1.Quality Evaluation of Polygonum cuspidatum by UPLC Fingerprint and QAMS
Hui LIANG ; Xiaojun PAN ; Wenhui YANG ; Weisheng LYU ; Yuqin LUO ; Jiaxuan WU ; Mei WEI ; Xueren CHENG ; Xiaoyong LAN ; Zhenyu LI
China Pharmacy 2021;32(15):1842-1848
OBJECTIVE:To establish the UPLC fingerprint of Polygonum cuspidatum ,and to determine the contents of four active ingredients and to provide reference for the quality evaluation of P. cuspidatum . METHODS :The determination was performed on Waters BEH C 18 column(100 mm×2.1 mm,1.7 μm)with mobile phase consisted of acetonitrile- 0.2% formic acid (gradient elution )at flow rate of 0.4 mL/min. The column temperature was 40 ℃,and detection wavelength was 290 nm. The sample size was 1 μL. The fingerprints were evaluated by similarity calculation,cluster analysis and orthogonal partial least square discriminant analysis (OPLS-DA). Using polydatin as internal standard ,relative calibration factors of resveratrol ,emodin-8-O- β-D-glucoside and emodin were determined to develop a method of QAMS. The contents of 4 above components in 15 batches of P. cuspidatum were calculated by relative calibration factors. The results of QAMS were compared with those of external standard. RESULTS:UPLC fingerprints of 15 batches of P. cuspidatum were established ,and 12 common peaks were confirmed. Five components were identified ,i.e. polydatin ,resveratrol,emodin-8-O-β-D-glucoside,emodin,emodin methyl ether. The fingerprint similarity of 15 batches of P. cuspidatum was in the range of 0.865-0.976. According to cluster analysis ,15 batches of P. cuspidatum were classified into 4 categories,showing certain regularity of origin. Seven markers were identified by OPLS-DA method. The order of difference significance was peak 7>emodin-8-O-β-D-glucoside>resveratrol>peak 8>polydatin>peak 1> peak 10. The relative deviation among the contents of resveratrol ,emodin-8-O-β-D-glucoside and emodin in 15 batches of P. cuspidatum determined by QAMS and external standard method was less than 5.0%,indicating that there was no significant difference between the two methods. CONCLUSIONS :UPLC fingerprint combined with QAMS method is convenient and reliable for the quality evaluation of P. cuspidatum ;the quality of P. cuspidatum produced in Chongqing and Anhui province is better.
2.Identification and Study on Processing End-point of Raw and Processed Products of Morus alba Based on UPLC Fingerprint and Chromaticity
Mengting HUANG ; Ling PAN ; Lihong DENG ; Mingyan XIE ; Yongfu MA ; Mei WEI ; Xueren CHENG ; Jie XU
China Pharmacy 2021;32(1):56-63
OBJECTIVE:To provide reference for the identification and proces sing end-point determination of raw Morus alba and its processed products (honey-processed M. alba ). METHODS :UPLC method was adopted. The determination was performed on Waters BEH Shield RP C 18 column with mobile phase consisted of acetonitrile- 0.1% phosphoric acid solution (gradient elution ) at the flow rate of 0.30 mL/min. The column temperature was set at 30 ℃. The program wavelengths were set at 280 nm(0-4 min) and 320 nm(4-35 min). Similarity Evaluation System for Chromatogram Fingerprint of TCM (2012 edition)was used to establish UPLC fingerprint and carry out similarity evaluation of 13 batches of M. alba and honey-processed M. alba . The chromatographic peaks were identified with reference substance fingerprint. The colorimetric value (L,a,b) of 13 batches of M. alba and honey-processed M. alba powder were determined ,and average total colorimetric value (E)was calculated. OPLS-DA and cluster analysis were adopted to analyze the differences in fingerprints and colorimetric values of M. alba before and after processing. At the same time ,the dynamic change rule of fingerprint and colorimetric value of honey-processed M. alba at different processing time points were analyzed to determine the processing end-point. RESULTS :There were obvious differences in fingerprints before and after processing ,and the similarity of 13 batches of M. alba and honey-processed M. alba were all higher than 0.9. Totally 21 common peaks were calibrated for M. alba ,and 23 common peaks for honey-processed M. alba ;peak 1 and peak 2 were newly produced compounds of honey-processed M. alba . Peak 2,peak 7,peak 14 and peak 19 were identified as 5-hydroxymethylfurfural, mulberry glucoside A ,oxidized resveratrol ,mulberry flavonoids G. Results of OPLS-DA showed that the peak area-sample quantity ratio of peak 1,peak 2,peak 18,peak 20 and the chromaticity values (L,a,b)were the most important factors affecting the difference of raw and processed products of M. alba . When the E ranged 75.84-80.88 as the processing end-point of honey-processed M. alba ,the processing time was determined as 22-34 min. CONCLUSIONS : The established UPLC fingerprint and colorimetric value determination method can be used to identify the raw and processed products of M. alba as well as determine the processing end-point of honey-processed M. alba .
3.Research on quality difference of standard decoction of raw and fried Paeoniae Radix Alba based on fingerprint and multicomponent determination.
Li GAN ; Yu-Jing YAN ; Qing DING ; Wan-Min HONG ; Yu-Hua JI ; Xiao-Dong YANG ; Liao-Yuan LIU ; Mei WEI
China Journal of Chinese Materia Medica 2021;46(6):1410-1416
The extract rates, multicomponent content and fingerprint were determined in this study to investigate the quality diffe-rence between standard decoction of raw Paeoniae Radix Alba and fried Paeoniae Radix Alba. UPLC fingerprint was established for 17 batches of standard decoction of raw and fried Paeoniae Radix Alba, and the contents of gallic acid, catechin, albiflorin, paeoniflorin and benzoyl paeoniflorin were determined. The peak areas of standard decoction were analyzed by the independent t-test and orthogonal partial least squares discriminant analysis. There was no significant difference in extract rates between the standard decoction of raw and fried Paeoniae Radix Alba. After fried processing, the content of albiflorin increased by 0.26%, while the contents of gallic acid, catechin, paeoniflorin and benzoyl paeoniflorin decreased by 13.04%, 27.97%, 10.30% and 18.79% respectively. There were 14 common peaks in the fingerprint of standard decoction of raw Paeoniae Radix Alba, and 16 common peaks in the fried Paeoniae Radix Alba. Peak 1 and peak 3 were new ones after processing, among which the peak 3 was 5-hydroxymethylfurfural. The results showed that peak 1, peak 3, peak 11 and peak 15 were the key compounds to distinguish standard decoction of raw and fried Paeoniae Radix Alba. In conclusion, this method is stable and can be used for the study of quantity transfer and quality control in the preparation process of standard decoction, granules and other dosage forms for raw and fried Paeoniae Radix Alba, providing reference for the identification of raw and fried Paeoniae Radix Alba and related preparations.
Chromatography, High Pressure Liquid
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Drugs, Chinese Herbal
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Paeonia
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Quality Control
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Reference Standards
4.Study on Correlation of Chromaticity Value with Multiple Indicators in Schizonepeta tenui folia Charcoal of Different Processing Time
Tian TIAN ; Banggui PENG ; Jie XU ; Wanmin HONG ; Lufang LIU ; Haibing HE ; Mei WEI
China Pharmacy 2021;32(12):1466-1472
OBJECTIVE:To study the co rrelation of the chro maticity value of Schizonepeta tenuifolia charcoal of different processing time(0-40 min,similarly herein after)with multiple indicators ,and to reveal the quality change law of S. tenuifolia charcoal during processing and confirm the terminal time. METHODS :The contents of ethanol-soluble extracts from S. tenuifolia charcoal decoction pieces of different processing time were determined. UPLC fingerprint of S. tenuifolia decoction pieces and S. tenuifolia charcoal decoction pieces of different processing time were established ,and the similarity evaluation was also conducted. The chromatographic peaks were confirmed by comparison with substance control. The same UPLC conditions were used to determine the contents of index components (hesperidin,rosmarinic acid ,menthone)in S. tenuifolia charcoal decoction pieces of different processing time. The colorimetric method was used to measure the chromaticity value of S. tenuifolia charcoal decoction pieces of different processing time. Meanwhile ,sample of processing 0 min was used as a control to calculate the total color value (E)and the total color difference value (ΔE). Pearson correlation analysis ,cluster analysis and orthogonal partial least squares discriminant analysis (OPLS-DA)were performed on the ethanol-soluble extracts ,index component contents ,chromatographic peak area and chromaticity value. The terminal time of processing S. tenuifolia charcoal was conf irmed,and validation test was also conducted. RESULTS :With the extension of processing time , the content of ethanol-soluble extract in S. tenuifolia charcoal qq.com decoction pieces gradually decreased. A total of 17 chromato- graphic peaks were identified in 12 batches of S. tenuifolia decoction piece ,and its si milarity with the control fingerprint was greater than 0.9. 21 chromatographic peaks were identified in S. tenuifolia charcoal decoction pieces of different processing time,and its similarity with the chromatogram of sample of processing 0 min decreased with the processing time ,and the similarity after 18 min was lower than 0.9. The chromatographic peak 9 was hesperidin ,peak 10 was rosmarinic acid and peak 17 was menthone. The determination of content and chromaticity value showed that with the extension of processing time ,the contents of hesperidin ,rosmarinic acid and menthone decreased gradually ;the color L,b and E values of S. tenuifolia charcoal decoction piece powder decreased gradually ,and the a and ΔE values increased gradually. Pearson correlation analysis showed that the contents of ethanol-soluble extract ,hesperidin,rosmarinic acid and menthone ,the peak areas of 15 chromatographic peaks (peak 2,7-15,17-21)were significantly positively correlated with E value(P<0.01);the peak areas of 5 chromatographic peaks (peak 1,3-6)were significantly negatively correlated with E value(P<0.01),but peak area of peak 16 was not related to E value(P> 0.05). Results of cluster analysis showed that S. tenuifolia charcoal decoction pieces of different processing time were divided into 2 categories;the first category was processed for 0-16 min,and the second category was processed for 18-40 min. The results of OPLS-DA showed that the VIP values of peak 6 area(2.800 75),L value(2.327 54),peak 3 area(1.793 39),b value(1.735 78) and peak 5 area(1.244 04)were greater than 1. The final processing time of S. tenuifolia charcoal was 18 min. The results of validation experiment showed that the L,a and b values of S. tenuifolia charcoal decoction piece were 20.22-22.00,4.44-7.67, 9.78-13.00,and ΔE were 13.50-14.12,respectively. CONCLUSIONS :The chromaticity value of S. tenuifolia charcoal decoction pieces of different processing time is closely related to the contents of ethanol-soluble extract ,hesperidin,rosmarinic acid , menthone and the area of 20 chromatographic peaks. It is suggested that the terminal time of processing S. tenuifolia is 18 min.
5.Comparison of Chemical Constituents of Sinapis alba before and after Stir-frying Based on UPLC-MS and Chemometrics Methods
Xiaozhou JIA ; Xiaolong YANG ; Xiaoying LU ; Yueyi LIANG ; Minyou HE ; Xiangdong CHEN ; Mei WEI ; Dongmei SUN ; Zhenyu LI
China Pharmacy 2021;32(22):2731-2735
OBJECTIVE:To compare the chemical components in Sinapis alba before and after stir-frying. METHODS : UPLC-Q-Exactive Obitrap MS was adopted to analyze chemical constituents of S. alba before and after stir-frying. The determination was performed on Waters CORTECS T 3 column with mobile phase consisted of methanol- 0.1% formic acid solution (gradient elution )at the flow rate of 0.25 mL/min. The column temperature was 30 ℃ and the sample size was 2 μL. High resolution MS adopted heating electrospray electron source ,positive ion scanning mode ,scanning range m/z 120-1 000. The chemical constituents of S. alba before and after stir-frying were identified by Compound Discover 3.2 software combined with relevant database ,and the content changes of chemical constituents were analyzed by using peak area. Chemometrics analysis was performed for the content changes of chemical constituents using peak area as variable. RESULTS :A total of 54 chemical components were identified in S. alba ,mainly fatty acids (represented by erucic acid ),alkaloids(represented by sinapine ), flavonoids. After stir-frying ,the contents of 19 chemical components changed significantly ,of which the contents of 10 components decreased significantly and those of 9 components increased significantly (P<0.05). Principal component analysis and orthogonal partial least squares discriminant analysis could clearly distinguish S. alba from stir-fried S. alba . CONCLUSIONS :The contents of some chemical components of S. alba change significantly after stir-frying ,which may be one of the important reasons for the change of efficacy after stir-frying.
6.Quality evaluation of Bolbostemmatis Rhizoma by UPLC fingerprint combined with QAMS.
Min-Ye HUANG ; Zhen-Yu LI ; Pei-Zhen TONG ; Si-Qiong CAO ; Mei WEI ; Dong-Mei SUN ; Li-Ye PAN ; Xiang-Dong CHEN
China Journal of Chinese Materia Medica 2020;45(14):3459-3466
The present study was performed to establish the UPLC fingerprints of Bolbostemmatis Rhizoma and determine the contents of three saponins by quantitative analysis of multi-components by single marker(QAMS), and provide basis for quality evaluation of Bolbostemmatis Rhizoma. The analysis was carried out on an analytical column of Waters Cortecs T3(2.1 mm×100 mm,1.6 μm)with gradient elution by acetonitrile-0.1% phosphoric acid solution, at a flow rate of 0.3 mL·min~(-1). The detection wavelength was 203 nm, the column temperature was 30 ℃ and the injection volume was 1 μL. The UPLC fingerprints of Bolbostemmatis Rhizoma were established and evaluated by similarity calculation, cluster analysis and principal component analysis. The relative calibration factors of toberoside B and toberoside C were determined with toberoside A as internal reference. The content was calculated by relative calibration factors to develop a method of QAMS. Comparing the results of QAMS with those of ESM, the accuracy and feasibility of one-eva-luation and multi-evaluation can be determined. RESULTS:: showed that the fingerprints of 19 batches of Bolbostemmatis Rhizoma have four common peaks with similarities ranging from 0.754 to 1.000. Cluster analysis and principal component analysis classified 19 batches of Bolbostemmatis Rhizoma into three categories, which was consistent with the similarity evaluation results. The relative deviation between the content of tubeicosides B and C in 19 batches of Bolbostemmatis Rhizoma determined by QAMS and ESM is less than 5.0%, indicating that there was no significant difference between the two methods. Therefore, the UPLC fingerprints combined with QAMS and similarity evaluation can be effectively used to evaluate the quality of Bolbostemmatis Rhizoma.
Chromatography, High Pressure Liquid
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Drugs, Chinese Herbal
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Principal Component Analysis
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Quality Control
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Rhizome
7.Chinese expert investigation on diagnosis and disease activity evaluation in Takayasu's arteritis
Xiaomin DAI ; Zhihui DONG ; Sheng CHEN ; Yongjing CHENG ; Zhanyun DA ; Shengming DAI ; Jing DONG ; Yong HOU ; Fen LI ; Xiaobing LIU ; Yifang MEI ; Yufeng QING ; Chunhua SHI ; Weihao SHI ; Qiang SHU ; Yong WANG ; Hongyan WEN ; Jian XU ; Shengqian XU ; Jing XUE ; Shuang YE ; Jian ZHU ; Lindi JIANG
Fudan University Journal of Medical Sciences 2017;44(2):127-133
Objective To investigate the current situation in Chinese rheumatologic physicians' clinical diagnosis and evaluation of Takayasu's arteritis (TA).Methods Nineteen rheumatology experts and three vascular surgery specialists in China were invited to make the nationwide investigation for the first time about the diagnosis and disease activity evaluation of TA in China,through the questionnaire survey on the internet.Weighted average was used to calculate the average scores of corresponding problems.Results Chinese experts mainly adopted 1990 American College of Rheumatology (ACR) classification criteria for clinical diagnosis of TA.In details,symptoms of age,limb claudication and amaurosis,signs including pulselessness or pulse weakening,vascular bruits,increasing bilateral pulse pressure and hypertension and acute phase reactants (APR) were critical to the clinical diagnosis of TA.Besides,noninvasive imaging examinations,such as computed tomography angiography (CTA),magnetic resonance angiography (MRA),vascular ultrasonography,and positron emission tomography (PET) were also of great importance.In the aspect of disease activity assessment,Chinese experts mainly used Kerr scoring tool.APR and noninvasive radiological examinations were considered with vital value.Some TA patients with carotid artery involvement were recommended using vascular ultrasonography,while others with pulmonary artery and thoracic/abdominal aorta trunk involvement were preferred CTA other than MRA.Conclusions APR and noninvasive imaging examinations were thought with great help to make clinical diagnosis and evaluation of TA for Chinese physicians.
8.The expression and clinical significance of proprotein convertase subtilisin kexin 9 in rheumatoid arthritis
Qing DU ; Xiaojing YU ; Hongjuan LI ; Shangqi GUAN ; Zhiyi ZHANG ; Yifang MEI
Chinese Journal of Internal Medicine 2017;56(9):655-659
Objective To assess the expression and significance of proprotein convertase subtilisin kexin 9 (PCSK9) in patients with rheumatoid arthritis (RA).Methods Sixty-five RA patients and forty-seven healthy controls were recruited in this study.The body mass index (BMI) and serum total cholesterol (TC),triglyceride (TG),high density lipoprotein (HDL),lipoprotein a,low density lipoprotein (LDL),very low density lipoprotein(VLDL),apolipoprotein A (ApoA),apolipoprotein B (ApoB) and the ratio of LDL-C/HDL-C were tested.Other parameters included disease activity score 28 (DAS28),rheumatoid factor (RF),anti-cyclic citrullinated peptide (CCP) antibody,erythrocyte sedimentation rate (ESR),c-reactive protein (CRP).Serum PCSK9 level was measured by ELISA and compared between RA patients and healthy controls.Results (1) The serum PCSK9 levels in RA patients were higher than those in healthy controls [(409.36 ±223.52) μg/L vs (292.19 ± 109.79) μg/L,P < 0.05].(2) Compared with subgroup of moderate and low active disease and patients in remission,PCSK9 was significantly higher in patients with highly active disease (P < 0.05).(3) The serum PCSK9 levels were positively correlated with RF,TC,TG,LDL,very low density lipoprotein (VLDL),ApoB,with r values as 0.303,0.490,0.320,0.451,0.319,0.463,respectively (P < 0.05).(4) Multiple stepwise regression analysis showed that DAS28,RF,TC and LDL-C/HDL-C were relevant factors for PCSK9 in RA patients.Conclusions The serum PCSK9 level is elevated in RA patients,which is related to RF,disease activity,TC,TG,LDL,VLDL,ApoB.This suggests that PCSK9 is potentially linked to inflammatory reaction and lipid metabolism in rheumatoid arthritis.
9.The application of systemic lupus erythematosus-specific quality of life questionnaire in systemic lupus erythematosus
Shuya WANG ; Wei TIAN ; Liang CHEN ; Zhiyi ZHANG ; Yifang MEI
Chinese Journal of Rheumatology 2014;18(3):190-194
Objective To elucidate the relationship between quality of life (QOL) and disease activity of systemic lupus erythematosus (SLE),as well as to reveal the factors impacting disease activity and the QOL of SLE utilizing the combination of SLE-specific quality of life questionnaire (SLEQOL) and the medical outcomes survey short form 36 (SF-36).Methods SLEQOL and SF-36 health survey questionnaire were applied.Information on gender,disease duration,age,education level were collected.Serum complement (C3 and C4) level and erythrocyte sedimentation rate (ESR) were measured.Patients were divided into inactive,mild active,moderate active and severe active respectively according to SLE disease activity index (SLEDAI).Pearson's product moment correlation coefficient was used to analyze the correlation between the activity of disease and the QOL.Multiple linear regression was employed to explore the factors which could impact on SLEQOL.Results The physical function of SLEQOL was positively correlated with SLEDAI (r=0.36; P<0.05).The association between reported health transition of SF-36 and SLEDAI was positive (r=0.19; P<0.05).Physical functioning,role-physical,role-emotional,body pain and vitality were all negatively correlated with SLEDAI (r:-0.20,-0.19,-0.19,-0.19,-0.21 respectively; P<0.05).The scores of patients with severe disease activity were significantly increased in the physical functioning of SLEQOL than other three groups (18±10 vs 11±5,12±6,13±7; P<0.05).Scores on the Health transition of patients with moderate and severe disease activity were lower than those of whom with mild disease activity (23±28.14±17 vs 34±39,P<0.05).Patients with mild or severe disease activity had lower score than those of patieuts in disease inactive (30±41,34±39 vs 44±44,P<0.05).Multiple linear regression analyses showed that disease duration and education level might be the influencing factors of SLEQOL.Conclusion QOL of patients with SLE is related to the level of disease activity and is impacted by disease duration and education.
10.Analysis of optimizing countermeasure for doctor-patient relationship based on social exchange theory
Haihong ZHANG ; Zhiyi ZHANG ; Juan ZHANG ; Yifang MEI ; Yanping ZHAO
Chinese Journal of Medical Education Research 2013;(11):1185-1188
From the perspectives of social equitable exchange theory, contents and features of exchange between medical staff and patients in the doctor-patient relationship as well as their evalua-tion on social equitable exchange theory were analyzed according to basic features of doctor-patient relationship. Suggestions were proposed from government, industry, hospital and medical staff.

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