Establishment of HPLC fingerprint and content determination of multiple index components in Xiao’er resuqing oral liquid / 中国药房

OBJECTIVE To establish an HPLC fingerprint of Xiao’er resuqing oral liquid， and to determine the contents of twelve index components. METHODS HPLC method was adopted. The determination was performed on Venusil MP C18 column with mobile phase consisting of acetonitrile-0.1% phosphate aqueous solution （gradient elution） at a flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm， the column temperature was 30 ℃， the injection volume was 10 μL. HPLC fingerprint of Xiao’er resuqing oral liquid was established by using the Similarity Evaluation System of Chromatographic Fingerprint of TCM （2012 edition） to evaluate the similarity. The contents of 12 components were determined， including （R， S）-goitrin， 3，5-O-dicaffeoyl quinic acid， puerarin， forsythin， forsythoside A， chlorogenic acid， baicalin， saikosaponins d， wogonoside， baicalein， emodin and chrysophanol. RESULTS The similarity of HPLC fingerprints of 13 batches of Xiao’er resuqing oral liquid was greater than 0.97， and 14 common peaks were confirmed. The contents of the above 12 index components in 13 batches of Xiao’er resuqing oral liquid were as follows： 0.078-0.172， 1.564-2.736， 1.338-2.578， 0.426-0.872， 1.477-2.628， 1.396-2.447， 4.052-9.146， 0.367- 0.692， 1.974-4.674， 1.274-2.969， 0.085-0.167 and 0.155-0.307 mg/mL. CONCLUSIONS The established HPLC fingerprint and content determination methods have high accuracy and high specificity， which can be used for the quality evaluation of Xiao’er resuqing oral liquid.

Improvement on Quality Standard of Yuanhu Zhitong Oral Liquid / 中国实验方剂学杂志

ObjectiveTo improve the quality standard of Yuanhu Zhitong oral liquid in order to strengthen the quality control of this oral liquid. MethodThin layer chromatography（TLC） was used for the qualitative identification of Corydalis Rhizoma and Angelicae Dahuricae Radix in Yuanhu Zhitong oral liquid by taking tetrahydropalmatine， corydaline reference substances and Corydalis Rhizoma reference medicinal materials as reference， and cyclohexane-trichloromethane-methanol（5∶3∶0.5） as developing solvent， Corydalis Rhizoma was identified using GF254 glass thin layer plate under ultraviolet light（365 nm）. And taking petroleum ether（60-90 ℃） -ether-formic acid（10∶10∶1） as developing solvent， Angelicae Dahuricae Radix was identified using a silica gel G TLC plate under ultraviolet light（305 nm）. High performance liquid chromatography（HPLC） was performed on a Waters XSelect HSS T3 column（4.6 mm×250 mm， 5 μm） with acetonitrile（A）-0.1% glacial acetic acid solution（adjusted pH to 6.1 by triethylamine）（B） as the mobile phase for gradient elution（0-10 min， 20%-30%A； 10-25 min， 30%-40%A； 25-40 min， 40%-50%A； 40-60 min， 50%-60%A）， the detection wavelength was set at 280 nm， then the fingerprint of Yuanhu Zhitong oral liquid was established， and the contents of tetrahydropalmatine and corydaline were determined. ResultIn the thin layer chromatograms， the corresponding spots of Yuanhu Zhitong oral liquid， the reference substances and reference medicinal materials were clear， with good separation and strong specificity. A total of 12 common peaks were identified in 10 batches of Yuanhu Zhitong oral liquid samples， and the peaks of berberine hydrochloride， dehydrocorydaline， glaucine， tetrahydropalmatine and corydaline. The similarities between the 10 batches of samples and the control fingerprint were all >0.90. The results of determination showed that the concentrations of corydaline and tetrahydropalmatine had good linearity with paek area in the range of 0.038 6-0.193 0， 0.034 0-0.170 0 g·L-1， respectively. The methodological investigation was qualified， and the contents of corydaline and tetrahydropalmatine in 10 batches of Yuanhu Zhitong oral liquid samples were 0.077 5-0.142 9、0.126 1-0.178 2 g·L-1， respectively. ConclusionThe established TLC， fingerprint and determination are simple， specific and reproducible， which can be used to improve the quality control standard of Yuanhu Zhitong oral liquid.

Research on Material Basis of Homologous and Heterogeneous Effect of Aurantii Fructus Immaturus and Aurantii Fructus Based on Total Statistical Moment Analysis and Molecular Connectivity Index / 中国实验方剂学杂志

ObjectiveTo investigate the material basis of homologous and heterogeneous effect of Aurantii Fructus Immaturus（AFI） and Aurantii Fructus（AF） based on the total statistical moment analysis and molecular connectivity index（MCI）. MethodRelevant literature at home and abroad and Traditional Chinese Medicine Systems Pharmacology Database and Analysis Platform（TCMSP） were consulted to establish the chemical composition database of AFI and AF， and set up their fingerprints by ultra-high performance liquid chromatography（UPLC）， and the total statistical moments and similarity parameters of the fingerprint were calculated. According to MCI， all components of AFI and AF were divided into different component groups， the average values of 0-8th order（0χ-8χ） MCI of the common component groups of AFI and AF were calculated. ResultThe values of total zero-order moment（AUCT） of AFI and AF were （10.57±2.45）×106， （5.09±0.89）×106 μV·s， the values of total first-order moment（MCRTT） were （11.57±1.58）， （12.10±1.29） min， the values of total second-order moments（VCRTT） were（24.49±2.30）， （26.49±2.54） min2， respectively. It showed that qualitative and quantitative parameters of AFI and AF were significantly different. The components with high similarity such as neohesperidin， hesperidin and narirutin were screened as the common potential pharmacodynamic components of AFI and AF. The non-common components of AFI， such as alysifolinone and imperatorin， and the non-common components of AF， such as neoeriocitrin and isosakuranin， with high similarity were screened out as potential heterogeneous components of AFI and AF. The composition groups of AFI and AF were classified into six categories， and the similarities between the composition groups of AFI and AF and the total constituents were 0.872-0.979 and 0.918-0.997， the average values of 0χ-8χ MCI of alkaloids in AFI and AF were 3.65 and 3.14， the average values of 0χ-8χ MCI of flavonoids were 8.47 and 8.47， the average values of 0χ-8χ MCI of volatile oils were 2.71 and 3.48， respectively. It showed that there were some differences in MCI of chemical constituents（groups） between AFI and AF. ConclusionThe chemical constituents（groups） of AFI and AF not only differ in content and species， but also in structural characteristics and structure-activity relationship， which can provide a basis for further explaining the scientific connotation of homologous and heterogeneous effect of AFI and AF.

Establishment of HPLC fingerprint and content determination of 8 components in Jianpi huayu decoction / 中国药房

OBJECTIVE To establish the HPLC fingerprint of Jianpi huayu decoction， and to determine the contents of 8 components. METHODS Thermo Hypersil Gold C18 column was used with mobile phase consisted of methanol-0.05% phosphoric acid aqueous solution （gradient elution） at the flow rate of 1.0 mL/min. The column temperature was 30 ℃， the injection volume was 5 μL. The detection wavelength of matrine was 211 nm， and the other components’ detection wavelength was 283 nm. The similarity evaluation of HPLC fingerprints for 10 batches of Jianpi huayu decoction was performed by using the Similarity Evaluation System of Chromatographic Fingerprint of Traditional Chinese Medicine （2012 edition）. The contents of chlorogenic acid， vanillic acid， p-coumaric acid， ferulic acid， hesperidin， quercetin， bergapten and matrine in the samples were determined by HPLC. RESULTS HPLC fingerprint of Jianpi huayu decoction was established. A total of 27 common peaks were identified， and 8 components were identified. The similarity between 10 batches of samples and the control map ranged from 0.942-0.999. RSDs of precision， repeatability and stability tests were less than 3% （n＝6）. The average recoveries of chlorogenic acid， vanillic acid， p-coumaric acid， ferulic acid， hesperidin， quercetin， bergapten and matrine were 99.48%， 101.32%， 101.18%， 100.79%， 101.12%， 99.19%， 99.81% and 102.46%， respectively； RSDs were 1.34%， 0.93%， 1.90%， 1.84%， 0.54%， 1.53%， 1.33% and 1.01%， respectively （n＝6）. The contents were 0.021-0.061， 0.025-0.034， 0.116-0.295， 0.006- 0.062， 0.014-0.053， 0.017-0.026， 0.014-0.027 and 14.05-24.11 mg/g， respectively. CONCLUSIONS The established fingerprint and content determination method can provide a reference for the quality control and subsequent preparation development for Jianpi huayu decoction.

HPLC fingerprint，content determination and transferring patterns of index components of Xintongshu spray / 中国药房

OBJECTIVE To establish the HPLC fingerprint of Xintongshu spray， determine the contents of identified components， and investigate the transferring patterns of the index components of decoction pieces， intermediates and spray， so as to provide scientific reference for technology management and quality control of Xintongshu spray. METHODS HPLC fingerprints of 13 batches of Xintongshu spray were established by the Similarity Evaluation System for Chromatographic Fingerprints of TCM （2012 edition）， and common peaks were identified； the contents of identified components were determined by HPLC. The paeonol in Moutan Cortex and ferulic acid in Chuanxiong Rhizoma were used as index components to investigate the transferring patterns of them in decoction pieces， intermediates and spray. RESULTS There were a total of 33 common peaks in the fingerprints of 13 batches of Xintongshu spray， and the similarities were more than 0.994. Eight components were identified， i.e. gallic acid （peak 5）， oxypaeoniflorin （peak 9）， chlorogenic acid（peak 10）， caffeic acid （peak 14）， paeoniflorin （peak 17）， ferulic acid （peak 21）， senkyunolide Ⅰ （peak 27） and paeonol （peak 31）. The contents of 8 components ranged from 0.590 3- 0.719 7， 0.565 7-0.851 3， 0.279 4-0.368 1， 0.080 6-0.106 1， 1.922 5-3.033 5， 0.151 3-0.191 6， 0.250 6-0.336 0， 3.056 7-4.161 0 mg/mL， respectively. The average transfer rates of paeonol and ferulic acid from decoction pieces to sprays were 63.76% and 38.06%， respectively. It was also found that the process in which the loss of paeonol was more than 30% was the extraction by percolation and negative pressure concentration of Moutan Cortex. The process in which the loss of ferulic acid was more than 50% was the steam distillation extraction process of Chuanxiong Rhizoma. CONCLUSIONS The established HPLC fingerprint and content determination method of Xintongshu spray are reproducible and specific. The key processes that cause a decrease in the average transfer rates of the index components are the extraction by percolation and negative pressure concentration of Moutan Cortex and steam distillation extraction of Chuanxiong Rhizoma.

Establishment of fingerprint and determination of differential components of Sophora flavescens / 中国药房

OBJECTIVE To establish the fingerprint of Sophora flavescens， and to screen differential components and determine their contents.　METHODS HPLC fingerprints of 12 batches of S. flavescens were established by using Similarity Evaluation System of Chromatographic Fingerprints of TCM （2012 edition）； common peaks were identified and their similarities were evaluated. Chemical pattern recognition analysis [cluster analysis （CA），principal component analysis （PCA） and orthogonal partial least squares-discriminant analysis（OPLS-DA）] were performed with SIMCA 14.1 and SPSS 23.0 software， and differential components which influenced the quality of S. flavescens were screen with variable importance in the projection（VIP）＞1 as standard. Meanwhile， the contents of 4 kinds of differential components were determined by the same HPLC method.　RESULTS There were 17 common peaks in the fingerprints of 12 batches of S. flavescens，and their similarities were all higher than 0.96. A total of 6 common peaks were identified， i.e. oxymatrine （peak 1）， oxysophocarpine （peak 2）， matrine （peak 10）， trifolirhizin （peak 14）， kurarinone （peak 16） and norkurarinone （peak 17）. Results of CA， PCA and OPLS-DA showed that 12 batches of S. flavescens were divided into 3 categories according to producing area， i.e. S1-S7 （Shangzhou District of Shaanxi Province） were grouped into one category， S8-S10 （Yichuan County of Henan Province） into one category and S11-S12 （Chifeng City of Inner Mongolia） into one category. VIPs of matrine， norkurarinone， kurarinone and oxysophocarpine and the chemical components represented by peak 11 and 9 were all greater than 1. The contents of matrine， norkurarinone， kurarinone and oxysophocarpine in 12 batches of S. flavescens were 2.65-4.93， 1.54-3.44， 9.63-12.94 and 5.08-6.10 mg/g， respectively. CONCLUSIONS HPLC fingerprint of S. flavescens is established successfully in the study， and can be used to screen 6 differential components by combining with chemical pattern recognition analysis， which can provide reference for quality control of S. flavescens.

Rapid identification and differential markers of Curcumae Radix decoction pieces of different sources based on Heracles Neo ultra-fast gas phase electronic nose / 中国中药杂志

Since Curcumae Radix decoction pieces have multiple sources, it is difficult to distinguish depending on traditional cha-racters, and the mixed use of multi-source Curcumae Radix will affect its clinical efficacy. Heracles Neo ultra-fast gas phase electronic nose was used in this study to quickly identify and analyze the odor components of 40 batches of Curcumae Radix samples from Sichuan, Zhejiang, and Guangxi. Based on the odor fingerprints established for Curcumae Radix decoction pieces of multiple sources, the odor components was identified and analyzed, and the chromatographic peaks were processed and analyzed to establish a rapid identification method. Principal component analysis(PCA), discriminant factor analysis(DFA), and soft independent modeling cluster analysis(SIMCA) were constructed for verification. At the same time, one-way analysis of variance(ANOVA) combined with variable importance in projection(VIP) was employed to screen out the odor components with P<0.05 and VIP>1, and 13 odor components such as β-caryophyllene and limonene were hypothesized as the odor differential markers of Curcumae Radix decoction pieces of diffe-rent sources. The results showed that Heracles Neo ultra-fast gas phase electronic nose can well analyze the odor characteristics and rapidly and accurately discriminate Curcumae Radix decoction pieces of different sources. It can be applied to the quality control(e.g., online detection) in the production of Curcumae Radix decoction pieces. This study provides a new method and idea for the rapid identification and quality control of Curcumae Radix decoction pieces.

Effects of mycorrhizal planting on small molecular chemical components of Dendrobium officinale / 中国中药杂志

This study aimed to provide a scientific basis for the application of the mycorrhizal planting technology of Dendrobium officinale by investigating the effects of mycorrhizal planting on the fingerprints of D. officinale and the content of six chemical components. Seventeen samples of D. officinale under mycorrhizal and conventional planting were collected from four regions, such as Jinhua of Zhejiang. The HPLC fingerprints were established to evaluate the similarity of the samples. The content of six chemical components of the samples was determined by HPLC. There were 15 common peaks in the fingerprints, and five of them were identified by marker compounds, which were naringenin, 4,4'-dihydroxy-3,5-dimethoxybibenzyl, 3,4'-dihydroxy-5-methoxybibenzyl, 3',4-dihydroxy-3,5'-dimethoxybibenzyl(gigantol), and 3,4-dihydroxy-4',5-dimethoxybibenzyl(DDB-2). The similarities of the fingerprints of mycorrhizal and conventional planting samples and the control fingerprint were in the ranges of 0.733-0.936 and 0.834-0.942, respectively. The influences of mycorrhizal planting on fingerprints were related to planting regions, the germplasm of D. officianle, and the amount of fungal agent. The content of six chemical components in the samples varied greatly, and the content of DDB-2 was the highest, ranging from 69.83 to 488.47 μg·g~(-1). The mycorrhizal planting samples from Chongming of Shanghai and Taizhou of Jiangsu showed an increase in the content of 5-6 components, while samples from Zhangzhou of Fujian and Jinhua of Zhejiang showed an increase in the content of 1-2 components. The results showed that mycorrhizal planting technology did not change the chemical profile of small molecular chemical components of D. officinale, but affected the content of chemical components such as bibenzyls, which has a good application prospect.

Recovery and Visualisation of Methamphetamine-Contaminated Fingermarks from Non-Porous Surfaces

@#Introduction: Fingermarks left at a crime scene can indicate the presence of an individual and his/her involvement in the crime. Fingermarks, usually invisible, can appear on any surface and may be contaminated by any exogenous substances, including drug substance. Recovery of fingermarks contaminated by drug substance is crucial to link an individual with the drug-related crimes. Hence, this study was aimed to investigate the recovery and visualisation of methamphetamine-contaminated fingermarks from various non-porous surface materials. Methods: In this study, fingermarks were deposited on 11 types of surface materials varied by the presence of methamphetamine contamination, immediacy of deposition, and their concentration levels. Each fingermark was then developed using white and black fingerprint powders, graded, and compared based on the different settings. Results: Application of fingerprint powder was good in developing fingermarks; however, its suitability depends on the nature of the surface materials. Black fingerprint powder produced better visualisation where the fingermarks on all the 11 surface materials tested in this study were successfully recovered compared to white fingerprint powders. Methamphetamine-contaminated fingermarks could still be recovered using the fingerprint powder dusting method, but the fingermark grade was reduced due to the presence of exogenous substance. Conclusion: To conclude, the recovery and visualisation of methamphetamine-contaminated fingermarks on non-porous surfaces were successfully carried out through the application of fingerprint powder. A more severe contamination might lead to lower fingermark grade showing lesser ridge details.

Study on the fingerprint of total saponins from Mussaenda pubescens and the spectrum-effect relationship of its hepatoprotective activity / 中国药房

OBJECTIVE To establish the fingerprint of total saponins from Mussaenda pubescens， and to study the spectrum- effect relationship of its hepatoprotective activity. METHODS Ten batches of total saponins from M. pubescens from different origins were prepared using 75% ethanol as solvent. High-performance liquid chromatography （HPLC） and the Similarity Evaluation System for Traditional Chinese Medicine Chromatographic Fingerprints （2012 edition） were used to draw the fingerprints of 10 batches of total saponins from M. pubescens. The similarity evaluation and identification of common peaks were conducted. The same HPLC method was adopted to determine the contents of five triterpenoid saponins （mussaendoside H， mussaendoside U， mussaglaoside C， mussaendoside G and mussaendoside O）. The hepatoprotective effect of total saponins from M. pubescens was investigated by establishing carbon tetrachloride-induced acute liver injury model mice， and the spectrum-effect relationship was studied by using grey correlation analysis. RESULTS There were 11 common peaks in 10 batches of total saponins from M. pubescens， 5 of which were identified， i.e. mussaendoside H （peak 3）， mussaendoside U （peak 7）， mussaglaoside C （peak 8）， mussaendoside G （peak 9） and mussaendoside O （peak 11）； the similarities of 10 batches of samples ranged 0.940- 0.991. Average contents of mussaendoside H， mussaendoside U， mussaglaoside C， mussaendoside G， mussaendoside O were 0.01- 0.05， 0.10-0.21， 0.10-0.18， 0.03-0.08， 0.20-0.40 mg/g， respectively. Ten batches of total saponins from M. pubescens could generally reduce the contents of alanine aminotransferase （ALT） and aspartate aminotransferase （AST） in serum， and tumor necrosis factor-α （TNF-α）， interleukin-6 （IL-6） and IL-1β in liver tissue of model mice （P＜0.05 or P＜0.01）. The E-mail：13878195336@139.com correlation between the common peak areas and the contents of ALT， AST， TNF-α， IL-6 and IL-1β were 0.602-0.757， 0.585-0.833， 0.593-0.795， 0.618-0.820， 0.607-0.804， respectively； the peaks with high correlation were peaks 11， 9 and 8 in order. CONCLUSIONS Ten batches of total saponins from M. pubescens have similar components， and the average contents of mussaendoside H， mussaendoside U， mussaglaoside C， mussaendoside G and mussaendoside O are different. The batches of samples have a certain degree of hepatoprotective effect； mussaendoside O， mussaendoside G and mussaglaoside C may be its main active components.

Establishment of UPLC fingerprint and study on anti-respiratory syncytial virus spectrum-effective relationship of ethanol extract from Callicarpa nudiflora / 中国药房

OBJECTIVE To establish the fingerprint of the ethanol extract from Callicarpa nudiflora， analyze its anti- respiratory syncytial virus （RSV） activity in vitro， and study the relationship between spectrum and effect. METHODS Using 10%， 30%， 50%， 70% and 90% ethanol as solvent， 20 batches of ethanol extracts from 4 batches of C. nudiflora were prepared. The fingerprints for 20 batches of ethanol extracts from C. nudiflora were mapped by ultra-high-performance liquid chromatography （UPLC）， and the similarity evaluation was conducted by using the Similarity Evaluation System for Traditional Chinese Medicine Chromatographic Fingerprints （2012 edition）. The cytopathic effect method and MTT method were used to investigate the in vitro inhibitory activity of the ethanol extracts from C. nudiflora on RSV. Pearson correlation analysis， grey correlation degree and orthogonal partial least squares （OPLS） analysis were used to study the spectrum-effect relationship. RESULTS There were 25 common peaks in 20 batches of ethanol extracts from C. nudiflora， and the similarities ranged from 0.912 to 0.998， and the RSDs of common peak areas were 33.54%-162.28%. The average values of IC50 for RSV of 20 batches of ethanol extracts from C. nudiflora were 9.55-272.23 μg/mL. The results of Pearson correlation analysis， grey correlation analysis and OPLS analysis showed that the Pearson correlation coefficients （P＜0.05） of the common peaks 8， 10， 12， 16， 18-19， 22-24 with pharmacodynamic indicators and regression coefficients were all negative， the correlation coefficients were all greater than 0.6， and the values of variable importance in projection were all greater than 1. CONCLUSIONS Twenty batches of ethanol extracts from C. nudiflora have similar components but significant differences in content， and exhibit different degrees of anti-RSV activity in vitro. The corresponding components of common peaks 8， 10， 12， 16， 18-19， 22-24 may be the characteristic components of anti-RSV of C. nudiflora.

Optimization of processing methods for Terminalia chebula based on fingerprint，antioxidant spectrum-effect correlation and multi-component contents / 中国药房

OBJECTIVE To compare the similarities and differences between raw and different preparations of Terminalia chebula based on fingerprint， antioxidant spectrum-effect correlation and multi-component contents， and to provide a reference for searching for modern processing methods of T. chebula that are similar to classical ancient methods. METHODS Ten batches of raw and different preparations of T. chebula （single stir-fried products， bran-roasted products， sand-scorched products， ash-roasted products， stir-fried charcoal products， and wine-steamed products） were used as test samples. The high-performance liquid chromatography （HPLC） fingerprints of different samples were established by using the Similarity Evaluation System for Chromatographic Fingerprint of TCM （2012 edition）， the chromatographic peaks were identified， and chemometrics analysis was carried out. At the same time， HPLC method was used to determine the contents of 8 identified components. The antioxidant capacity of raw and different preparations of T. chebula was determined by DPPH free radical scavenging method， and the spectrum- effect relationship was analyzed. RESULTS A total of 20 common peaks were identified in the fingerprints of the raw and different preparations of T. chebula， and the similarity of each sample was ＞0.9. Nine common peaks were identified from the raw and different preparations of T. chebula， including chromatographic peak 2 （chebulic acid）， 3 （gallic acid）， 6 （punicalagin A）， 8 （punicalagin B）， 12 （corilagin）， 15 （chebulagic acid）， 18 （ellagic acid）， 19 （1，2，3，4，6-O-pentagalloyl glucose）， 20 （chebulinic acid）， etc. Compared with crude drug， the contents of the above 8 components （punicalagin A and B are recorded as punicalagin） in different preparations of T. chebula were changed， and the changes of the contents of the stir-fried charcoal and wine-steamed products were more obvious than those of other processed products. Chemometric analysis showed that the fingerprints of stir-fried charcoal and wine-steamed products of T. chebula were obviously distinguished from other processed products， and the fingerprint information of raw products and other processed products of T. chebula was partially overlapped. Four main differential components （chebulinic acid， chebulagic acid， gallic acid， ellagic acid） were obtained between raw and processed products of T. chebula； and four main effective components （chebulinic acid， chebulagic acid， gallic acid， corilagin） were obtained by analyzing the spectrum-effect relationship of antioxidant activity. The single stir-fried product of T. chebula showed the strongest antioxidant activity. CONCLUSIONS The single stir-frying method is a modern processing method of T. chebula which is similar to the classical ancient method and is more excellent.

Identification of components，fingerprint and content determination of the effective parts of Dracocephalum moldavica / 中国药房

OBJECTIVE To provide a reference for comprehensive quality evaluation and control of the effective parts of Dracocephalum moldavica （EPDM）. METHODS A total of 10 batches of EPDM were prepared， and chemical information of EPDM was collected by HPLC-Q-Exactive-MS. EPDM components were identified by literature search， database comparison and manual analysis. HPLC fingerprints of 10 batches of EPDM were established by using the Similarity Evaluation System for Traditional Chinese Medicine Chromatographic Fingerprint （2004 A edition）； the similarity evaluation and common peak identification were carried out， and the contents of 5 index components were determined by HPLC. RESULTS A total of 11 compounds in EPDM were identified. The fingerprint similarities of EPDM samples from 10 batches were all above 0.96. Among 11 chromatographic peaks， 5 peaks were identified， such as luteolin-7-O-β-D-glucuronide（LG）， apigenin-7-O-glucuronide（APG）， rosmarinic acid（RA）， diosmetin-7-O-β-D-glucuronide（DG）， tilianin（TL） . The results of the quantitative analysis showed that all above 5 components had good linearity （R2≥0.999）， and the average recoveries were in the range of 95.12%-98.37%. The contents of LG， APG， RA， DG， TL were 21.268 3-29.243 9， 6.365 4-7.771 7， 37.327 4-45.671 2， 17.169 9-21.985 9， 66.940 4-91.206 3 mg/g， respectively. CONCLUSIONS The established method of component identification， fingerprint and content determination is stable， feasible and reliable， which is suitable for the comprehensive quality evaluation and control of EPDM.

Identification and quality evaluation of mixed herb in different parts of Plantago depressa Willd. and Plantago asiatica L / 国际中医中药杂志

Objective:To establish the fingerprints of Plantaginis Herba.Methods:The fingerprints were determined by UPLC. The peak areas of fingerprints of different parts and origins were analyzed by variance analysis and independent sample t-test. PCA, HCA, PLS-DA and other chemical patterns were analyzed by Simca14.1. The index weight was calculated by CRITIC, and the quality of plantain evaluation was combined with grey correlation degree.Results:The fingerprints of grass, stem, leaf and spike of Plantago depressa Willd. calibrated for 24, 16, 23 and 22 common peaks. The fingerprints of grass, stem, leaf and spike of Plantaginis Herba calibrated for 22, 10, 16 and 22 common peaks, and the fingerprints of commercial mixed plantain calibrated for 23 common peaks. 10 peaks were identified. The analysis of variance showed that there were differences in chromatographic peak areas between different parts of Plantago asiatica L. and Plantago depressa Willd.. And combinedede with PLS-DA, it showed that there were 16 important characteristic indexes in the classification, and the importance ranking was peak 3, 8, 28, 12, 14, 7, 5, 17, 6, 19, 23, 11, 22, 27, 9, 16. The quality evaluation results of critical method combined with grey correlation degree showed that among Plantago depressa Willd., Plantago asiatica L. and commercial mixed plantain herbs, the quality of Plantago asiatica L. was the best. Conclusion:The mixture of plantain exists in the market. The fingerprints established in this study can be used for the identification and quality evaluation of Plantaginis Herba from different sources.

Qualitative evaluation of Bupleuri Radix in different areas by UPLC fingerprint combined with Principle Component Analysis / 国际中医中药杂志

Objective:To establish the fingerprint of Bupleuri Radix with Ultra High Performance Liquid Chromatography (UPLC) method and combining Principal Component Analysis to evaluate the quality of Bupleuri Radix in different areas. Methods:Acquity UPLC BEH-C 18 (2.1 mm×100 mm, 1.7 μm) column was used with acetonitrile (A)-water (B) solution, gradient elution. The column temperature was 30 ℃, the flow rate was 0.3 ml/min, and the detection wavelength was 200 nm, injection volume 5 μl. Results:There were 7 common peaks in the UPLC fingerprints of 10 batches of medicinal materials, and the similarity was 0.940-0.975. Through the principal component analysis, the cumulative contribution rate of three main component factors was 90.977%,and comprehensive score of S5 (Hubei) was the highest with the best quality.Conclusions:There are certain quality differences of different areas in Bupleuri Radix. Through the combination of fingerprint and principal component analysis, it can provide reference for quality control, development and application of Bupleuri Radix.

Study on UPLC fingerprint and multi-component content determination of Microctis Folium from different origins / 国际中医中药杂志

Objective:To establish the fingerprints of Microctis Folium by ultra high performance liquid chromatography (UPLC); To determine the contents of three flavonoids in the Microctis Folium; To evaluate the quality difference of Microctis Folium from different producing areas. Methods:The fingerprints were performed on Agilent ZORBAX SB C18 column (2.1 mm×150 mm,1.8 μm). The mobile phase was acetonitrile - 0.1 % acetic acid solution with gradient elution at a flow rate of 0.30 ml/min. The column temperature was 30 ℃ and the detection wavelength was 315 nm. The common fingerprint peaks were identified by UPLC-mass spectrometry, and the identification results were confirmed by comparison of reference materials. Waters Cortecs T3 C18 chromatographic column (2.1 mm × 100 mm,1.6 μm) was used for content determination. The mobile phase was methanol-0.1 % formic acid solution with gradient elution at a flow rate of 0.35 ml/min. The column temperature was 30 ℃ and the detection wavelength was 339 nm. The contents of vitexin, isovitexin and narcissoside in 15 batches of Microctis Folium from different habitats were determine. Results:There were 11 common peaks in the fingerprint of Microctis Folium. Identified by mass spectrometry and confirmed by reference substance,10 chemical components were identified, including caffeic acid, p-hydroxycinnamic acid, ferulic acid, vitexin, isovitexin, kaempferol-3-O-rutoside, astragaloside, narcissoside, isorhamnetin-3-O-glucoside and linden glycoside. The similarity between the fingerprints of 15 batches of Microctis Folium and the control fingerprint was greater than 0.95, indicating that the overall similarity of the fingerprints of Microctis Folium from different producing areas was high. The total contents of three active components were 3.23-5.64 mg/g in Yangjiang City, Guangdong, 3.60-5.78 mg/g in Zhanjiang City, Guangdong, 4.68-5.73 mg/g in Yulin City, Guangxi and 3.87-5.21 mg/g in Wuzhishan City, Hainan . There was no significant difference in the content of three active components in different producing areas. Conclusion:The fingerprints and the determination method established in the study are stable and feasible, which can be used for the quality evaluation of Microctis Folium.

Comparison of the fingerprint and multi-component contents between Liuwei dihuang powder decoction pieces and traditional decoction pieces with different decocting time / 中国药房

OBJECTIVE To compare the change law of multi-components in the extraction process between Liuwei dihuang powder decoction pieces and traditional decoction pieces （hereinafter referred to as powder decoction pieces and traditional decoction pieces）， and to provide scientific basis for the modern technology research of Liuwei dihuang formula. METHODS Taking powder decoction pieces and traditional decoction pieces as samples， the samples were taken when soaking for 60 min， at 0， 5， 10， 15， 20， 25， 30， 40， 50， 60 min of the first decocting and at 5， 10， 20， 30， 40 min of the second decocting， respectively. HPLC method was used to establish the fingerprints of 2 kinds of decoction pieces with different decocting time. The similarity evaluation and peak identification were performed. The contents of 8 components including 5-hydroxyfurfural， catechin， monoglycoside， loganin， swertin glycoside， dihydroquercetin， paeonol and benzoyl paeoniflorin were all determined. RESULTS With different decocting time， the similarties between 2 kinds of decoction pieces and their respective control fingerprints R were all greater than 0.98. In the fingerprints of traditional decoction pieces， five chromatographic peaks were identified， namely， 5- hydroxyfurfural， monetin， swertiaoside， dihydroquercetin and paeonol； in the fingerprints of powder decoction pieces， six chromatographic peaks were identified， namely， 5-hydroxyfurfural， monoglycoside， swertiamarin， dihydroquercetin， paeonol and benzoyl paeoniflorin. The results of content determination showed that in the first 5 minutes of the first decocting， the decocting rate of almost all the ingredients in the powder decoction pieces was faster than that of the traditional decoction pieces； after 40 min， the contents of other active ingredients were lower than those of traditional decoction pieces except for 5-hydroxyfurfural and paeonol. In the process of second decocting， except for paeonol and loganin， the contents of other ingredients in powder decoction pieces were higher than that in traditional decoction pieces； catechin was completely decocted from the traditional decoction pieces in the first decocting， while it could still be detected in the powder decoction pieces in the second decocting. There was little difference in the total decocted amount of the 8 ingredients in the two decoction pieces. CONCLUSIONS The chemical composition of powder decoction pieces of Liuwei dihuang formula has no obvious advantages compared with traditional decoction pieces， and can not save the decocting time and the amount of medicinal materials.

Study on UPLC fingerprint and content determination of mangiferin of Gentiana rhodantha / 中国药房

OBJECTIVE To provide reference for quality control of Gentiana rhodantha. METHODS Taking 52 batches of G. rhodantha as subject， ultra-high performance liquid chromatography （UPLC） fingerprint was adopted. The similarity of 52 batches of medicinal materials samples was evaluated by the Similarity Evaluation System for Chromatographic Fingerprints of Traditional Chinese Medicine （2004A edition）； the content of mangiferin was determined； chemometric analyses [cluster analysis， principal component analysis （PCA） and orthogonal partial least squares-discriminant analysis （OPLS-DA）] were performed. RESULTS UPLC fingerprints of 52 batches of G. rhodantha were established， 17 common peaks were identified， and 6 of them were identified， which were loganic acid （peak 1）， neomangiferin （peak 3）， swertiamarin （peak 5）， dangyin （peak 6）， mangiferin （peak 7） and isoorientin （peak 9）. The similarities of 52 batches of medicinal materials samples were all greater than 0.9； cluster analysis showed that S1-S46， S48-S52 clustered into one class， and S47 alone； PCA results showed that the cumulative variance contribution rate of the first six principal components was 82.928%； OPLS-DA results showed that the corresponding components of swertiamarin， mangiferin and chemical composition represented by peak 4， 14， 15， 16 were the main iconic components affecting the quality differences of G. rhodantha medicinal materials. The contents of mangiferin in 52 batches of medicinal material samples ranged from 18.2 to 101.0 mg/g， mostly in accordance with 2020 edition of Chinese Pharmacopoeia. CONCLUSIONS The established UPLC fingerprint and chemometric analysis methods combined with content determination method of mangiferin can comprehensively evaluate the quality of G. rhodantha.

Study on "Spectrum-material-effect" relationship of Compound Muji Granules against liver tumor based on microfluidic chip / 中国药理学通报

Aim To explore the material basis of anti-tumor effect of Compound Muji Granules. Methods The anti-tumor pharmacodynamics of Compound Muji Granules in vitro was studied by microfluidic chip technology. The fingerprint of Compound Muji Granules was established by HPLC. The "Spectrum-Material-Effect" of Compound Muji Granules was analyzed by grey correlation analysis,partial least squares regression analysis and network pharmacology approach. Results Seven batches of Compound Muji Granules with different extraction methods were successfully established. The results of grey correlation analysis showed that there was a positive correlation between Compound Muji Granules and 7 of the 14 components with pharmacodynamic correlation coefficient >0.80. The contribution of anti liver tumor was peak number 48(luteolin)>6(gallic acid)>19(chlorogenic acid)>59(quercetin)>67(kaempferol)>65(naringin)>38(ellagic acid),in that order. Conclusions Through the establishment of "Spectrum-Material-Effect" research method,it is clear that the above seven active monomers may be the anti-tumor material basis of Compound Muji Granules.

Discussion on Current National Standards for Traditional Chinese Medicine Dispensing Granules / 中国实验方剂学杂志

Strengthening the standard formulation and quality management of traditional Chinese medicine（TCM） dispensing granules is an important part of the strategic planning for the development of TCM in China. In order to examine the clinical application and overall quality control of the existing national standards for TCM dispensing granules， this study classified and summarized the varieties in the existing standards， analyzed their clinical applicability， and discussed the characteristics of the test methods for identification， content determination and specific chromatogram/fingerprint. It was found that the coverage of the existing standards was inadequate in terms of quantity， and it was even weaker in the aspects of therapeutic efficacy， herb family， processing method and preparation method of TCM dispensing granules. It was concluded that the characteristics of national standards in test methods were summarized as follows：guided by clinical application， based on the reference system， taking specific chromatogram as a breakthrough， so as to improve the overall quality control of TCM dispensing granules. It is suggested that the coverage of national standards should be subsequently expanded to meet the needs of market development. In order to enhance clinical applicability， the content of national quality standards should be increased， including increasing variety diversity to meet the needs of clinical application， raising the standard requirements to improve the clinical medication experience， and strengthening effectiveness research to highlight clinical efficacy. At the same time， the accessibility of regulatory inspection is enhanced， the rules for the management of varieties without national standards are promulgated to lay the foundation for the healthy and orderly development of TCM dispening granule industry.