1.Study on comprehensive quality evaluation of Sargentodoxae Caulis from different habitats
Weisheng LYU ; Cuijie WEI ; Zhenyu LI ; Hui LIANG ; Binbin SHEN ; Xiangdong CHEN ; Congyou DENG ; Xiaozhou JIA
International Journal of Traditional Chinese Medicine 2023;45(8):1004-1010
Objective:To comprehensively evaluated the quality of Sargentodoxae Caulis from different habitats with a combination of indexes and characteristic chromatogram method from Chinese Pharmcopoeia (Edition 2020). Methods:The contents of water content, total ash, ethanolic extract, sulfur dioxide residue, heavy metals and harmful elements, total phenols, chlorogenic acid, salidroside and characteristic chromatogram of 17 batches of Sargentodoxae Caulis were determined. The quality of Sargentodoxae Caulis was comprehensively evaluated by combining chemical pattern recognition method. Results:The water content, total ash content, extracts, and content determination of 17 batches of Sargentodoxae Caulis from different habitats complyed with the provisions of the Chinese Pharmcopoeia (Edition 2020). There were differences in the contents of extracts, chlorogenic acid, and salidroside, among which the content of Anhui origin was higher. A total of 8 common peaks were identified from the 17 batches samples. Conclusion:Comprehensive evaluation of multiple indicators can demonstrate the quality of Sargentodoxae Caulis more correctly, and shows that the quality of Sargentodoxae Caulis from different habitats is different. The quality of Sargentodoxae Caulis from Anhui is better than that from other habitats.
2.Quality study of Perillae caulis formula granules based on standard decotion
Jie YANG ; Weisheng LYU ; Fang CHEN ; Liping DENG ; Ruoyun SHI ; Zhiwen DUAN ; Minyou HE ; Mei WEI ; Zhenyu LI
International Journal of Traditional Chinese Medicine 2022;44(10):1144-1149
Objective:To establish the quality evaluation method of Perillae caulis formula granules based on the three kind of quality indexes of standard decoction. Methods:Eighteen batches of Perillae caulis were collected from different habitats according to different technical requirements, eighteen batches of standard decoction and three batches of formula granules were prepared and the paste-forming rates were calculated. The content of Caffeic acid and Rosmarinic acid were determined and calculated by Ultra High Performance Liquid Chromatography (UPLC). Then the fingerprints of standard decoction of and formula granules of Perillae caulis were established by UPLC . The similarity values of fingerprints between formula granules and standard decoction were calculated. Results:The average paste-forming rate of standard decoction was (7.16±1.97)%. The paste-forming rates of three batches of formula granules were 5.52%, 5.25% and 5.34%, respectively. The average content of Caffeic acid and Rosmarinic acid in standard decoction was (12.06±3.37)mg/g. The contents of three batches of formula granules were 5.52, 5.82, 5.77 mg/g, respectively. Seven common fingerprint peaks were identified in the fingerprints of standard decoction and formula granules, three of which were identified as Caffeic acid, N-Feruloyl Octopus amine and Rosmarinic acid by comparison of reference substance. The fingerprints similarity of Perillae caulis dispensing granules and standard decoction were 1.000, 0.995 and 0.997, respectively. Conclusions:The quality indexes of three batches of formulation granules are consistent with standard decoction. This method can provide basis for the establishment of quality standard of Perillae caulis dispensing granules.
3.Establishment of UPLC characteristic chromatogram of Pulsatilla chinensis and its application in origin differentiation and counterfeit identification
Guangming HE ; Rui LUO ; Heping ZENG ; Xiaoying LU ; Xiaolong YANG ; Weisheng LYU ; Yueyi LIANG ; Zhenyu LI ; Dongmei SUN ; Xiangdong CHEN
International Journal of Traditional Chinese Medicine 2024;46(6):743-749
Objective:To establish ultra performance liquid chromatography (UPLC) characteristic chromatogram of Pulsatilla chinensis; To provide reference for the origin identification and quality control of Pulsatilla chinensis. Methods:UPLC Method was adopted. The determination was performed on a column of Agilent SB C18 (2.1 mm×100 mm, 1.8 μm) . The mobile phase was acetonitrile-methanol (2:1) -0.1% phosphoric acid solution by fradient elution at a flow rate of 0.30ml/min. The column temperature was 30 ℃. The detection wavelength was 215 nm. The injection volume was 2 μl. The common counterfeit products and medicinal herbs of Pulsatilla chinensis from different areas were evaluated by comparison of characteristic chromatogram, principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA). Results:There were 9 characteristic peaks in the characteristic chromatogram of Pulsatilla chinensis, and 8 common peaks were identified by high resolution mass spectrometry and comparison of reference materials. Through PCA analysis, it was possible to clearly distinguish the medicinal herbs of Pulsatilla chinensis from different areas. Combined with OPLS-DA analysis, it was found that peak 2, peak 3, peak 6 were the main markers of Pulsatilla chinensis from different producing areas. Conclusion:The established method has good specificity, repeatability and durability, and it can effectively distinguish the common counterfeits of Pulsatilla chinensis, and provide the basis of quality control and selection of origin for Pulsatilla chinensis.
4.Study on UPLC fingerprint of Mume flos at different flowering stages based on chemometrics analysis
Shuang HUANG ; Yueyi LIANG ; Jie YANG ; Weisheng LYU ; Xiaoying LU ; Guangming HE ; Zhipeng CHEN ; Xuxuan HOU ; Tianrui XIA ; Zhenyu LI ; Congyou DENG ; Xiangdong CHEN ; Dongmei SUN
International Journal of Traditional Chinese Medicine 2024;46(7):898-904
Objective:To establish the ultra high performance liquid chromatography (UPLC) fingerprints of Mume flos at different flowering stages; To provide reference for the quality research of Mume flos.Methods:The fingerprints of Mume flos were established by UPLC method, and the common peaks were identified by high performance liquid chromatography high resolution mass spectrometry (LC-MS). Chemometrics analysis was carried out with the fingerprints' common peak area of plum blossom at different flowering stages as a variable. Semiquantitative analysis of changes in flavonoids and phenolic acids in Mume flos at different flowering stages was conduct using peak area calculation method.Results:Totally 31 common peaks were identified in the fingerprints of plum blossom medicinal materials at different flowering stages and 9 components were identified. Clustering analysis (HCA) and principal component analysis (PCA) both classified plum blossom medicinal herbs at different flowering stages into three categories. Among them, there were significant differences between the groups at the bud stage, blooming period, and final flowering period, while the differences between the groups at blooming period and final flowering period were relatively small. The orthogonal partial least squares discriminant analysis (OPLS-DA) screened 16 different components with VIP>1.0. The contents of phenolic acids in different flowering stages were as follows: bud stage>blooming period>final flowering period, while the contents of flavonoids were as follows: blooming period>final flowering period>bud stage.Conclusions:This method is simple and reliable, and can provide reference for the quality evaluation of plum blossom medicinal materials at different flowering stages.
5.Study on Quality Evaluation of Notopterygii Rhizoma et Radix through UPLC Fingerprint Combined with Chemometrics Analysis and Multi Index Component Content Determination
Guangming HE ; Xiaoying LU ; Tianrui XIA ; Feifei XIE ; Rui LUO ; Weisheng LYU ; Yueyi LIANG ; Zhenyu LI ; Xiuzhi LI ; Jianxiang ZHANG ; Xiangdong CHEN ; Dongmei SUN
Chinese Journal of Information on Traditional Chinese Medicine 2024;31(8):126-132
Objective To establish the ultra-high performance liquid chromatography(UPLC)chromatographic fingerprint of Notopterygii Rhizoma et Radix;To determine the contents of ferulic acid,nodakenin,ammijin,notopterol,isoimperatorin and volatile oil of Notopterygii Rhizoma et Radix from different producing areas;To provide reference for quality evaluation of Notopterygii Rhizoma et Radix.Methods Waters BEH C18 chromatographic column(2.1 mm×150 mm,1.7 μm)was used,with mobile phase acetonitrile-0.02%formic acid aqueous solution gradient elution,flow rate 0.25 mL/min,column temperature 25℃,detection wavelength 330 nm,injection volume 2 μL.UPLC fingerprints of 25 batches of Notopterygii Rhizoma et Radix were established,and the similarity analysis and chemometrics analysis were carried out.The contents of ferulic acid,nodakenin,ammijin,notopterol and isoimperatorin were determined simultaneously,and the contents of volatile oil was determined by steam distillation method.Results Totally 23 common fingerprint peaks were calibrated,11 known components were identified.According to the results of the cluster analysis and principal component analysis,25 batches of Notopterygii Rhizoma et Radix samples were divided into 3 categories,and the 6 potential differential components were screened out by orthogonal partial least squares-discriminant analysis(OPLS-DA).The results showed that the contents of notopterol and volatile oil from Sichuan Province were higher than those from Gansu Province and Qinghai Province.Conclusion The method established in the study is accurate and reliable,which can provide scientific basis and reference for the quality evaluation and control of Notopterygii Rhizoma et Radix.
6.Fingerprint Establishment of Rhizoma Ligustici from Different Origins and Their Chemometrics Analysis
Hui LIANG ; Xiaojun PAN ; Weisheng LYU ; Wenhui YANG ; Yuqin LUO ; Liye PAN ; Wenjie HUO ; Zhenyu LI
China Pharmacy 2021;32(19):2358-2362
OBJECTIVE:To establish UPLC fingerpri nt of Ligusticum sinense ,Ligusticum jeholense and Conioselinum vaginatium,and to conduct their chemometrics analysis so as to provide reference for the identification of Rhizoma Ligustici from different origins. METHODS :UPLC method combined with Similarity Evaluation System of TCM Chromatographic Fingerprints (2012 edition) were used to establish the fingerprints of Rhizoma Ligustici from different origins. Chromatographic peak identification and similarity evaluation were carried out. Cluster analysis (CA),principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA)were performed to analyze Rhizoma Ligustici from different origins,and screen differential components. RESULTS :Totally 13,11,11 characteristic peaks were identified in UPLC fingerprints of L. sinense ,L. jeholense and C. vaginatium ,respectively. Similarity evaluation showed that the similarity between C. vaginatium and L. jeholense were 0.312-0.541;that between C. vaginatium and L. sinense were 0.324-0.682;that between L. sinense and L. jeholense were 0.312-0.671,indicating there was great difference among Rhizoma Ligustici from different origins. CA,PCA and OPLS-DA showed that Rhizoma Ligustici from different origins were clustered into each category respectively ; chemical components represented by peak 10,peak 13,peak 12,peak 7 and peak 6 were differential components for Rhizoma Ligustici from 3 origins. CONCLUSIONS :The study establishes UPLC fingerprint of Rhizoma Ligustici from different origins , and screens 5 differential components ,which can be used to identify Rhizoma Ligustici from different origins.
7.Establishment of the fingerprint of Cnidium monnieri and a method for the content determination of 4 kinds of coumarins
Xiaojun PAN ; Weisheng LYU ; Wenhui YANG ; Yuqin LUO ; Yueyi LIANG ; Mei WEI ; Dongmei SUN ; Xiangdong CHEN ; Wenjie HUO ; Zhenyu LI
China Pharmacy 2022;33(2):185-190
OBJECTIVE To establi sh the fingerprint of Cnidium monnieri and a method for the content determination of 4 kinds of coumarins. METHODS Ultra-high performance liquid chromatography (UPLC) method was adopted to establish the fingerprints of 21 batches of C. monnieri ; their similarities were evaluated with Similarity Evaluation System of TCM Chromatographic Fingerprint (2012 edition);common peaks were identification by comparison with reference substance. Using 10 common peak areas as variables ,cluster analysis was performed for 21 batches of C. monnieri by the method of between groups. The relative correction factors of xanthotoxin ,bergapten and imperatorin were calculated by the same UPLC method with osthole as the internal reference. The contents of them were calculated by quantitative analysis of multi-components by single marker (QAMS),and compared with the results of external standard method. RESULTS Totally 10 common peaks were identified in the fingerprints of 21 batches of C. monnieri ;the similarities ranged from 0.997 to 1.000. Peak 4 was identified as xanthotoxin ,peak 8 as bergapten ,peak 9 as imperatorin and peak 10 as osthole. A total of 21 batches of samples were divided into 3 categories,of which S 7 was clustered into one category ,S14 was clustered into one category ,and the other 19 batches were clustered into one category. The relative deviations of the contents of xanthotoxin ,bergapten and imperatorin determined by QAMS and external standard method were in the range of 0.88% -1.07% ,2.22% -2.29% ,0.67% -2.93% ,respectively. CONCLUSIONS UPLC fingerprint of C. monnieri is successfully established ,and QAMS method for content determination of 4 coumarins is also established.
8.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.
9.Variations of Chemical Components in Inula japonica by UPLC-MS/MS before and after Honey-frying
Weisheng LYU ; Cuijie WEI ; Xiaojun PAN ; Wenhui YANG ; Minyou HE ; Xiangdong CHEN ; Dongmei SUN ; Mei WEI ; Zhenyu LI
China Pharmacy 2021;32(20):2478-2484
OBJECTIVE:To compare the c hemical components differences of Inula japonica before and after honey-frying. METHODS:UPLC-MS/MS method was adopted. The determination was performed on Waters ACQUITY UPLC BEH C 18 column with mobile phase consisted of 0.1% formic acid-acetonitrile (gradient elution )at the flow rate of 0.3 mL/min. The column temperature was set at 30 ℃,and sample size was 5 µL. The electrospray ion source was scanned by positive ion mode. The first order mass spectrometry scanning range was m/z 70-1 050,the second order mass spectrometry scanning range was m/z 50-1 050, and the normalized collision energy was 40,60 eV ;mass spectrum type was the peak figure ,the flow rate of sheath gas was 35 arb,the auxiliary airflow speed was 10 arb,the spray voltage was 3.80 kV,the S-lens voltage was 50 V,the heating temperature was 350 ℃,and the capillary temperature was 350 ℃. The components were identified by Qual Browser 4.1.39.1 software, referring to the online high-resolution database mzCloud and local database OTCML of high-resolution mass spectrometry of TCM , and combined with relevant literature. The principal component analysis (PCA)and orthogonal partial least squared-discriminant analysis(OPLS-DA)of I. japonica before and after honey-fried were performed by using SIMCA 14.1 statistical software ,and variable importance projection (VIP)value greater than 1 was used as the standard to screen the differential components before and after honey-frying. RESULTS :A total of 29 common chemical components were identified from I. japonica and honey-fried I. japonica,including 5 phenolic acids as 1-caffeoylquinic acid ,chlorogenic acid and 3,5-dicaffeoylquinic acid ,12 flavonoids as quercetin,luteolin and evamectin ,as well as 12 sesquiterpene lactones as 1-O-acetylinula diester ,inula bicolor lactone B and 1-O-acetyl-6-O-isobutyryl inulin. The results of PCA showed that I. japonica and honey-fried I. japonica were located on both sides of the score diagram respectively. The results of OPLS-DA showed that the VIP values of 7 components were greater than 1,which were peak 19(britanin),peak 6(quercetagitrin),peak 1(1-caffeoylquinic acid ),peak 21(vitexicarpin),peak 20(tomentosin), peak 13(spinacetin)and peak 3(daphnetin). CONCLUSIONS :After honey-fried ,the content of chemical components of I. japonica changed and decreased to a certain extent. Britanin ,quercetagitrin,1-caffeoylquinic acid ,tomentosin,vitexicarpin, spinacetin and daphnetin may be the differential components of I. japonica and honey-fried I. japonica .