.40%, respectively. There was a significantly positive correlation between oxymatrine and oxysophocarpine. Total oxymatrine and matrine had same correlation with total oxysophocarpine and sophocarpine. The moisture content and extractive in 32 batches of samples fulfilled the require of not more than 11.0% and not less than 20.0%, respectively. Thirteen tested pesticides were not detected in 12 batches of samples. The present study provided the evidence for the revision of quality standard of Sophora Flavescentis Radix.

[Improvement researches on quality standard of Anemarrhenae Rhizoma and its raw processed products].

This study is to improve the quality standard and supply the scientific basis for Anemarrhenae Rhizoma and its raw processed products. Steroidal saponin including timosaponin BⅡ, timosaponin AⅢ and flavonoids including neomangiferin and mangiferin were selected as the indicative components. Silica gel G thin layer chromatography(TLC) and polyamide TLC were used to detect the two types of compounds, respectively. The contents of timosaponin BⅡ and timosaponin AⅢ were determined by HPLC-ELSD and the content of neomangiferin, mangiferin and isomangiferin were determined by HPLC-UV. Moisture, total ash and acid insoluble ash were determined according to Chinese Pharmacopoeia(2015 edition). And 80% ethanol was selected as the solvent and the content determination of total extract were determined. The fingerprints of Anemarrhenae Rhizoma and its raw processed products were established by HPLC-UV and HPLC-ELSD. The results showed that the methods of TLC and HPLC have been successfully stablished. There are 2 and 3 peaks which have been identified by HPLC-ELSD and HPLC-UV, respectively. The HPLC fingerprint methods are specific and can be used to identify and quality control for Anemarrhenae Rhizoma and its raw processed products in the mass. Comparing to Chinese Pharmacopoeia(2015 edition), the TLC identification and content determination were revised and the total extract determination and HPLC fingerprints were added in the present study. Our results can be used as the scientific basis of quqlity control for Anemarrhenae Rhizoma and its raw processed products.

Improvement researches on quality standard of Anemarrhenae Rhizoma and its raw processed products / 中国中药杂志

This study is to improve the quality standard and supply the scientific basis for Anemarrhenae Rhizoma and its raw processed products. Steroidal saponin including timosaponin BⅡ, timosaponin AⅢ and flavonoids including neomangiferin and mangiferin were selected as the indicative components. Silica gel G thin layer chromatography(TLC) and polyamide TLC were used to detect the two types of compounds, respectively. The contents of timosaponin BⅡ and timosaponin AⅢ were determined by HPLC-ELSD and the content of neomangiferin, mangiferin and isomangiferin were determined by HPLC-UV. Moisture, total ash and acid insoluble ash were determined according to Chinese Pharmacopoeia(2015 edition). And 80% ethanol was selected as the solvent and the content determination of total extract were determined. The fingerprints of Anemarrhenae Rhizoma and its raw processed products were established by HPLC-UV and HPLC-ELSD. The results showed that the methods of TLC and HPLC have been successfully stablished. There are 2 and 3 peaks which have been identified by HPLC-ELSD and HPLC-UV, respectively. The HPLC fingerprint methods are specific and can be used to identify and quality control for Anemarrhenae Rhizoma and its raw processed products in the mass. Comparing to Chinese Pharmacopoeia(2015 edition), the TLC identification and content determination were revised and the total extract determination and HPLC fingerprints were added in the present study. Our results can be used as the scientific basis of quqlity control for Anemarrhenae Rhizoma and its raw processed products.

Improvement of Identification Method （3）of Isatis indigotica from 2015 Edition of Chinese Pharmacopeia （PartⅠ） / 中国药房

OBJECTIVE： To investigate the rationality of TLC identification method （3） of （R，S）-epigoitrin in Isatis indigotica stated in 2015 edition of Chinese Pharmacopeia （partⅠ） （later abbreviated as pharmacopeia）， and make some improvements. METHODS： Three batches I. indigotica were collected and prepared into decoction pieces according to the processing method of I. indigotica in pharmacopoeia. TLC identification of （R，S）-goitrin in I. indigotica decoction piece and medicinal material were conducted according to identification method （3） in pharmacopeia （80％ ethanol as solvent for sample treatment， ultrasound extraction）； the rationality of pharmacopoeia method was investigated. Then the method was improved by changing the extraction solvent and pretreatment method （method one： using water as solvent， ultrasound extraction； method two： soaking in water for 1 h， then adding into methanol， ultrasound extraction； method three： the sample was wetted and then dried， using 80％ methanol as solvent， ultrasound extraction） of samples， and the optimal method was verified. According to the optimal method， the TLC identification of （R，S）-goitrin was detected by using chromatographic plates from different manufacturers， under the conditions of low temperature and low humidity （7 ℃， relative humidity 48％） and high temperature and high humidity （35 ℃， relative humidity 75％） respectively，to investigate the durability of the method. RESULTS： According to the method of pharmacopeia， in the chromatograms of decoction pieces， the same color spots appeared at the corresponding chromatographic positions of reference substance， but no corresponding spots appeared in the medicinal material chromatograms. After the samples were treated by three improvement methods， in medicinal material chromatograms， the same color spots appeared in the corresponding chromatographic positions of reference substances. There were single chromatographic spot after medicinal materials were treated with method one， and there were more spots after medicinal materials were treated with method two and three， and method two consumed less time than method three. The results of validation tests and method durability tests  showed that after the treatment of I. indigotica and its decoction pieces according to method two， the same color spots appeared in the corresponding positions of the decoction pieces and the medicinal materials chromatograms as those of the control. CONCLUSIONS： The improved TLC identification method is effective， the chromatographic spots are clear， and the repeatability is good.

Study on Quality Standard of Mongolia Medicine Sabina vulgaris / 中国药房

OBJECTIVE： To establish the quality standard of Sabina vulgaris， and to provide reference for its quality control. METHODS： Totally 9 batches of S. vulgaris were collected from Inner Mongolia area. The characteristics of S. vulgaris samples were observed and microscopic identification was conducted for the transverse section and powder of its branches and leaves. TLC was used for qualitative analysis of S. vulgaris. The contents of water， total ash， acid-insoluble ash and alcohol-soluble extract in S. vulgaris were determined according to the method stated in 2015 edition of Chinese Pharmacopeia （part Ⅳ）. The contents of quercetin and amentoflavone in S. vulgaris were determined by HPLC. RESULTS： The branchlets of S. vulgaris were cylindrical or rhombic， with varying length of thorns， dark green or yellowish green. The microscopic observation showed that the epidermal cells of scale leaves were arranged orderly； there were larger cavities in the middle of scale leaves， large cells in spongy tissue； epidermal cells were rectangular with more stomata and large guard cells. Results of TLC showed that the spots of the same color were found in the corresponding positions of chromatogram for substance control （dendrooside and rutin）. In the 9 batch of samples， the contents of water were 3.2％-5.6％； the contents of total ash were 3.4％-5.8％； the contents of acid-insoluble ash were lower than 0.8％； the contents of alcohol-soluble extract were 28.0％-33.8％； the contents of quercetin were 0.11％-0.28％； the contents of amentoflavone were 0.15％-0.25％. CONCLUSIONS： It is preliminarily proposed that the content of water in S. vulgaris is not more than 8.0％； the content of total ash is not more than 7.0％； the content of alcohol-soluble extract is not less than 24.0％； the content of quercetin is not less than 0.11％； the content of amentoflavone is not less than 0.15％. Established standard can be used for the quality control of S. vulgaris.

Study on Qualitative and Quantitative Analysis of Zhendian Kaiqiao Granules / 中国中医药信息杂志

Objective To establish a method for qualitative and quantitative analysis of Zhendian Kaiqiao Granules. Methods Gentiane Radix et Rhizoma, Scuteliariae Radix, Rhei Radix et Rhizoma, Radices Paeoniae Alba in the preparation were identified by TLC. Gentiopicrin and paeoniflorin were determined by HPLC. The analysis was performed on a Phenomenex C18 column (250 mm × 4.6 mm, 5 μm), with the mobile phase of methyl alcohol-water (12:88). The flow rate was 1.0 mL/min and the column temperature was maintained at room temperature; the detection wavelengths were set at 273 nm (gentiopicrin) and 230 nm (paeoniflorin). Results Gentiane Radix et Rhizoma, Scuteliariae Radix, Rhei Radix et Rhizoma, Radices Paeoniae Alba could be detected by TLC. Gentiopicrin showed a good linear relationship at a range of 2.396–11.980 μg, r=0.999 6. The average recovery was 99.72%, and RSD was 2.70%. Paeoniflorin showed a good linear relationship at a range of 2.728–13.640 μg, r=0.999 0. The average recovery was 98.74%, and RSD was 2.42%. Conclusion The established method is simple, reliable and reproductive.The method can be used for control quality of Zhendian Kaiqiao Granules.

Research on Quality Standards of Granati Pericarpium and Granati Semen / 世界科学技术-中医药现代化

This study was aimed to establish quality standards of Granati pericarpium and Granati semen. The microscopy and thin layer chromatography (TLC) were used in the identification of Granati semen. According to the 2010 Chinese Pharmacopoeia, the content of moisture, total ash, acid-insoluble ash and alcohol-soluble extract were determined. And the HPLC was used in the content determination of ellagic acid in Granati semen and Granati pericarpium. The results showed that the microscopic characteristics of Granati semen were identified. And TLC identification of Granati semen was established. The content determination method of ellagic acid in Granati pericarpium and Granati semen were established. It was concluded that the established qualitative and quantitative method can be used for quality control of Granati pericarpium and Granati semen.

Methodological Research on TLC Identification of Radix Mirabilis himalaica / 世界科学技术-中医药现代化

This study was aimed to establish the TLC identification method of Radix Mirab ilis himalaic a. The β-sitosterol and daucosterol were used as the reference substances. The single-factor test was used. A variety of factors which affected TLC were systematically investigated to filter out the best TLC conditions for identification of different batches of medicines. The results showed that the best TLC conditions were as follows: silica gel G plates, extraction solvent (methanol), reagent (5% sulfuric acid in ethanol), extraction method (ultrasonic extraction with methanol), ex-tracted time (30 min), the agent (petroleum ether-ethyl acetate-acetone (5:2:1)) and sample volume (6 μL). It was concluded that the method, which had high separation degree, was reproducible and simple. It can be used as the quality control of Radix Mirab ilis himalaic a.

Pharmacognostical Study on Castanea Mollissima Blume Shell / 世界科学技术-中医药现代化

This study was aimed to offer a scientific basis for the differentiation and control quality of Castanea mol-lissima Blume shell. The determination was given from the morphological identification, microscopical identification and TLC identification. The results showed that through obtained information such as morphological traits, tissue powder and TLC characteristics, the longitudinal section micrographs of C. mollissima Blume shell and the micro-scopic images of tissue powder had been received. It was concluded that the study provided a reliable reference for the identification of the quality control standards of C. mollissima Blume shell.

Pharmacognostic study on Ficus hirta / 中草药

Objective: To clarify the origin of Ficus hirta and to control the quality of the crude drug. Methods: The reference on F. hirta, the microscopic features of powder and tissue of the crude drug, plant morphology, and phytochemical TLC were observed and studied. Results: The result of study provides the using history and experiment research of F. hirta and characteristics of the crude drug, which could be used for the identification of the crude drug and Chinese patent medicine. Conclusion: The convenient and effective method for identification of crude drug and patent drug has been established, which provides the basis for quality control.

Study on quality standards of Huoxue Zhitong Preparations / 中国药学杂志

OBJECTIVE: To improve the quality standards of Huoxue Zhitong Powders and Huoxue Zhitong Capsules. METHODS: Angelicae Sinensis Radix, Olibanum and Borneolum Syntheticum were identified simultaneously by TLC method. Ferulic acid was detected by HPLC method. RESULTS: Clear spots were obtained with good separation in TLC identification. For the HPLC determination of ferulic acid, the calibration curve was linear in the range of 0.2-200 μg · mL-1, the limit of detection was 0.054 μg · mL-1 and recoveries were between 95%-105%. CONCLUSION: The proposed method is specific, accurate, simple and applicable for better control of Huoxue Zhitong Preparations' quality.

Study on TLC Identification and Content Determination of Compound Yantongxiao Spray / 中药新药与临床药理

Objective To establish the methods for TLC identification and contents determination of Compound Yantongxiao Spray.Methods Flos Lonicera,Borneolum Syntheticum and Menthol in the spray were identified by TLC,and the content of chlorogenic acid was determined by HPLC.Results The TLC characteristic spots of Flos Lonicera,Borneolum Syntheticum and Menthol can be identified.For content determination,the linear range of chlorogenic acid was in 0.08～0.28 ?g(r=0.999 0),the average recovery of chlorogenic acid was 102.34 %(n=6)and RSD was 2.03 %.Conclusions The methods are simple,accurate,specific and reproducible,can be used for the quality control of Compound Yantongxiao Spray.

Study on Quality Control Method for Renshensinitang Oral Liquid(Radix Ginseng,Radix Aconiti Praeparata,etc.) / 中成药

This paper reported TLC identification of various Chinese medicines in Renshensinitang Oral Liq- uid,limit dose detection and content determination of aconitine.These methods could be available for internal quality control of Renshensinitang Oral Liquid.