1.Analysis on Quality Standard of Sennae Folium(Cassia angustifolia) Dispensing Granules Based on Standard Decoctions
Jinxin LI ; Xue DONG ; Shuai DUAN ; Guiyun CAO ; Jinghua ZHANG ; Yongfu LUAN ; Yongqiang LIN ; Xiaodi DONG ; Zhaoqing MENG
Chinese Journal of Experimental Traditional Medical Formulae 2025;31(9):192-200
ObjectiveTo establish the quality standards for Sennae Folium(Cassia angustifolia) dispensing granules based on standard decoctions. MethodsHigh performance liquid chromatography(HPLC) specific chromatograms were established for 15 batches of Sennae Folium(C. angustifolia) standard decoctions and 10 of Sennae Folium(C. angustifolia) dispensing granules from different manufacturers, and the similarity evaluation, hierarchical cluster analysis(HCA) and principal component analysis(PCA) were performed. Linear calibration with two reference substances(LCTRS) and quantitative analysis of multi-components by single-marker(QAMS) were established for the common peaks in the specific chromatograms to determine the contents of main components in the decoction pieces, standard decoctions and dispensing granules, and to calculate their transfer rates from decoction pieces to standard decoctions and dispensing granules. ResultsThe similarities of specific chromatograms of 15 batches of Sennae Folium(C. angustifolia) standard decoctions and 10 batches of Sennae Folium(C. angustifolia) dispensing granules were all greater than 0.95, and a total of 8 characteristic peaks were calibrated, and five of them were identified, including kaempferol-3,7-O-diglucoside, apigenin-6,8-di-C-glucoside, quercetin-3-O-gentianoside, sennoside B and sennoside A. HCA and PCA results showed that there were certain differences in the composition of different batches of standard decoctions, but no clustering was observed in the production area. As the standard decoctions, the extract rate of 15 batches of samples was 26.54%-45.38%, the contents of kaempferol-3,7-O-diglucoside, apigenin-6,8-di-C-glucoside, quercetin-3-O-gentianoside, sennoside B and sennoside A were 12.16-19.26, 2.57-4.94, 3.27-5.11, 6.75-11.39, 4.69-7.79 mg·g-1, and their transfer rates from decoction pieces to standard decoctions were 45.41%-79.02%, 29.12%-55.07%, 40.52%-67.90%, 24.72%-49.12%, 27.54%-49.34%, respectively. The extract rates of Sennae Folium(C. angustifolia) dispensing granules(C8-C10) were 38.10%-39.50%, the transfer rates of the above five components from decoction pieces to dispensing granules were 72.85%-73.58%, 53.43%-53.94%, 40.19%-40.74%, 24.62%-25.00%, 28.65%-29.11%, respectively, which were generally consistent with the transfer rates from decoction pieces to standard decoctions. ConclusionCompared with the relative retention time method, LCTRS has higher prediction accuracy and is more suitable for chromatographic columns. The established quality control standard of Sennae Folium(C. angustifolia) dispensing granules based on standard decoction is reasonable and reliable, and all indicators of samples from different manufacturers are within the range specified based on the standard decoction, which can provide reference for the quality control and process research of this dispensing granules.
2.Analysis on Quality Standard of Hedyotis Herba Dispensing Granules Based on Standard Decoction
Jinghua ZHANG ; Nana WU ; Yanan LYU ; Guiyun CAO ; Jiacheng XU ; Yongqiang LIN ; Xiaodi DONG ; Jinxin LI ; Zhaoqing MENG
Chinese Journal of Experimental Traditional Medical Formulae 2025;31(10):210-217
ObjectiveTo establish the specific chromatogram and quantitative analysis of multi-components by single-marker(QAMS) based on linear calibration using two reference substances(LCTRS), explore the consistency between Hedyotis Herba dispensing granules and standard decoction, and evaluate the quality of the dispensing granules. MethodsHigh performance liquid chromatography(HPLC) specific chromatogram was established based on 15 batches of Hedyotis Herba standard decoction and 10 batches of the dispensing granules, and LCTRS was used to locate chromatographic peaks. The actual retention times of 7 characteristic peaks in the specific chromatogram was measured on 24 different types of C18 columns, taking deacetyl asperulosidic acid and asperulosidic acid as the dual standard compounds, the retention times of the other 5 characteristic peaks were predicted and validated. Based on this, QAMS was developed to determine the contents of four components(deacetyl asperulosidic acid, deacetyl asperulosidic acid methyl ester, asperulosidic acid, and p-coumaric acid). Then, the relative correction factors of deacetyl asperulosidic acid, deacetyl asperulosidic acid methyl ester and p-coumaric acid were calculated using the reference peak of asperulosidic acid in the dual standard compounds, and each component was quantified accordingly. Finally, the consistency between the dispensing granules and standard decoction was assessed by taking extract rate of the standard decoction, consistency of the specific chromatograms, contents and transfer rates of the indicator components as indexes, and the quality of the dispensing granules was evaluated. ResultsThere were 7 common peaks in the characteristic chromatogram of samples of Hedyotis Herba standard decoction and the dispensing granules, and four of them were identified by reference standards, namely deacetyl asperulosidic acid(peak 1), deacetyl asperulosidic acid methyl ester(peak 3), asperulosidic acid(peak 6) and p-coumaric acid(peak 7). The similarity between the dispensing granules and the standard decoction was >0.9. The absolute deviation in the predicted retention time for each component by LCTRS was lower than that of the relative retention time method. The extract rate of the 15 batches of Hedyotis Herba standard decoction ranged from 7.89% to 14.60%, the contents of deacetyl asperulosidic acid, deacetyl asperulosidic acid methyl ester, asperulosidic acid and p-coumaric acid were 6.62-19.70, 3.83-17.99, 1.57-6.69, 1.62-4.52 mg·g-1, and the transfer rates of these components from decoction pieces to the standard decoction were 22.89%-39.60%, 34.03%-62.24%, 24.25%-43.70%, and 40.58%-73.71%, respectively. The extract rate, index component contents and transfer rates from decoction pieces to the three batches of Hedyotis Herba dispensing granules(P1-P3), produced by manufacturer A, were similar to those of the standard decoction prepared from the same batch of decoction pieces, and all fell within the specified range. The contents of the 4 indicator components in 7 batches of the dispensing granules(P4-P10) from manufacturers B-E were all within the range of the content converted from the standard decoction based on the quantity of the dispensing granules. ConclusionThe established specific chromatogram and QAMS based on LCTRS are reasonable and reliable. Based on the evaluation indicators of standard decoction yield, consistency of specific chromatograms, contents and transfer rates of the four index components, the 10 batches of Hedyotis Herba dispensing granules from various manufacturers have exhibited good consistency with the standard decoction, indicating that the current production process is relatively reasonable.
3.Quality Evaluation of Chuanxiong Rhizoma Dispensing Granules Based on HPLC Specific Chromatogram and Two Reference Substances for Determination of Multiple Components
Jinxin LI ; Xue DONG ; Shuai DUAN ; Guiyun CAO ; Jinghua ZHANG ; Yongfu LUAN ; Yongqiang LIN ; Xiaodi DONG ; Zhaoqing MENG
Chinese Journal of Experimental Traditional Medical Formulae 2025;31(11):246-253
ObjectiveTo establish the specific chromatogram of Chuanxiong Rhizoma dispensing granules(CRdg), and to evaluate its quality by chemometrics and two reference substances for determination of multiple components(TRSDMC). MethodsHigh performance liquid chromatography(HPLC) specific chromatograms were established using 13 batches of CRdg from 7 manufacturers, and preliminary quality evaluation was performed by similarity evaluation and chemometrics analysis. Eight characteristic peaks in the specific chromatogram of CRdg were measured on 22 different types of C18 columns, and the actual retention times were recorded. Taking chlorogenic acid(peak 1) and senkyunolide A(peak 8) as double standard compounds, the retention times of the eight characteristic peaks were predicted by linear calibration using two reference substances(LCTRS), and the method was validated on three other columns of different brands. Taking chlorogenic acid as reference peak, the relative correction factor method(RCFM) was used to quantify cryptochlorogenic acid, caffeic acid, ferulic acid, senkyunolide I and senkyunolide A, and the results were compared with the external standard method(ESM). ResultsThe similarities of specific chromatograms of 13 batches of CRdg were all >0.90, and a total of 8 characteristic peaks were calibrated, and six of them were identified, including chlorogenic acid(peak 1), cryptochlorogenic acid(peak 2), caffeic acid(peak 3), ferulic acid(peak 5), senkyunolide I(peak 6) and senkyunolide A(peak 8). Through chemometric analysis, it was found that ferulic acid, chlorogenic acid, senkyunolide I and cryptochlorogenic acid were the main components causing quality difference in CRdg, and the accuracy of LCTRS in predicting the retention time of 8 characteristic peaks was superior to that of the relative retention time method(RRT). Further comparison of the results obtained from RCFM and ESM showed that there was no statistically significant difference between the two methods. ConclusionA quality evaluation method for CRdg based on HPLC specific chromatogram and TRSDMC is established, its qualitative accuracy is better than that of RRT, the quantitative accuracy is similar to that of ESM, and 4 quality-differentiated components among different manufacturers are found. This method is stable and reliable, and has reference value for the quality evaluation of other dispensing granules.
4.Quality Evaluation of Chuanxiong Rhizoma Dispensing Granules Based on HPLC Specific Chromatogram and Two Reference Substances for Determination of Multiple Components
Jinxin LI ; Xue DONG ; Shuai DUAN ; Guiyun CAO ; Jinghua ZHANG ; Yongfu LUAN ; Yongqiang LIN ; Xiaodi DONG ; Zhaoqing MENG
Chinese Journal of Experimental Traditional Medical Formulae 2025;31(11):246-253
ObjectiveTo establish the specific chromatogram of Chuanxiong Rhizoma dispensing granules(CRdg), and to evaluate its quality by chemometrics and two reference substances for determination of multiple components(TRSDMC). MethodsHigh performance liquid chromatography(HPLC) specific chromatograms were established using 13 batches of CRdg from 7 manufacturers, and preliminary quality evaluation was performed by similarity evaluation and chemometrics analysis. Eight characteristic peaks in the specific chromatogram of CRdg were measured on 22 different types of C18 columns, and the actual retention times were recorded. Taking chlorogenic acid(peak 1) and senkyunolide A(peak 8) as double standard compounds, the retention times of the eight characteristic peaks were predicted by linear calibration using two reference substances(LCTRS), and the method was validated on three other columns of different brands. Taking chlorogenic acid as reference peak, the relative correction factor method(RCFM) was used to quantify cryptochlorogenic acid, caffeic acid, ferulic acid, senkyunolide I and senkyunolide A, and the results were compared with the external standard method(ESM). ResultsThe similarities of specific chromatograms of 13 batches of CRdg were all >0.90, and a total of 8 characteristic peaks were calibrated, and six of them were identified, including chlorogenic acid(peak 1), cryptochlorogenic acid(peak 2), caffeic acid(peak 3), ferulic acid(peak 5), senkyunolide I(peak 6) and senkyunolide A(peak 8). Through chemometric analysis, it was found that ferulic acid, chlorogenic acid, senkyunolide I and cryptochlorogenic acid were the main components causing quality difference in CRdg, and the accuracy of LCTRS in predicting the retention time of 8 characteristic peaks was superior to that of the relative retention time method(RRT). Further comparison of the results obtained from RCFM and ESM showed that there was no statistically significant difference between the two methods. ConclusionA quality evaluation method for CRdg based on HPLC specific chromatogram and TRSDMC is established, its qualitative accuracy is better than that of RRT, the quantitative accuracy is similar to that of ESM, and 4 quality-differentiated components among different manufacturers are found. This method is stable and reliable, and has reference value for the quality evaluation of other dispensing granules.
5.Analysis on Quality Standard of Fraxini Cortex(Fraxinus chinensis) Dispensing Granules Based on Standard Decoction
Guiyun CAO ; Bo NING ; Jinmiao QIN ; Xuesong ZHUANG ; Daijie WANG ; Yongqiang LIN ; Xiaodi DONG ; Yi LUO ; Zhaoqing MENG
Chinese Journal of Experimental Traditional Medical Formulae 2023;29(13):122-129
ObjectiveTo establish the quality standard for Fraxini Cortex(Fraxinus chinensis) dispensing granules based on standard decoction, and to provide a basis for the quality control of this dispensing granules. MethodHigh performance liquid chromatography(HPLC) specific chromatograms of 15 batches of Fraxini Cortex(F. chinensis) standard decoctions and 3 batches of Fraxini Cortex(F. chinensis) dispensing granules were established with the mobile phase of 0.1% phosphoric acid aqueous solution(A)-acetonitrile(B) for gradient elution(0-10 min, 12%-15%B; 10-30 min, 15%-32%B) and the detection wavelength of 220 nm. And similarity evaluation, cluster analysis and principal component analysis(PCA) were also carried out. HPLC quantitative analysis of multi-components by single marker(QAMS) was established to determine the contents of the main components in the standard decoctions and dispensing granules. The contents of the corresponding components in Fraxini Cortex(F. chinensis) decoction pieces were also detected, and the transfer rates from decoction pieces to standard decoctions and dispensing granules were calculated. ResultThe similarities between specific chromatograms of 15 batches of Fraxini Cortex(F. chinensis) standard decoctions and 3 batches of Fraxini Cortex(F. chinensis) dispensing granules were all>0.9, and 7 common peaks were identified. The results of cluster analysis and PCA showed that there was some differences in the composition of different batches of standard decoctions, but did not show aggregation of origin. As the standard decoctions, the extract rate was 6.18%-11.62%, the contents of esculin, syringin, fraxin, esculetin, fraxetin, calceolarioside B were 44.92-103.51, 1.36-11.87, 33.26-90.73, 4.63-29.75, 2.40-16.86, 2.49-17.35 mg·g-1, and the transfer rates from decoction pieces to standard decoction were 25.21%-42.54%, 52.57%-88.84%, 43.43%-79.45%, 49.15%-88.27%, 49.22%-72.69%, 27.66%-47.67%, respectively. The extract rates of Fraxini Cortex(F. chinensis) dispensing granules were 10.4%-10.7%, the transfer rates of the above six components from decoction pieces to dispensing granules were 42.76%-43.17%, 80.01%-80.90%, 59.59%-59.88%, 51.35%-52.67%, 60.50%-60.93%, 37.98%-38.37%, respectively, which were generally consistent with the transfer rates from decoction pieces to standard decoctions. ConclusionThe established quality control standard of Fraxini Cortex(F. chinensis) dispensing granules based on standard decoctions is reasonable and reliable, which can provide reference for the quality control and process research of this dispensing granules.
6.Phosphatidylethanolamine functionalized biomimetic monolith for immobilized artificial membrane chromatography
Peijie ZHU ; Weijia CHEN ; Qiqin WANG ; Huihui WU ; Meng RUAN ; Hongwu WANG ; Zhengjin JIANG
Journal of Pharmaceutical Analysis 2022;12(2):332-338
In this research,a new phospholipid based monolith was fabricated by in situ co-polymerization of 1-dodecanoyl-2-(11-methacrylamidoundecanoyl)-sn-glycero-3-phosphoethanolamine and ethylene dimethacrylate to mimick bio-membrane environment.Excellent physicochemical properties of this novel monolith that were achieved included column efficiency,stability,and permeability.Moreover,the biomimetic monolith showed outstanding separation capability for a series of intact proteins and small molecules.In particular,it exhibited good potential as an alternative to the commercial immobilized artificial membrane(IAM)column(IAM.PC.DD2)for studying drug-membrane interactions.This study not only enriched the types of IAM stationary phases,but also provided a simple model for the prediction of phosphatidylethanolamine related properties of drug candidates.
7.Malignancy of renal angiomyolipoma from tuberous sclerosis complex with TSC2 mutation.
Yu-Jing HUANG ; Zong-Pei JIANG ; Yu-Ping CHEN ; Jin-Quan WU ; Jia-Li HUANG ; Yan-Qiang CHEN ; Meng-Jun LIANG
Chinese Medical Journal 2019;132(1):103-105
Adult
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Angiomyolipoma
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diagnosis
;
genetics
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Exons
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genetics
;
Humans
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Kidney Neoplasms
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diagnosis
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genetics
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Male
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Mutation
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genetics
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Tuberous Sclerosis
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complications
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Tuberous Sclerosis Complex 2 Protein
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genetics
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Young Adult
8.Optimization of the Hot Sand Processing Technology for Alpinia officinarum by Central Composite Design-response Surface Method
Xianmei DENG ; Simin HUANG ; Yuling CHEN ; Jiang MENG ; Bin ZHAO
China Pharmacy 2019;30(7):931-936
OBJECTIVE:To optimize the hot sand processing technology of Alpinia officinarum,and to provide scientific evidence for the standardized processing of A. officinarum. METHODS:The contents of galangin and curcumin in processed A. officinarum were determined by HPLC. Based on single factor test,using processing temperature and processing time as factors,comprehensive score of galangin and curcumin contents as index,central composite design-response surface method was used to optimize hot sand processing technology of A. officinarum,and the processing technology was validated. RESULTS:The optimal processing technology included processing temperature of 200 ℃ and processing time of 5.5 min. In validation tests,average comprehensive score was 94.38 (RSD=1.02%),relative deviation of which to predicted value 93.74 was 0.68%. CONCLUSIONS:The optimized processing technology is simple and predictable. It can be used for hot sand processing technology of A. officinarum.
9.Chemical Constituents from Tong An Injection (Ⅰ)
Chan SHANG ; Haibo LI ; Mengxuan LI ; Zhenzhen SU ; Zhaoqing MENG ; Wenzhe HUANG ; Zhenzhong WANG ; Gang DING ; Zhonglin YANG ; Wei XIAO
World Science and Technology-Modernization of Traditional Chinese Medicine 2016;18(12):2118-2124
This study aimed at investigating the antiviral constituents from the active fractions of Tong-An (TA) injection.In this study,the active constituents of TA injection were screened by LPS-induced PGE2 production mode to detect the contents of PGE2.The chemical constituents were isolated by HP-20 macroporous resin,silica gel column chromatography,ODS column chromatography,Sephadex LH-20 column chromatography and preparative and semi-preparative HPLC.The structures were identified by spectral data and physicochemical property.As a result,the 95% ethanol eluate of TA injection on the macroporous adsorption resin column was proved to be the active fraction of TA injection.Seventeen compounds were isolated from TA injection and identified as syringaresinol (1),N-Trans-Feruloyltyramine (2),chelerythrine (3),sinomenine (4),coptisine (5),sanguinarine (6),chelidoniny (7),magnoflorine (8),allocryptopine (9),protopine (10),farrerol (11),dihydrosanguinarine (12),heptadec-(9Z)-enoic acid (13),chlorogenic acid (14),cryptochlorogenin acid (15),3,5-di-O-caffeoylquinic acid (16) and 4,5-di-O-caffeoylquinic acid (17).PGE2 inhibitory activities of these compounds were determined,among which six compounds presented inhibitory activities against PGE2.It was concluded that all the isolated compounds from TA injection were firstly reported with the favorable inhibitory activities of compounds 2,5,9,10,11,12 against PGE2.
10.Study on Quality ofYuan-Hu Zhi-TongTablet from Different Manufacturers by HPLC Fingerprint
Hailin ZHU ; Zhaoqing MENG ; Gang DING ; Zhenzhong WANG ; Wei XIAO
World Science and Technology-Modernization of Traditional Chinese Medicine 2015;(7):1460-1466
This study was aimed to evaluate the quality ofYuan-Hu Zhi-Tong (YHZT) tablet from different manufacturers by high performance liquid chromatography (HPLC) fingerprint. An HPLC method was developed to establish the fingerprint of 12 batches of YHZT from 10 manufacturers. The common peaks were confirmed by mass spectrometric analysis. Similarity analysis (SA), hierarchical cluster analysis (HCA) and principal component analysis (PCA) were applied to analyze the fingerprint chromatography. The results showed that there were 15 common peaks in which 12 components were from Corydalis Rhizoma and 3 from Radix Angelicae Dahuricae. The similar degrees of 12 batches of YHZT tablet were between 0.498 and 0.999. Based on the values, they could fall into three groups. The result of HCA showed that 12 batches of samples could be divided into 3 classes. The results of PCA indicated that the first three principal components (PCs) could represent the 15 common peaks. According to the scores of 3 PCs, 12 batches of samples could be divided into three categories. The classification result was mainly affected by the components of Corydalis Rhizoma. The classification results of three methods were basically the same. Based on the combination of three methods, 12 samples can be divided into three grades in the aspect of quality. It was concluded that the quality differences of YHZT tablet from different manufacturers were obvious. The combining application of three methods can be used in the evaluation on fingerprint of samples from different sources and influence factor analysis. It can be used as an effective method for quality evaluation.

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