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Article(id=1200860517179977945, tenantId=1146029695717560320, journalId=1189982191388893191, issueId=1200860506031518620, articleNumber=null, orderNo=null, doi=10.16438/j.0513-4870.2023-1365, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1701705600000, receivedDateStr=2023-12-05, revisedDate=1706544000000, revisedDateStr=2024-01-30, acceptedDate=null, acceptedDateStr=null, onlineDate=1764237058204, onlineDateStr=2025-11-27, pubDate=1715443200000, pubDateStr=2024-05-12, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1764237058204, onlineIssueDateStr=2025-11-27, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1764237058204, creator=13701087609, updateTime=1764237058204, updator=13701087609, issue=Issue{id=1200860506031518620, tenantId=1146029695717560320, journalId=1189982191388893191, year='2024', volume='59', issue='5', pageStart='1101', pageEnd='1508', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1764237055547, creator=13701087609, updateTime=1764241222263, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1200877982563824311, tenantId=1146029695717560320, journalId=1189982191388893191, issueId=1200860506031518620, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1200877982563824312, tenantId=1146029695717560320, journalId=1189982191388893191, issueId=1200860506031518620, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=1374, endPage=1381, ext={EN=ArticleExt(id=1200860518882865469, articleId=1200860517179977945, tenantId=1146029695717560320, journalId=1189982191388893191, language=EN, title=Determination of 19 components in Microctis Folium from different production areas based on UPLC-MS/MS, columnId=1190335348761793317, journalTitle=Acta Pharmaceutica Sinica, columnName=Original Articles, runingTitle=null, highlight=null, articleAbstract=

The paper is to establish an UPLC-MS/MS method for the simultaneous determination of 19 components in Microctis Folium from different production areas. The 50% methanol was used as extraction solvent. The Agilent ZORBAX SB C18 (150 mm × 2.1 mm, 1.8 μm) column was used; mobile phase was acetonitrile - 0.1% acetic acid with gradient elution, flow rate was 0.3 mL·min-1, colume temperature was 30 ℃, and the injection volume was 2 μL; electrospray ionizaton source was used and detected in negative ion mode. The results showed that the established UPLC-MS/MS method could well separate the 19 components, and the methodological investigation results of 19 components were good. By means of orthogonal partial least squares discriminant analysis (OPLS-DA), 28 batches of Microctis Folium samples from different production areas can be divided into three categories, Guangdong, Guangxi and Hainan are each classified into one category, and 10 signature compounds which affecting the quality differences of different production areas were screened out. The established method is accurate, reliable, sensitive and reproducible. It can provide a basis for the establishment of the quality standard of Microctis Folium, as well as for safety and quality research.

, correspAuthors=Min-you HE, authorNote=null, correspAuthorsNote=null, copyrightStatement=Copyright ©2024 Acta Pharmaceutica Sinica. All rights reserved., copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, authorCompany=null, fund=null, authors=null, authorsList=Min-you HE, Li-wei WANG, Lin LIU, Po-yu ZHANG, Jin-quan LAN, Xin-ya WAN, Zhen-yu LI, Xiang-dong CHEN, Dong-mei SUN), CN=ArticleExt(id=1200860522431246962, articleId=1200860517179977945, tenantId=1146029695717560320, journalId=1189982191388893191, language=CN, title=基于UPLC-MS/MS法比较不同产地布渣叶中19个成分含量, columnId=1190335348896011050, journalTitle=药学学报, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=

基于UPLC-MS/MS法同时测定不同产地布渣叶中19个化合物的含量。以50%甲醇为提取溶剂, 采用Agilent ZORBAX SB C18 (150 mm × 2.1 mm, 1.8 μm) 色谱柱; 以乙腈-0.1%乙酸为流动相进行梯度洗脱, 流速为0.3 mL·min-1, 柱温30 ℃, 进样量为2 μL; 采用电喷雾离子源, 在负离子模式下进行检测。结果表明, 建立的UPLC-MS/MS方法可较好地分离19个成分, 19个成分的方法学考察结果良好。通过正交偏最小二乘法-判别分析(OPLS-DA) 可将28批不同产地布渣叶样品分为3类, 广东、广西、海南各自归为一类, 并筛选出影响不同产地质量差异的10个标志性化合物。本实验所建立的方法准确、可靠、灵敏度高、重复性好, 可为布渣叶质量标准的建立及后续深入完善其质量控制体系、临床安全用药等相关研究提供依据。

, correspAuthors=何民友, authorNote=null, correspAuthorsNote=
*何民友, E-mail:
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Chin Tradit Herb Drugs (中草药), 2021, 52: 3679-3688., articleTitle=null, refAbstract=null)], funds=[Fund(id=1201106659960648167, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, awardId=2022-230-221, language=CN, fundingSource=国家工信部2022年产业技术基础公共服务平台项目-中药全产业链质量技术服务平台(2022-230-221), fundOrder=null, country=null), Fund(id=1201106660208112113, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, awardId=null, language=CN, fundingSource=2022年佛山市南海区重点领域科技攻关专项, fundOrder=null, country=null)], companyList=[AuthorCompany(id=1201106646928945917, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, xref=null, ext=[AuthorCompanyExt(id=1201106646954111743, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, companyId=1201106646928945917, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Guangdong Yi Fang Pharmaceutical Co., Ltd., Guangdong Provincial Key Laboratory of Traditional Chinese Medicine Formula Granule, Foshan 528244, China), AuthorCompanyExt(id=1201106646979277567, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, companyId=1201106646928945917, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=广东一方制药有限公司, 广东省中药配方颗粒企业重点实验室, 广东 佛山 528244)])], figs=[ArticleFig(id=1201106655695040786, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=EN, label=null, caption=null, figureFileSmall=4pxP4Co1lkNDfX9KUx3EtQ==, figureFileBig=tns0SZUhsyjLFdnNskYN0w==, tableContent=null), ArticleFig(id=1201106655959281952, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=CN, label=Figure 1, caption= TIC chromatograms of mixed standard solutions (A, B), Microctis Folium sample solution (C), and blank solution (D). 1: Caffeic acid; 2: Procyanidin B2; 3: Epicatechin; 4: Vicenin-2; 5: 4-Hydroxycinnamic acid; 6: Ferulic acid; 7: Schaftoside; 8: Isoschafutaside; 9: Vvitexin; 10: Yphaneoside; 11: Isovitexin; 12: Rutin; 13: Isoquercitrin; 14: Isorhamnetin-3-<i>O</i>-nehesperidine; 15: Kaempferol-3-<i>O</i>-rutinoside; 16: Astragalin; 17: Narcissoside; 18: Isorhamnetin-3-<i>O</i>-glucoside; 19: Tiliroside , figureFileSmall=4pxP4Co1lkNDfX9KUx3EtQ==, figureFileBig=tns0SZUhsyjLFdnNskYN0w==, tableContent=null), ArticleFig(id=1201106656168997169, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=EN, label=null, caption=null, figureFileSmall=sviV426lGbaZBVN39PnY/Q==, figureFileBig=/OIZUteOkgV0yn0sEUNpHg==, tableContent=null), ArticleFig(id=1201106656399683898, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=CN, label=Figure 2, caption= Orthogonal partial least squares discriminant analysis model permutation test diagram , figureFileSmall=sviV426lGbaZBVN39PnY/Q==, figureFileBig=/OIZUteOkgV0yn0sEUNpHg==, tableContent=null), ArticleFig(id=1201106656680702281, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=EN, label=null, caption=null, figureFileSmall=OQT3WGAQa2gf5pf6SQNiLw==, figureFileBig=ii6U+YHMKHH+f1Zg98d0fA==, tableContent=null), ArticleFig(id=1201106656831697236, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=CN, label=Figure 3, caption= Orthogonal partial least squares discriminant analysis scores diagram , figureFileSmall=OQT3WGAQa2gf5pf6SQNiLw==, figureFileBig=ii6U+YHMKHH+f1Zg98d0fA==, tableContent=null), ArticleFig(id=1201106657003663713, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=EN, label=null, caption=null, figureFileSmall=b1QOBFPVjAfDdLj5hV+Ofw==, figureFileBig=vOP8y+5/T37kjuzCZN38Ew==, tableContent=null), ArticleFig(id=1201106657188213100, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=CN, label=Figure 4, caption= VIP diagram of orthogonal partial least squares discriminant analysis , figureFileSmall=b1QOBFPVjAfDdLj5hV+Ofw==, figureFileBig=vOP8y+5/T37kjuzCZN38Ew==, tableContent=null), ArticleFig(id=1201106658417144183, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
Sample No.OriginSample No.Origin
BZY01Xiashan-1, Zhanjiang, GuangdongBZY15Tanshui-1, Yangchun, Guangdong
BZY02Xiashan-2, Zhanjiang, GuangdongBZY16Tanshui-2, Yangchun, Guangdong
BZY03Xiashan-3, Zhanjiang, GuangdongBZY17Tanshui-3, Yangchun, Guangdong
BZY04Suixi-1, Zhanjiang, GuangdongBZY18Bajia-1, Yangchun, Guangdong
BZY05Suixi-2, Zhanjiang, GuangdongBZY19Bajia-2, Yangchun, Guangdong
BZY06Suixi-3, Zhanjiang, GuangdongBZY20Yulin-1, Guangxi
BZY07Xingning-1, Meizhou, GuangdongBZY21Yulin-2, Guangxi
BZY08Xingning-2, Meizhou, GuangdongBZY22Yulin-3, Guangxi
BZY09Xingning-3, Meizhou, GuangdongBZY23Qinzhou-1, Guangxi
BZY10Yangxi-1, Yangjiang, GuangdongBZY24Qinzhou-2, Guangxi
BZY11Yangxi-2, Yangjiang, GuangdongBZY25Qinzhou-3, Guangxi
BZY12Yangxi-3, Yangjiang, GuangdongBZY26Wuzhishan-1, Hainan
BZY13Yangxi-4, Yangjiang, GuangdongBZY27Wuzhishan-2, Hainan
BZY14Yangxi-5, Yangjiang, GuangdongBZY28Wuzhishan-3, Hainan
), ArticleFig(id=1201106658622665089, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=CN, label=Table 1, caption=

Origin information of Microctis Folium samples

, figureFileSmall=null, figureFileBig=null, tableContent=
Sample No.OriginSample No.Origin
BZY01Xiashan-1, Zhanjiang, GuangdongBZY15Tanshui-1, Yangchun, Guangdong
BZY02Xiashan-2, Zhanjiang, GuangdongBZY16Tanshui-2, Yangchun, Guangdong
BZY03Xiashan-3, Zhanjiang, GuangdongBZY17Tanshui-3, Yangchun, Guangdong
BZY04Suixi-1, Zhanjiang, GuangdongBZY18Bajia-1, Yangchun, Guangdong
BZY05Suixi-2, Zhanjiang, GuangdongBZY19Bajia-2, Yangchun, Guangdong
BZY06Suixi-3, Zhanjiang, GuangdongBZY20Yulin-1, Guangxi
BZY07Xingning-1, Meizhou, GuangdongBZY21Yulin-2, Guangxi
BZY08Xingning-2, Meizhou, GuangdongBZY22Yulin-3, Guangxi
BZY09Xingning-3, Meizhou, GuangdongBZY23Qinzhou-1, Guangxi
BZY10Yangxi-1, Yangjiang, GuangdongBZY24Qinzhou-2, Guangxi
BZY11Yangxi-2, Yangjiang, GuangdongBZY25Qinzhou-3, Guangxi
BZY12Yangxi-3, Yangjiang, GuangdongBZY26Wuzhishan-1, Hainan
BZY13Yangxi-4, Yangjiang, GuangdongBZY27Wuzhishan-2, Hainan
BZY14Yangxi-5, Yangjiang, GuangdongBZY28Wuzhishan-3, Hainan
), ArticleFig(id=1201106658782048656, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
No.CompoundtR/minParent ion (m/z)Daughter ion (m/z)DP/VCE/V
1Caffeic acid7.48179.03135.04*3013
134.0413
2Procyanidin B28.55577.14289.07*4845
125.0230
3Epicatechin10.15289.07245.08*5015
109.0325
4Vicenin-212.80593.15353.07*7537
383.0837
54-Hydroxycinnamic acid13.19163.04119.05*3013
120.0513
6Ferulic acid17.23193.05134.04*3015
137.0215
7Schaftoside18.49563.14353.07*7040
383.0840
8Isoschafutaside22.82563.14353.07*7040
383.0840
9Vitexin23.17431.10311.06*4522
283.0633
10Typhaneoside24.26769.22314.04*8545
299.0265
11Isovitexin24.45431.10311.06*4520
341.0720
12Rutin25.03609.15300.03*7542
271.0265
13Isoquercitrin26.06463.09300.03*5530
271.0250
14Isorhamnetin-3-O-nehesperidine27.55623.16314.04*7535
271.0260
15Kaempferol-3-O-rutinoside32.12593.15284.03*6038
285.0440
16Astragalin33.18447.09284.03*5028
255.0342
17Narcissoside34.12623.16315.05*6530
299.0250
18Isorhamnetin-3-O-glucoside35.37477.10314.04*6030
243.0342
19Tiliroside43.72593.13284.03*6035
255.0360
), ArticleFig(id=1201106658933043612, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=CN, label=Table 2, caption=

UPLC-MS/MS parameters of each component. DP: Declustering potential; CE: Collision energy. "*" is quantitative ion

, figureFileSmall=null, figureFileBig=null, tableContent=
No.CompoundtR/minParent ion (m/z)Daughter ion (m/z)DP/VCE/V
1Caffeic acid7.48179.03135.04*3013
134.0413
2Procyanidin B28.55577.14289.07*4845
125.0230
3Epicatechin10.15289.07245.08*5015
109.0325
4Vicenin-212.80593.15353.07*7537
383.0837
54-Hydroxycinnamic acid13.19163.04119.05*3013
120.0513
6Ferulic acid17.23193.05134.04*3015
137.0215
7Schaftoside18.49563.14353.07*7040
383.0840
8Isoschafutaside22.82563.14353.07*7040
383.0840
9Vitexin23.17431.10311.06*4522
283.0633
10Typhaneoside24.26769.22314.04*8545
299.0265
11Isovitexin24.45431.10311.06*4520
341.0720
12Rutin25.03609.15300.03*7542
271.0265
13Isoquercitrin26.06463.09300.03*5530
271.0250
14Isorhamnetin-3-O-nehesperidine27.55623.16314.04*7535
271.0260
15Kaempferol-3-O-rutinoside32.12593.15284.03*6038
285.0440
16Astragalin33.18447.09284.03*5028
255.0342
17Narcissoside34.12623.16315.05*6530
299.0250
18Isorhamnetin-3-O-glucoside35.37477.10314.04*6030
243.0342
19Tiliroside43.72593.13284.03*6035
255.0360
), ArticleFig(id=1201106659079844264, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
CompoundRegression equationrLinear range/μg·mL-1LOQ/ng·mL-1LOD/ng·mL-1
Caffeic acidY = 1 367.23X - 20.780.999 60.206-10.3190.103 20.020 6
Procyanidin B2Y = 186.78X + 91.870.999 82.448-61.1990.153 00.045 9
EpicatechinY = 48.19X + 209.140.996 43.992-199.5990.099 80.033 3
Vicenin-2Y = 2 028.64X + 229.590.998 80.205-5.1350.102 70.020 5
4-Hydroxycinnamic acidY = 545.45X - 86.560.995 90.203-5.0640.101 30.033 8
Ferulic acidY = 879.31X - 124.260.998 20.203-10.1440.020 30.006 8
SchaftosideY = 1 545.59X + 120.540.999 60.205-10.2630.102 60.034 2
IsoschafutasideY = 1 291.65X + 737.450.999 20.504-25.1940.050 40.001 7
VitexinY = 1 992.41X + 7 606.010.995 31.500-75.0240.075 00.015 0
TyphaneosideY = 3 480.32X + 651.140.999 40.603-30.1500.120 60.040 2
IsovitexinY = 1 897.28X + 2 663.830.997 51.005-50.2540.100 50.033 5
RutinY = 4 168.39X + 962.020.999 80.404-20.2070.010 10.003 4
IsoquercitrinY = 2 534.90X + 302.360.999 70.420-20.9760.042 00.014 0
Isorhamnetin-3-O-nehesperidineY = 3 654.74X + 1 196.790.999 60.418-20.8770.083 50.027 8
Kaempferol-3-O-rutinosideY = 2 827.71X + 1 661.220.999 31.005-50.2350.100 50.020 1
AstragalinY = 2 861.84X + 87.660.999 40.205-10.2510.102 50.034 2
NarcissosideY = 2 155.58X + 7 581.830.997 62.006-100.3150.200 60.066 9
Isorhamnetin-3-O-glucosideY = 2 591.73X + 2 721.200.997 41.013-50.6250.101 30.033 8
TilirosideY = 3 904.58X + 3 818.860.996 90.399-19.9720.039 90.012 0
), ArticleFig(id=1201106659251810742, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=CN, label=Table 3, caption=

Regression equations, linear range, limit of quantitation (LOQ) and limit of detection (LOD) of 19 compounds

, figureFileSmall=null, figureFileBig=null, tableContent=
CompoundRegression equationrLinear range/μg·mL-1LOQ/ng·mL-1LOD/ng·mL-1
Caffeic acidY = 1 367.23X - 20.780.999 60.206-10.3190.103 20.020 6
Procyanidin B2Y = 186.78X + 91.870.999 82.448-61.1990.153 00.045 9
EpicatechinY = 48.19X + 209.140.996 43.992-199.5990.099 80.033 3
Vicenin-2Y = 2 028.64X + 229.590.998 80.205-5.1350.102 70.020 5
4-Hydroxycinnamic acidY = 545.45X - 86.560.995 90.203-5.0640.101 30.033 8
Ferulic acidY = 879.31X - 124.260.998 20.203-10.1440.020 30.006 8
SchaftosideY = 1 545.59X + 120.540.999 60.205-10.2630.102 60.034 2
IsoschafutasideY = 1 291.65X + 737.450.999 20.504-25.1940.050 40.001 7
VitexinY = 1 992.41X + 7 606.010.995 31.500-75.0240.075 00.015 0
TyphaneosideY = 3 480.32X + 651.140.999 40.603-30.1500.120 60.040 2
IsovitexinY = 1 897.28X + 2 663.830.997 51.005-50.2540.100 50.033 5
RutinY = 4 168.39X + 962.020.999 80.404-20.2070.010 10.003 4
IsoquercitrinY = 2 534.90X + 302.360.999 70.420-20.9760.042 00.014 0
Isorhamnetin-3-O-nehesperidineY = 3 654.74X + 1 196.790.999 60.418-20.8770.083 50.027 8
Kaempferol-3-O-rutinosideY = 2 827.71X + 1 661.220.999 31.005-50.2350.100 50.020 1
AstragalinY = 2 861.84X + 87.660.999 40.205-10.2510.102 50.034 2
NarcissosideY = 2 155.58X + 7 581.830.997 62.006-100.3150.200 60.066 9
Isorhamnetin-3-O-glucosideY = 2 591.73X + 2 721.200.997 41.013-50.6250.101 30.033 8
TilirosideY = 3 904.58X + 3 818.860.996 90.399-19.9720.039 90.012 0
), ArticleFig(id=1201106659369251263, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
Sample No.Caffeic acidProcyanidin B2EpicatechinVicenin-24-Hydroxycinnamic acidFerulic acidSchaftosideIsoschafutasideVitexinTyphaneosideIsovitexinRutinIsoquercitrinIsorhamnetin-3-O-nehesperidineKaempferol-3-O-rutinosideAstragalinNarcissosideIsorhamnetin-3-O-glucosideTiliroside
BZY010.072.561.650.150.090.130.070.210.420.410.600.140.150.180.920.192.060.880.54
BZY020.092.571.670.330.060.190.080.430.300.000.560.250.140.001.190.152.860.660.23
BZY030.042.252.180.190.160.130.090.280.570.300.770.130.100.101.000.201.660.720.87
BZY040.032.681.900.220.120.120.110.310.860.351.260.260.200.161.090.202.460.980.82
BZY050.042.501.650.270.120.130.110.360.710.311.020.280.170.101.260.202.791.050.77
BZY060.042.071.310.270.100.110.110.360.940.231.280.260.160.051.160.172.780.920.66
BZY070.041.490.740.210.040.100.080.280.540.270.720.250.230.110.880.182.230.970.40
BZY080.052.162.380.180.180.150.090.230.900.421.190.160.140.110.870.221.630.780.86
BZY090.051.810.910.180.040.110.070.230.510.370.710.260.240.110.800.172.060.860.31
BZY100.010.260.090.180.050.050.090.280.620.120.650.130.110.040.710.121.540.510.23
BZY110.010.420.170.260.100.070.110.390.440.120.500.080.050.040.750.121.840.590.27
BZY120.010.760.200.290.110.070.110.430.760.150.910.130.080.030.830.142.100.730.48
BZY130.050.900.360.120.130.120.100.160.970.201.180.130.110.090.720.142.080.750.41
BZY140.031.060.370.340.140.120.140.480.650.230.860.220.200.131.060.202.741.110.39
BZY150.041.610.740.180.030.110.090.250.370.130.610.400.440.040.920.162.771.190.20
BZY160.062.461.390.150.040.110.080.210.560.150.870.400.440.050.890.142.400.940.22
BZY170.091.961.580.120.060.140.050.170.260.010.400.260.310.010.840.121.950.820.12
BZY180.072.982.040.180.040.140.110.240.560.190.910.460.450.041.000.162.640.950.23
BZY190.072.021.190.140.040.130.060.190.470.180.760.310.320.060.910.152.330.880.20
BZY200.063.774.030.200.050.120.050.250.310.790.560.190.070.180.700.091.440.450.11
BZY210.053.533.690.180.050.100.050.231.620.790.530.170.070.140.670.091.340.420.14
BZY220.043.833.540.140.030.120.060.200.490.000.730.180.080.000.960.122.050.500.13
BZY230.063.173.030.270.050.110.090.330.690.411.020.260.210.131.080.182.550.970.39
BZY240.033.801.960.170.020.030.030.160.170.300.310.390.270.040.940.072.750.570.10
BZY250.023.892.320.160.020.020.050.200.390.040.600.160.150.010.730.071.920.500.11
BZY260.025.237.640.260.000.030.080.340.340.070.570.470.380.061.410.262.480.960.43
BZY270.104.557.800.240.040.140.120.631.000.311.150.640.560.051.470.273.712.370.36
BZY280.084.235.830.160.020.080.080.240.730.351.110.810.880.031.140.243.601.900.17
Aveg.0.052.522.230.210.070.110.080.290.610.260.800.280.240.070.960.162.310.890.36
), ArticleFig(id=1201106659537023435, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1200860517179977945, language=CN, label=Table 4, caption=

Results of content determination of 19 compounds (mg·g-1)

, figureFileSmall=null, figureFileBig=null, tableContent=
Sample No.Caffeic acidProcyanidin B2EpicatechinVicenin-24-Hydroxycinnamic acidFerulic acidSchaftosideIsoschafutasideVitexinTyphaneosideIsovitexinRutinIsoquercitrinIsorhamnetin-3-O-nehesperidineKaempferol-3-O-rutinosideAstragalinNarcissosideIsorhamnetin-3-O-glucosideTiliroside
BZY010.072.561.650.150.090.130.070.210.420.410.600.140.150.180.920.192.060.880.54
BZY020.092.571.670.330.060.190.080.430.300.000.560.250.140.001.190.152.860.660.23
BZY030.042.252.180.190.160.130.090.280.570.300.770.130.100.101.000.201.660.720.87
BZY040.032.681.900.220.120.120.110.310.860.351.260.260.200.161.090.202.460.980.82
BZY050.042.501.650.270.120.130.110.360.710.311.020.280.170.101.260.202.791.050.77
BZY060.042.071.310.270.100.110.110.360.940.231.280.260.160.051.160.172.780.920.66
BZY070.041.490.740.210.040.100.080.280.540.270.720.250.230.110.880.182.230.970.40
BZY080.052.162.380.180.180.150.090.230.900.421.190.160.140.110.870.221.630.780.86
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基于UPLC-MS/MS法比较不同产地布渣叶中19个成分含量
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何民友 * , 王利伟 , 刘林 , 张珀瑜 , 蓝金权 , 万欣亚 , 李振雨 , 陈向东 , 孙冬梅
药学学报 | 研究论文 2024,59(5): 1374-1381
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药学学报 | 研究论文 2024, 59(5): 1374-1381
基于UPLC-MS/MS法比较不同产地布渣叶中19个成分含量
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何民友* , 王利伟, 刘林, 张珀瑜, 蓝金权, 万欣亚, 李振雨, 陈向东, 孙冬梅
作者信息
  • 广东一方制药有限公司, 广东省中药配方颗粒企业重点实验室, 广东 佛山 528244

通讯作者:

*何民友, E-mail:
Determination of 19 components in Microctis Folium from different production areas based on UPLC-MS/MS
Min-you HE* , Li-wei WANG, Lin LIU, Po-yu ZHANG, Jin-quan LAN, Xin-ya WAN, Zhen-yu LI, Xiang-dong CHEN, Dong-mei SUN
Affiliations
  • Guangdong Yi Fang Pharmaceutical Co., Ltd., Guangdong Provincial Key Laboratory of Traditional Chinese Medicine Formula Granule, Foshan 528244, China
出版时间: 2024-05-12 doi: 10.16438/j.0513-4870.2023-1365
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摘要
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基于UPLC-MS/MS法同时测定不同产地布渣叶中19个化合物的含量。以50%甲醇为提取溶剂, 采用Agilent ZORBAX SB C18 (150 mm × 2.1 mm, 1.8 μm) 色谱柱; 以乙腈-0.1%乙酸为流动相进行梯度洗脱, 流速为0.3 mL·min-1, 柱温30 ℃, 进样量为2 μL; 采用电喷雾离子源, 在负离子模式下进行检测。结果表明, 建立的UPLC-MS/MS方法可较好地分离19个成分, 19个成分的方法学考察结果良好。通过正交偏最小二乘法-判别分析(OPLS-DA) 可将28批不同产地布渣叶样品分为3类, 广东、广西、海南各自归为一类, 并筛选出影响不同产地质量差异的10个标志性化合物。本实验所建立的方法准确、可靠、灵敏度高、重复性好, 可为布渣叶质量标准的建立及后续深入完善其质量控制体系、临床安全用药等相关研究提供依据。

布渣叶  /  UPLC-MS/MS  /  含量测定  /  统计学分析  /  黄酮类  /  酚酸类

The paper is to establish an UPLC-MS/MS method for the simultaneous determination of 19 components in Microctis Folium from different production areas. The 50% methanol was used as extraction solvent. The Agilent ZORBAX SB C18 (150 mm × 2.1 mm, 1.8 μm) column was used; mobile phase was acetonitrile - 0.1% acetic acid with gradient elution, flow rate was 0.3 mL·min-1, colume temperature was 30 ℃, and the injection volume was 2 μL; electrospray ionizaton source was used and detected in negative ion mode. The results showed that the established UPLC-MS/MS method could well separate the 19 components, and the methodological investigation results of 19 components were good. By means of orthogonal partial least squares discriminant analysis (OPLS-DA), 28 batches of Microctis Folium samples from different production areas can be divided into three categories, Guangdong, Guangxi and Hainan are each classified into one category, and 10 signature compounds which affecting the quality differences of different production areas were screened out. The established method is accurate, reliable, sensitive and reproducible. It can provide a basis for the establishment of the quality standard of Microctis Folium, as well as for safety and quality research.

Microctis Folium  /  UPLC-MS/MS  /  content determination  /  statistical analysis  /  flavonoid  /  phenolic acid
何民友, 王利伟, 刘林, 张珀瑜, 蓝金权, 万欣亚, 李振雨, 陈向东, 孙冬梅. 基于UPLC-MS/MS法比较不同产地布渣叶中19个成分含量. 药学学报, 2024 , 59 (5) : 1374 -1381 . DOI: 10.16438/j.0513-4870.2023-1365
Min-you HE, Li-wei WANG, Lin LIU, Po-yu ZHANG, Jin-quan LAN, Xin-ya WAN, Zhen-yu LI, Xiang-dong CHEN, Dong-mei SUN. Determination of 19 components in Microctis Folium from different production areas based on UPLC-MS/MS[J]. Acta Pharmaceutica Sinica, 2024 , 59 (5) : 1374 -1381 . DOI: 10.16438/j.0513-4870.2023-1365
正文
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布渣叶又名破布叶、麻布叶、蓑衣子等, 为椴树科植物破布叶Microcos paniculata L.的干燥叶[1, 2]。布渣叶主要分布在我国岭南地区, 为岭南特色药、食两用植物, 是两广地区多种凉茶类保健食品的主要原料之一, 在民间有“凉茶瑰宝”美誉[3, 4]。布渣叶早载于清代何克谏所撰的岭南中草药专著《生草药性备要》: “味酸, 性平, 无毒, 解一切蛊胀, 清黄气, 消热毒。作茶饮, 去食积。”充分阐明了其具有消食化滞, 清热利湿退黄等作用, 可用于饮食积滞、感冒发热、湿热黄疸[5]。现代药理研究及临床应用表明, 布渣叶具有调血脂、保护心血管、促进胃肠运动、退黄、镇痛、抗炎、抗氧化、抗衰老及杀虫等作用[6-8]。布渣叶化学成分主要有生物碱、黄酮类、三萜类、无机元素、甾体、有机酸、鞣质、酚类及糖类等成分[9-12], 其中黄酮类化合物为其主要活性成分, 具有抗炎、抗氧化、抗肿瘤、保肝、抗衰老等作用[13]。另布渣叶也含有原花青素类成分, 其具有较强的抗氧化、抗衰老等生理活性[14]。
药材的质量与其成分含量密切相关, 不同产地的布渣叶因种质资源、生长条件及采收时间等因素影响, 其成分含量存在较大的差异[15]。布渣叶含有的化学成分类型众多, 但关于布渣叶的含量指标成分测定均为黄酮类化学物, 且多集中于牡荆苷、异牡荆苷、水仙苷等, 目前尚未见酚酸类、原花青素类成分作为含量指标的研究, 且含量测定研究多采用高效液相色谱法进行测定[6, 7, 14]。中药药理药效作用的发挥是多种有效成分之间相互协同, 多靶点、多途径及整体性的作用, 发挥对机体的调节作用[16], 因而布渣叶的其他类成分亦为其药效发挥作用的基础。由于不同化合物吸收光谱不一样, 其最佳吸收波长不同, 黄酮类化合物测定多选择320 nm, 而酚酸类化合物多选择254 nm下测定, 采用高效液相同时测定多成分含量灵敏度较低且存在局限性。超高效液相色谱-三重四级杆串联质谱联用技术(UPLC-MS/MS) 具有灵敏度高、分辨率高、准确度高、选择性强、分离性能好、专属检测能力强等特点, 广泛应用于中药及其复方制剂复杂化学成分的定性研究、靶向定量分析、中药质量控制和药代动力学等方面的研究[17-19]。故本研究采用UPLC-MS/MS法测定布渣叶中19个成分的含量, 包括黄酮类、酚酸类和原花青素类化合物, 并结合化学计量学对不同产地布渣叶进行比较分析和综合评价, 为布渣叶及其相关制剂全面质量控制提供参考。
材料与方法
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仪器   Waters ACQUITY UPLC H-Class/Xevo TQD超高效液相色谱-三重四极杆质谱联用仪(美国Waters公司); Agilent ZORBAX SB C18 (150 mm × 2.1 mm, 1.8 μm) 色谱柱; XP26型百万分之一天平、ME204E型万分之一天平(瑞士梅特勒-托利多公司); KQ 500 DE型数控超声波清洗器(昆山市超声仪器有限公司); Milli-Q-Direct型超纯水系统(德国默克股份有限公司)。
样品与试剂   咖啡酸(批号110885-201703, 质量分数99.7%)、表儿茶素(批号110878-201703, 质量分数99.7%)、阿魏酸(批号110773-201915, 质量分数99.4%)、夏佛塔苷(批号111912-201703, 质量分数95.6%)、牡荆苷(批号111687-202105, 质量分数99.1%)、芦丁(批号10008-202012, 质量分数91.6%)、异槲皮苷(批号11809-201804, 质量分数97.2%)、水仙苷(批号111997-201501, 质量分数93.1%)、椴树苷(批号112000-201802, 质量分数98%) 对照品购自中国食品药品检定研究院; 原花青素B2 (批号21032902, 质量分数98.17%)、对羟基肉桂酸(批号21101401, 质量分数99.94%) 对照品购自成都普菲德生物技术有限公司; 维采宁-2 (批号DST210901-023, 质量分数99.09%)、异夏佛塔苷(批号DSTDY001901, 质量分数99.15%)、香蒲新苷(批号DST200207-024, 质量分数99.21%)、异牡荆苷(批号DSTDY005401, 质量分数98.75%)、异鼠李素-3-O-新橙皮苷(批号DSTDY007501, 质量分数98.71%)、紫云英苷(批号DSTDZ000101, 质量分数99.19%)、异鼠李素-3-O-葡萄糖苷(批号DST211203-083, 质量分数99.46%) 对照品购自乐美天医药科技有限公司, 山柰酚-3-O-芸香糖苷(批号CFS202102, 质量分数98%) 对照品购自Chem Faces公司。乙腈为色谱纯(德国默克股份有限公司); 乙酸为色谱纯(天津科密欧化学试剂有限公司); 其余试剂均为分析纯; 超纯水由Milli-Q-Direct型超纯水系统制备。实验用布渣叶样品为实地考察收集, 经广州中医药大学黄海波教授鉴定均为椴树科植物破布叶Microcos paniculata L.的干燥叶, 并经广东一方制药有限公司质量中心检测均符合药典规定, 样品产地信息详见表 1。
色谱条件   采用Agilent ZORBAX SB C18 (150 mm × 2.1 mm, 1.8 μm) 色谱柱; 流动相为乙腈(A)-0.1%乙酸溶液(B), 梯度洗脱(0~33 min, 91%~83% B; 33~37 min, 83%~75% B; 37~45 min, 75%~72% B; 45~65 min, 72%~20% B), 流速为0.3 mL·min-1, 柱温为30 ℃, 进样体积为2 μL。
质谱条件   采用电喷雾离子源(ESI); 选择负离子模式(ESI-); 毛细管电压为3.10 kV; 离子源温度为150 ℃; 锥孔气体积流量为55 L·h-1; 碰撞气流量为2.5 L·h-1; 脱溶剂气温度为500 ℃; 脱溶剂气流为900 L·h-1。质谱扫描采用多重反应检测(multiple reaction monitoring, MRM) 扫描模式。Cone参数和Collision质谱参数优化通过蠕动针泵注射的方法调谐各标准化合物。19个成分的质谱参数见表 2。
对照品溶液的配制   分别取咖啡酸、原花青素B2、表儿茶素、对羟基肉桂酸、阿魏酸、夏佛塔苷、牡荆苷、水仙苷和椴树苷对照品适量, 精密称定, 加50%甲醇制成浓度分别为10.32、10.20、99.80、10.13、10.14、10.26、25.01、10.03、9.99 μg·mL-1的混合对照品溶液A; 再分别取维采宁-2、异夏佛塔苷、香蒲新苷、异牡荆苷、芦丁、异槲皮苷、异鼠李素-3-O-新橙皮苷、山柰酚-3-O-芸香糖苷、紫云英苷和异鼠李素-3-O-葡萄糖苷对照品适量, 精密称定, 加50%甲醇制成浓度分别为10.27、25.19、10.05、25.13、10.10、10.49、10.44、25.12、10.25、25.31 μg·mL-1的混合对照品溶液B。
供试品溶液的制备   精密称取布渣叶样品粉末(过三号筛) 0.5 g, 置于具塞锥形瓶中, 加入50%甲醇25 mL, 称定重量, 加热回流30 min, 取出, 放冷, 用50%甲醇补足减失重量, 摇匀, 滤过, 取续滤液作为供试品溶液。
专属性考察   分别精密吸取混合对照品溶液(A、B)、布渣叶供试品溶液和空白溶液, 按上述色谱条件和质谱条件测定, 比较空白溶液、混合对照品溶液和供试品溶液的色谱图。
线性关系考察与定量限   分别精密吸取混合对照品溶液储备溶液0.2、0.5、1.0、2.0、5.0 mL置10 mL量瓶中, 加50%甲醇稀释至刻度, 摇匀, 用0.22 μm微孔滤膜滤过, 连同储备溶液按上述色谱条件和质谱条件进样测定。另取混合对照品溶液逐级稀释, 以信噪比为10的浓度为最低定量限(LOQ), 以信噪比为3的浓度为最低检测限(LOD)。
仪器精密度   分别精密吸取混合对照品溶液A、B, 按上述色谱条件和质谱条件连续进样6次, 测定并记录峰面积, 计算19个化合物峰面积的RSD值。
重复性   精密称取布渣叶样品(BZY01) 粉末(过三号筛) 0.5 g, 平行6份, 按上述“供试品溶液的制备”项下方法制备供试品溶液, 按上述色谱条件和质谱条件进样测定, 计算19个化合物含量及RSD值。
加样回收率   精密称取同一批次已知含量的布渣叶样品(BZY01) 粉末(过三号筛) 0.25 g, 平行6份, 分别加入与样品中各成分含量相近的混合对照品溶液, 按上述“供试品溶液的制备”项下方法制备供试品溶液, 按上述色谱条件和质谱条件进样测定, 计算加样回收率及RSD值。
稳定性   取同一份布渣叶样品(BZY01) 供试品溶液, 按上述色谱条件和质谱条件分别在0、2、4、8、12、18、24 h进样测定, 记录19个化合物峰面积并计算其RSD值。
样品含量测定   取布渣叶样品(BZY01~BZY28) 粉末(过三号筛) 0.5 g, 按上述“供试品溶液的制备”项下方法制备供试品溶液, 按上述色谱条件和质谱条件进样测定, 记录峰面积并计算样品的含量。
OPLS-DA分析   为明确引起不同产地间质量差异的特征性成分, 以各化合物含量测定结果为变量采用Simca 14.1软件进行正交偏最小二乘法-判别分析(OPLS-DA), 建立OPLS-DA模型, 并进一步生成OPLS-DA得分图。
结果
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1 方法学考察
1.1 专属性考察
混合对照品溶液(A、B)、布渣叶供试品溶液和空白溶液的总离子流图见图 1。供试品溶液中各成分间分离效果良好, 且保留时间与混合对照品基本一致, 各化合物之间无干扰, 表明该方法专属性良好。
1.2 仪器精密度
咖啡酸、原花青素B2、表儿茶素、维采宁-2、对羟基肉桂酸、阿魏酸、夏佛塔苷、异夏佛塔苷、牡荆苷、香蒲新苷、异牡荆苷、芦丁、异槲皮苷、异鼠李素-3-O-新橙皮苷、山柰酚-3-O-芸香糖苷、紫云英苷、水仙苷、异鼠李素-3-O-葡萄糖苷、椴树苷的峰面积RSD值分别为0.98%、0.27%、1.12%、1.36%、0.87%、0.65%、1.06%、1.60%、0.54%、0.47%、1.02%、1.69%、0.84%、0.36%、2.29%、0.55%、1.41%、2.08%、0.28%, 结果表明, 仪器精密度良好。
1.3 线性关系考察与定量限
以对照品质量浓度为横坐标(X, μg·mL-1), 峰面积为纵坐标(Y) 绘制标准曲线, 计算各成分的线性回归方程和相关系数, 19个成分在各自检测范围内相关系数均大于0.995, 结表明线性关系良好。回归方程、线性范围、检测限、定量限结果见表 3。
1.4 重复性
咖啡酸、原花青素B2、表儿茶素、维采宁-2、对羟基肉桂酸、阿魏酸、夏佛塔苷、异夏佛塔苷、牡荆苷、香蒲新苷、异牡荆苷、芦丁、异槲皮苷、异鼠李素-3-O-新橙皮苷、山柰酚-3-O-芸香糖苷、紫云英苷、水仙苷、异鼠李素-3-O-葡萄糖苷和椴树苷含量RSD分别为0.32%、0.67%、1.25%、2.16%、0.47%、1.86%、0.54%、2.09%、1.36%、2.11%、0.49%、0.58%、2.35%、1.42%、0.58%、1.60%、0.83%、0.97%、0.71%, 结果表明该方法重复性良好。
1.5 加样回收率
咖啡酸、原花青素B2、表儿茶素、维采宁-2、对羟基肉桂酸、阿魏酸、夏佛塔苷、异夏佛塔苷、牡荆苷、香蒲新苷、异牡荆苷、芦丁、异槲皮苷、异鼠李素-3-O-新橙皮苷、山柰酚-3-O-芸香糖苷、紫云英苷、水仙苷、异鼠李素-3-O-葡萄糖苷和椴树苷的平均回收率分别为98.25%、100.36%、101.25%、96.27%、98.10%、99.05%、100.87%、99.06%、98.11%、95.43%、97.62%、97.89%、98.53%、96.71%、103.08%、100.25%、98.09%、98.47%、99.52%, RSD值分别为2.32%、1.97%、3.05%、3.27%、2.66%、1.84%、2.73%、3.56%、4.02%、3.91%、2.07%、1.88%、4.16%、3.18%、4.05%、2.48%、3.36%、4.52%、1.56%。结果显示19个化合物加样回收率为95.43%~103.08%, RSD值≤5%, 表明该方法准确度良好。
1.6 稳定性
咖啡酸、原花青素B2、表儿茶素、维采宁-2、对羟基肉桂酸、阿魏酸、夏佛塔苷、异夏佛塔苷、牡荆苷、香蒲新苷、异牡荆苷、芦丁、异槲皮苷、异鼠李素-3-O-新橙皮苷、山柰酚-3-O-芸香糖苷、紫云英苷、水仙苷、异鼠李素-3-O-葡萄糖苷和椴树苷的峰面积RSD值分别为0.25%、0.36%、1.08%、0.76%、1.35%、2.07%、1.13%、0.68%、1.39%、1.08%、1.57%、2.34%、2.31%、0.87%、0.92%、0.89%、1.43%、1.68%、1.80%, 表明供试品溶液在24 h内稳定性良好。
2 样品含量测定
28批布渣叶中19个化合物的含量测定结果见表 4。结果显示, 19个化合物在布渣叶中存在一定差异, 其中原花青素B2、表儿茶素和水仙苷的平均含量较高, 咖啡酸的平均含量最低; 且各批次间19个化合物间含量差异明显。
3 统计学分析
OPLS-DA模型共筛选5个主成分, 其R2Y为0.866和Q2为0.680, 说明该模型稳定性和预测能力均较好。经过200次置换检验, R2与Y轴正半轴的截距为0.295 (< 0.4) 和Q2与Y轴负半轴的截距为-0.765 (< -0.05), 证明建立的模型稳定有效, 可进一步应用于布渣叶质量稳定性差异标志物的筛选(图 2)[20]。进一步生成OPLS-DA得分图(图 3), 28批布渣叶样品分为3类, 来着广东产地样品(BZY01~BZY19) 归为Ⅰ类, 广西产地样品(BZY20~BZY25) 归为Ⅱ类, 海南产地样品(BZY26~BZY28) 归为Ⅲ类, 3组样品聚类良好, 样品集中度较高, 通过OPLS-DA得分图可将来自不同产地样品进行分类。变量重要性投影值(VIP) 是OPLS-DA模型筛选潜在差异标志物最重要的分析, 成分指标VIP值越大, 表示其对于解释变量的贡献越大和差异相关性越高[21]。以VIP值> 1.0为变量差异性筛选标准, 共筛选得到10个质量差异标志物的化合物(图 4), 按VIP大小顺序依次为紫云英苷 > 原花青素B2 > 表儿茶素 > 异鼠李素-3-O-新橙皮苷 > 芦丁 > 异槲皮苷 > 夏佛塔苷 > 对羟基肉桂酸 > 水仙苷 > 山柰酚-3-O-芸香糖苷, 这些化合物除黄酮类化合物外, 还含有多酚类化合物, 表明多酚类化合物亦为布渣叶不同产地质量稳定性差异的主要影响因素; 因此, 对布渣叶药材研究除关注黄酮类成分外, 还需要关注多酚类成分对其质量的影响。
讨论
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在实验过程中对色谱条件和质谱条件进行了优化, 考察了不同流动相体系(乙腈-水、乙腈-0.1%甲酸溶液、乙腈-0.1%乙酸溶液、乙腈-0.05%乙酸溶液、乙腈-0.2%乙酸溶液、甲醇-0.1%乙酸溶液)、不同品牌色谱柱(Waters Cortecs T3、Waters BEH C18、Agilent ZORBAX SB C18), 不同柱温(25、30、35 ℃) 等对色谱峰峰形及其响应值的影响。结果显示, 以乙腈-0.1%乙酸溶液为流动相, 柱温为30 ℃, 选择Agilent ZORBAX SB C18 (150 mm × 2.1 mm, 1.8 μm) 色谱柱时, 所得色谱峰的峰型较好, 且响应值强度较高。同时, 对离子化模式进行确认, 在负离子模式下各化合物响应值较高。本研究还根据不同碰撞能量对19个化合物母离子进行撞击以确定最佳碰撞能量, 并选择响应强度最高的离子对作为定量离子对, 并通过电压优化确定了最终的碰撞能量。
本研究前期对布渣叶提取溶剂(乙醇、70%乙醇、50%乙醇、甲醇、70%甲醇、50%甲醇)、提取方式(超声处理、加热回流)、提取时间(15、30、60 min) 及提取溶剂用量(25、50、100 mL) 进行了单因素考察, 以各化合物响应值为评价指标, 最终确定提取最优条件为取0.5 g布渣叶粉末, 加50%甲醇25 mL, 加热回流30 min。
本研究采用UPLC-MS/MS法对不同产地的布渣叶中19个化合物含量进行比较, 并结合化学计量学分析方法探究不同产地布渣叶的质量差异。实验结果表明, 不同产地的布渣叶中各成分含量存在一定差异, 这种差异具有统计学上的显著性, 且通过OPLS-DA可将不同产地布渣叶进行区分。文献[14]研究表明, 黄酮类是布渣叶的主要物质成分和药理药效成分, 具有抗动脉粥样硬化、抗肿瘤、抗衰老、保护心血管等作用。中药化学成分复杂多样, 是通过多成分间相互作用、协同以发挥其临床药效, 单一类成分难以准确表达其功效。本研究VIP值结果显示, VIP值大于1.0共筛选得到10个标志性化合物, 该10种化合物为影响不同产地差异的主要因素, 在建立布渣叶及其制剂质量标准应充分考虑这些成分作为含量指标, 该10种化合物除包含黄酮类成分外, 还包含多酚类化合物(对羟基肉桂酸、原花青素B2), 其中原花青素B2在布渣叶样品中平均含量最高; 因此, 在布渣叶质量评价中, 应全面考虑各成分对其质量的影响, 为布渣叶质量标准的建立提供科学依据。
综上所述, 本研究收集了不同产地28批布渣叶, 构建了UPLC-MS/MS法测定样品中各活性成分的含量, 并以19个化合物含量为指标, 采用统计学分析比较不同产地间差异, 并找到影响产地质量差异的标志化合物, 可为后续深入完善其质量控制体系、临床安全用药等相关研究提供依据。
作者贡献: 何民友负责方法建立、实验数据处理、撰写文章及编辑部修改意见核修等; 王利伟和刘林负责实验材料收集; 张珀瑜、蓝金权和万欣亚负责实验研究; 李振雨和陈向东负责实验的设计、课题的指导和论文框架的构建; 孙冬梅负责实验的整体设计把关和文章审阅, 并最终定稿。
利益冲突: 无任何利益冲突。
基金
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  • 国家工信部2022年产业技术基础公共服务平台项目-中药全产业链质量技术服务平台(2022-230-221)
  • 2022年佛山市南海区重点领域科技攻关专项
文献
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2024年第59卷第5期
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doi: 10.16438/j.0513-4870.2023-1365
  • 接收时间：2023-12-05
  • 首发时间：2025-11-27
  • 出版时间：2024-05-12
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  • 收稿日期：2023-12-05
  • 修回日期：2024-01-30
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国家工信部2022年产业技术基础公共服务平台项目-中药全产业链质量技术服务平台(2022-230-221)
2022年佛山市南海区重点领域科技攻关专项
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    广东一方制药有限公司, 广东省中药配方颗粒企业重点实验室, 广东 佛山 528244

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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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