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Article(id=1210517373895970907, tenantId=1146029695717560320, journalId=1189982191388893191, issueId=1210517366081975259, articleNumber=null, orderNo=null, doi=10.16438/j.0513-4870.2022-0811, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1656691200000, receivedDateStr=2022-07-02, revisedDate=1662307200000, revisedDateStr=2022-09-05, acceptedDate=null, acceptedDateStr=null, onlineDate=1766539432261, onlineDateStr=2025-12-24, pubDate=1668182400000, pubDateStr=2022-11-12, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1766539432261, onlineIssueDateStr=2025-12-24, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1766539432261, creator=13701087609, updateTime=1766539432261, updator=13701087609, issue=Issue{id=1210517366081975259, tenantId=1146029695717560320, journalId=1189982191388893191, year='2022', volume='57', issue='11', pageStart='3259', pageEnd='3450', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1766539430399, creator=13701087609, updateTime=1766539608198, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210518111875363690, tenantId=1146029695717560320, journalId=1189982191388893191, issueId=1210517366081975259, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210518111875363691, tenantId=1146029695717560320, journalId=1189982191388893191, issueId=1210517366081975259, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=3405, endPage=3410, ext={EN=ArticleExt(id=1210517374470590582, articleId=1210517373895970907, tenantId=1146029695717560320, journalId=1189982191388893191, language=EN, title=Simultaneous determination of seven components in Qutan Zhike granules by QAMS, columnId=1190335348761793317, journalTitle=Acta Pharmaceutica Sinica, columnName=Original Articles, runingTitle=null, highlight=null, articleAbstract=

We have established a quantitative analysis of multi-components by single marker method (QAMS) for the simultaneous determination of apigenin-7-glucuronide, quercitrin, yuankanin, luteolin, apigenin, hydroxygenkwanin, and genkwanin in Qutan Zhike Granules. The chromatographic column used was an Agilent EC-C18(150 mm × 4.6 mm, 4 μm), the mobile phase was methanol-0.15% phosphoric acid solution (gradient elution), and the detection wavelength was 338 nm. Apigenin was chosen as the internal reference standard, the relative correction factors for the six components were determined by multi-point correction method and included apigenin-7-glucuronide, quercitrin, yuankanin, luteolin, hydroxygenkwanin and genkwanin. According to the two-point correction method combined with the relative retention time correction of the components to be tested, the peak location was determined. The contents of these seven compounds in 10 batches of Qutan Zhike Granules samples were determined with relative correction factors, and the relative error (RE) was used to compare the results to that of the external standard using the External Standard Method to verify the accuracy of QAMS. The relative correction factors for apigenin-7-glucuronide, quercitrin, yuankanin, luteolin, hydroxygenkwanin and genkwanin were 1.762 8, 2.310 4, 1.898 4, 1.282 8, 1.191 3 and 1.066 9, respectively. RSDs of the relative correction factors were all lower than 3%. The peaks for each constituent were accurately located by the two-point correction method combined with relative retention time correction, and the predicted retention time was close to the actual retention time. The relative error of the contents by QAMS and determined by ESM in 10 batches of Qutan Zhike Granules were between -5% and 5%. This content determination method can be used for the simultaneous determination of seven components in Qutan Zhike Granules.

, correspAuthors=Jian-ming LI, authorNote=null, correspAuthorsNote=null, copyrightStatement=Copyright ©2022 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=Jia-yi CHEN, Jian-ming LI, Li-hong GU, Hui-chan HOU, Jing-you LI), CN=ArticleExt(id=1210517374969712793, articleId=1210517373895970907, tenantId=1146029695717560320, journalId=1189982191388893191, language=CN, title=一测多评法同时测定祛痰止咳颗粒中7种成分的含量, columnId=1190335348896011050, journalTitle=药学学报, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=

建立同时测定祛痰止咳颗粒中芹菜素-7-葡萄糖醛酸、槲皮苷、芫根苷、木犀草素、芹菜素、羟基芫花素、芫花素7种成分含量的一测多评法。采用AgilentEC-C18(150mm×4.6mm, 4μm)色谱柱, 以甲醇-0.15%磷酸(梯度洗脱)为流动相, 检测波长为338nm, 以芹菜素为内参物, 分别建立6种成分的相对校正因子, 并采用两点校正法结合相对保留时间法对各成分进行色谱峰定位。分别按一测多评法和外标法检测7种成分的含量, 并进行比较。上述6种成分的相对校正因子分别为芹菜素-7-葡萄糖醛酸1.7628、槲皮苷2.3104、芫根苷1.8984、木犀草素1.2828、羟基芫花素1.1913、芫花素1.0669, 在不同色谱条件下其相对校正因子的RSD均小于3%。采用两点校正法结合相对保留时间法能准确定位各成分色谱峰, 预测保留时间与实际保留时间非常接近。10批样品一测多评计算结果与外标法测定结果之间的相对误差在-5%~5%。一测多评法操作简便, 经济实用, 结果准确, 可应用于祛痰止咳颗粒中7个成分的含量测定。

, correspAuthors=栗建明, authorNote=null, correspAuthorsNote=
*栗建明, Tel: 86-20-26283696, E-mail:
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Chin Pharm J (中国药学杂志), 2022, 57: 69-75., articleTitle=Simultaneous determination of four components in Zhachong shisanwei pills by QAMS, refAbstract=null)], funds=[Fund(id=1210517380984345146, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1210517373895970907, awardId=2021Z031, language=CN, fundingSource=国家药典委员会2021年国家药品标准提高(2021Z031), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1210517375229759660, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1210517373895970907, xref=null, ext=[AuthorCompanyExt(id=1210517375242342575, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1210517373895970907, companyId=1210517375229759660, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1. 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Guangzhou Huacheng Pharmaceutical Company Limited, Guangzhou 510555, China), AuthorCompanyExt(id=1210517375456252097, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1210517373895970907, companyId=1210517375426891962, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.广州花城药业有限公司, 广东 广州 510555)])], figs=[ArticleFig(id=1210517379633779160, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1210517373895970907, language=EN, label=null, caption=null, figureFileSmall=cxcwgsnkOy+N+2oMzaHgFw==, figureFileBig=adxZb5uZ0dMRADLQIvNx/Q==, tableContent=null), ArticleFig(id=1210517379730248159, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1210517373895970907, language=CN, label=Figure 1, caption= HPLC chromatograms of mixed references (A), Qutan Zhike granules (B), negative sample of Genkwa Flos (C), negative sample of Rhododendron Mariae Folium et Cacumen (D). 1: Apigenin-7-glucuronide (AGC); 2: Quercitrin (QT); 3: Yuankanin (YK); 4: Luteolin (LO); 5: Apigenin (AG); 6: Hydroxygenkwanin (HGK); 7: Genkwanin (GW) , figureFileSmall=cxcwgsnkOy+N+2oMzaHgFw==, figureFileBig=adxZb5uZ0dMRADLQIvNx/Q==, tableContent=null), ArticleFig(id=1210517380049015281, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1210517373895970907, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
AnalyteRegression equationR2Linear range/μg·mL-1
AGCY = 143.32 x + 1 2000.998 734.83-348.26
QTY = 113.3 x + 22.3540.999 92.71-27.10
YKY = 137.55 x + 38.7450.999 93.47-34.72
LOY = 205.66 x + 5.7930.999 90.65-6.48
AGY = 261.23 x + 69.7890.999 93.32-33.20
HGKY = 218.28 x + 57.6610.999 92.79-27.88
GWY = 244.33 x + 81.5700.999 93.78-37.84
), ArticleFig(id=1210517380191621627, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1210517373895970907, language=CN, label=Table 1, caption=

Linear relationships of seven components

, figureFileSmall=null, figureFileBig=null, tableContent=
AnalyteRegression equationR2Linear range/μg·mL-1
AGCY = 143.32 x + 1 2000.998 734.83-348.26
QTY = 113.3 x + 22.3540.999 92.71-27.10
YKY = 137.55 x + 38.7450.999 93.47-34.72
LOY = 205.66 x + 5.7930.999 90.65-6.48
AGY = 261.23 x + 69.7890.999 93.32-33.20
HGKY = 218.28 x + 57.6610.999 92.79-27.88
GWY = 244.33 x + 81.5700.999 93.78-37.84
), ArticleFig(id=1210517380300673536, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1210517373895970907, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
InstrumentColumntR
tAGC/AGtQT/AGtYK/AGtLO/AGtHGK/AGtGW/AG
Agilent 1260ⅡC10.5630.5900.6810.8511.1561.219
C20.5850.6140.6640.8561.1061.162
C30.6540.6810.7220.9191.0731.117
Waters e2695C30.6350.6620.6990.8971.0821.128
Shimadzu LC-20AC30.6520.6770.7160.9011.0781.121
Average0.6180.6450.6960.8851.0991.149
RSD/%5.9935.6323.1023.0132.7913.328
), ArticleFig(id=1210517380468445708, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1210517373895970907, language=CN, label=Table 2, caption=

Relative retention time of 6 components. C1: BDS Hypersil C18; C2: Phenomenex Kinetex C18; C3: Agilent EC-C18

, figureFileSmall=null, figureFileBig=null, tableContent=
InstrumentColumntR
tAGC/AGtQT/AGtYK/AGtLO/AGtHGK/AGtGW/AG
Agilent 1260ⅡC10.5630.5900.6810.8511.1561.219
C20.5850.6140.6640.8561.1061.162
C30.6540.6810.7220.9191.0731.117
Waters e2695C30.6350.6620.6990.8971.0821.128
Shimadzu LC-20AC30.6520.6770.7160.9011.0781.121
Average0.6180.6450.6960.8851.0991.149
RSD/%5.9935.6323.1023.0132.7913.328
), ArticleFig(id=1210517380535554583, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1210517373895970907, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
InstrumentColumnCorrection equationRetention time /min
AGCQTYKLOAGHGKGW
Agilent 1260ⅡC3Actual M26.98528.12429.79437.95941.28444.30746.098
C1Y = 1.120 4 x - 10.301Actual M20.22621.21024.46830.58735.95541.58043.812
Forecast19.93321.20923.08032.22835.95339.34041.347
RE%1.4460.0035.671-5.3660.0045.3875.624
C2Y = 1.104 6 x - 7.927 8Actual M22.05823.13925.00732.26037.67641.65343.791
Forecast21.88023.13824.98334.00237.67441.01442.992
RE%0.8060.0050.095-5.3980.0041.5351.823
Waters e2695C3Y = 1.030 5 x - 2.479 1Actual M25.42326.50427.98835.94540.06643.33545.189
Forecast25.32926.50328.22436.63840.06443.17945.025
RE%0.3710.006-0.843-1.9260.0050.3590.363
Shimadzu LC-20ATC3Y = 1.040 6 x - 0.532 2Actual M27.66828.73330.38638.23542.42745.72847.551
Forecast27.54928.73430.47238.96842.42845.57347.438
RE%0.4310.003-0.283-1.9180.0030.3390.239
), ArticleFig(id=1210517380661383712, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1210517373895970907, language=CN, label=Table 3, caption=

Peak time to locate chromatographic peaks predicted by correction equation. M: Measured value

, figureFileSmall=null, figureFileBig=null, tableContent=
InstrumentColumnCorrection equationRetention time /min
AGCQTYKLOAGHGKGW
Agilent 1260ⅡC3Actual M26.98528.12429.79437.95941.28444.30746.098
C1Y = 1.120 4 x - 10.301Actual M20.22621.21024.46830.58735.95541.58043.812
Forecast19.93321.20923.08032.22835.95339.34041.347
RE%1.4460.0035.671-5.3660.0045.3875.624
C2Y = 1.104 6 x - 7.927 8Actual M22.05823.13925.00732.26037.67641.65343.791
Forecast21.88023.13824.98334.00237.67441.01442.992
RE%0.8060.0050.095-5.3980.0041.5351.823
Waters e2695C3Y = 1.030 5 x - 2.479 1Actual M25.42326.50427.98835.94540.06643.33545.189
Forecast25.32926.50328.22436.63840.06443.17945.025
RE%0.3710.006-0.843-1.9260.0050.3590.363
Shimadzu LC-20ATC3Y = 1.040 6 x - 0.532 2Actual M27.66828.73330.38638.23542.42745.72847.551
Forecast27.54928.73430.47238.96842.42845.57347.438
RE%0.4310.003-0.283-1.9180.0030.3390.239
), ArticleFig(id=1210517380745269799, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1210517373895970907, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
ComponentMethodS1S2S3S4S5S6S7S8S9S10
AGESM18.11818.39421.15218.06124.22923.71416.19024.66827.40628.911
LOESM3.6823.8134.1203.5185.1294.0492.6625.0375.3235.442
QAMS3.5753.7044.0063.4164.9593.9112.5534.9155.1545.271
RE%-2.898-2.868-2.775-2.895-3.318-3.417-4.070-2.413-3.165-3.140
QTESM13.50414.24815.10220.11518.5998.7359.98725.27410.5689.851
QAMS13.20813.93814.78519.66818.1348.5299.69624.86210.3319.635
RE%-2.193-2.177-2.097-2.222-2.504-2.360-2.923-1.628-2.244-2.190
HGKESM12.56212.46413.99611.72225.67514.3298.89518.35921.10021.812
QAMS12.27012.17713.68211.45424.98513.9738.65718.05720.57621.275
RE%-2.319-2.299-2.244-2.293-2.686-2.481-2.672-1.647-2.484-2.460
YKESM17.22818.0229.87013.96318.02910.2688.09521.13719.87318.664
QAMS16.51017.2599.57813.42717.45810.1688.08120.57219.21118.090
RE%-4.169-4.236-2.956-3.837-3.166-0.979-0.172-2.669-3.334-3.075
AGCESM158.394158.006132.911126.222104.552129.57992.355142.559194.241192.658
QAMS156.339155.945131.850125.220107.226131.36495.019145.189193.728192.415
RE%-1.297-1.305-0.798-0.7942.5581.3782.8841.845-0.264-0.126
GWESM16.74515.78619.73713.95427.12025.43416.15220.97829.94431.598
QAMS16.28215.35619.20013.58126.30024.66415.63020.56729.06430.674
RE%-2.763-2.722-2.720-2.680-3.027-3.025-3.232-1.961-2.939-2.925
), ArticleFig(id=1210517380862710319, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1210517373895970907, language=CN, label=Table 4, caption=

Content (μg·g-1) of seven components determined by quantitative analysis of multi-components by single marker method (QAMS) and external standard method (ESM). RE% = (QAMS - ESM)/ESM × 100%

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ComponentMethodS1S2S3S4S5S6S7S8S9S10
AGESM18.11818.39421.15218.06124.22923.71416.19024.66827.40628.911
LOESM3.6823.8134.1203.5185.1294.0492.6625.0375.3235.442
QAMS3.5753.7044.0063.4164.9593.9112.5534.9155.1545.271
RE%-2.898-2.868-2.775-2.895-3.318-3.417-4.070-2.413-3.165-3.140
QTESM13.50414.24815.10220.11518.5998.7359.98725.27410.5689.851
QAMS13.20813.93814.78519.66818.1348.5299.69624.86210.3319.635
RE%-2.193-2.177-2.097-2.222-2.504-2.360-2.923-1.628-2.244-2.190
HGKESM12.56212.46413.99611.72225.67514.3298.89518.35921.10021.812
QAMS12.27012.17713.68211.45424.98513.9738.65718.05720.57621.275
RE%-2.319-2.299-2.244-2.293-2.686-2.481-2.672-1.647-2.484-2.460
YKESM17.22818.0229.87013.96318.02910.2688.09521.13719.87318.664
QAMS16.51017.2599.57813.42717.45810.1688.08120.57219.21118.090
RE%-4.169-4.236-2.956-3.837-3.166-0.979-0.172-2.669-3.334-3.075
AGCESM158.394158.006132.911126.222104.552129.57992.355142.559194.241192.658
QAMS156.339155.945131.850125.220107.226131.36495.019145.189193.728192.415
RE%-1.297-1.305-0.798-0.7942.5581.3782.8841.845-0.264-0.126
GWESM16.74515.78619.73713.95427.12025.43416.15220.97829.94431.598
QAMS16.28215.35619.20013.58126.30024.66415.63020.56729.06430.674
RE%-2.763-2.722-2.720-2.680-3.027-3.025-3.232-1.961-2.939-2.925
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一测多评法同时测定祛痰止咳颗粒中7种成分的含量
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陈家仪 1 , 栗建明 1, * , 顾利红 1 , 侯惠婵 1 , 李镜友 2
药学学报 | 研究论文 2022,57(11): 3405-3410
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药学学报 | 研究论文 2022, 57(11): 3405-3410
一测多评法同时测定祛痰止咳颗粒中7种成分的含量
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陈家仪1, 栗建明1, * , 顾利红1, 侯惠婵1, 李镜友2
作者信息
  • 1.广州市药品检验所, 国家药品监督管理局中成药质量评价重点实验室, 广东 广州 510160
  • 2.广州花城药业有限公司, 广东 广州 510555

通讯作者:

*栗建明, Tel: 86-20-26283696, E-mail:
Simultaneous determination of seven components in Qutan Zhike granules by QAMS
Jia-yi CHEN1, Jian-ming LI1, * , Li-hong GU1, Hui-chan HOU1, Jing-you LI2
Affiliations
  • 1. NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Medicine, Guangzhou Institute for Drug Control, Guangzhou 510160, China
  • 2. Guangzhou Huacheng Pharmaceutical Company Limited, Guangzhou 510555, China
出版时间: 2022-11-12 doi: 10.16438/j.0513-4870.2022-0811
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摘要
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建立同时测定祛痰止咳颗粒中芹菜素-7-葡萄糖醛酸、槲皮苷、芫根苷、木犀草素、芹菜素、羟基芫花素、芫花素7种成分含量的一测多评法。采用AgilentEC-C18(150mm×4.6mm, 4μm)色谱柱, 以甲醇-0.15%磷酸(梯度洗脱)为流动相, 检测波长为338nm, 以芹菜素为内参物, 分别建立6种成分的相对校正因子, 并采用两点校正法结合相对保留时间法对各成分进行色谱峰定位。分别按一测多评法和外标法检测7种成分的含量, 并进行比较。上述6种成分的相对校正因子分别为芹菜素-7-葡萄糖醛酸1.7628、槲皮苷2.3104、芫根苷1.8984、木犀草素1.2828、羟基芫花素1.1913、芫花素1.0669, 在不同色谱条件下其相对校正因子的RSD均小于3%。采用两点校正法结合相对保留时间法能准确定位各成分色谱峰, 预测保留时间与实际保留时间非常接近。10批样品一测多评计算结果与外标法测定结果之间的相对误差在-5%~5%。一测多评法操作简便, 经济实用, 结果准确, 可应用于祛痰止咳颗粒中7个成分的含量测定。

祛痰止咳颗粒  /  相对校正因子  /  一测多评  /  外标法  /  两点校正法

We have established a quantitative analysis of multi-components by single marker method (QAMS) for the simultaneous determination of apigenin-7-glucuronide, quercitrin, yuankanin, luteolin, apigenin, hydroxygenkwanin, and genkwanin in Qutan Zhike Granules. The chromatographic column used was an Agilent EC-C18(150 mm × 4.6 mm, 4 μm), the mobile phase was methanol-0.15% phosphoric acid solution (gradient elution), and the detection wavelength was 338 nm. Apigenin was chosen as the internal reference standard, the relative correction factors for the six components were determined by multi-point correction method and included apigenin-7-glucuronide, quercitrin, yuankanin, luteolin, hydroxygenkwanin and genkwanin. According to the two-point correction method combined with the relative retention time correction of the components to be tested, the peak location was determined. The contents of these seven compounds in 10 batches of Qutan Zhike Granules samples were determined with relative correction factors, and the relative error (RE) was used to compare the results to that of the external standard using the External Standard Method to verify the accuracy of QAMS. The relative correction factors for apigenin-7-glucuronide, quercitrin, yuankanin, luteolin, hydroxygenkwanin and genkwanin were 1.762 8, 2.310 4, 1.898 4, 1.282 8, 1.191 3 and 1.066 9, respectively. RSDs of the relative correction factors were all lower than 3%. The peaks for each constituent were accurately located by the two-point correction method combined with relative retention time correction, and the predicted retention time was close to the actual retention time. The relative error of the contents by QAMS and determined by ESM in 10 batches of Qutan Zhike Granules were between -5% and 5%. This content determination method can be used for the simultaneous determination of seven components in Qutan Zhike Granules.

Qutan Zhike granule  /  relative correction factor  /  quantitative analysis of multi-components with single marker  /  external standard method  /  two-point correction method
陈家仪, 栗建明, 顾利红, 侯惠婵, 李镜友. 一测多评法同时测定祛痰止咳颗粒中7种成分的含量. 药学学报, 2022 , 57 (11) : 3405 -3410 . DOI: 10.16438/j.0513-4870.2022-0811
Jia-yi CHEN, Jian-ming LI, Li-hong GU, Hui-chan HOU, Jing-you LI. Simultaneous determination of seven components in Qutan Zhike granules by QAMS[J]. Acta Pharmaceutica Sinica, 2022 , 57 (11) : 3405 -3410 . DOI: 10.16438/j.0513-4870.2022-0811
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祛痰止咳颗粒是以《金匮要略》的参夏汤与十枣汤化裁而成的验方[1], 主要由紫花杜鹃、醋芫花、醋甘遂、党参、姜水半夏、明矾六味药组成。现行质量标准收载于《中华人民共和国卫生部药品标准》中药成方制剂第十册, 只有芫花、甘遂和紫花杜鹃薄层色谱鉴别项目及颗粒剂通则检查, 无含量测定项[2]。因此, 建立多指标成分含量测定方法, 更有利于把控全方整体质量。
本方首选紫花杜鹃为治疗慢性支气管炎的良药, 醋芫花、醋甘遂为行痰利胸膈要药, 加入白矾可以协调经医古方炮制之芫花、甘遂燥湿化痰。久服本方恐有伤正气, 脾胃为生痰之源, 故又加入党参以扶正, 姜水半夏燥湿祛痰和胃降逆。结合功效主治, 紫花杜鹃为君药, 醋芫花、醋甘遂为臣药, 党参、明矾、姜水半夏为佐药。本方制备工艺为水煎醇沉, 由于方中甘遂主要活性成分为巨大戟二萜醇型化合物和三萜化合物[3-6], 极性较小, 在煎煮过程中成分较难溶出。姜水半夏和党参中指标性成分含量很低, 明矾为无机盐, 故醋甘遂、姜水半夏、党参、明矾均未纳入含量测定。有研究表明, 紫花杜鹃的黄酮类物质具有祛痰止咳、杀菌消炎、镇痛的效果, 紫花杜鹃中芸香苷、金丝桃苷、槲皮苷、槲皮素的含量测定曾有文献[7, 8]报道, 其中槲皮苷含量较高且稳定。现代药理研究表明, 芫花镇咳祛痰的药效成分为黄酮类成分, 芫花入药时必须经过醋制, 文献报道, 芫花在醋制过程中, 黄酮类大分子成分发生苷键断裂转化为小分子, 达到增效减毒的目的[9, 10]。芹菜素-7-葡萄糖醛酸、芫根苷、木犀草素、芹菜素、羟基芫花素和芫花素曾作为芫花含量测定指标性成分被报道[11, 12], 因此本实验同时监测上述6个成分, 能较全面体现芫花醋制过程中成分的动态变化。故本实验最终选择紫花杜鹃中槲皮苷、芫花中芹菜素-7-葡萄糖醛酸、芫根苷、木犀草素、芹菜素、羟基芫花素和芫花素作为指标性成分。
中国食品药品检定研究院暂未能提供芫根苷、羟基芫花素、芹菜素-7-葡萄糖醛酸对照品, 并且同时配制槲皮苷、芫花中芹菜素-7-葡萄糖醛酸、芫根苷、木犀草素、芹菜素、羟基芫花素和芫花素7个对照品溶液, 检验成本昂贵。一测多评法(quantitative analysis of multi-components by single-marker, QAMS) 的出现有效地解决了对照品购买困难、检验成本昂贵等难题, 而且QAMS目前也是中国药典的重点推广方法[13, 14]。本研究以芹菜素为内参物, 建立一测多评法同时测定祛痰止咳颗粒中槲皮苷、芹菜素-7-葡萄糖醛酸、芫根苷、木犀草素、羟基芫花素和芫花素的含量, 方法简便, 经济实用, 能有效地控制成品质量。
材料与方法
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仪器与试剂  Agilent1260Ⅱ型高效液相色谱仪(美国安捷伦公司); Waters2695型高效液相色谱仪(美国Waters公司); Shimadzu LC-20AT型高效液相色谱仪(日本岛津公司); Mettler AE240型电子天平(瑞士梅特勒公司); 超声波清洗器(型号: KQ-250DE型, 昆山市超声仪器有限公司); 色谱柱Thermo BDS Hypersil C18 (100 mm × 4.6 mm, 2.4 μm), 美国Thermo公司、Phenomenex Kinetex C18 (100 mm × 4.6 mm, 2.6 μm), 美国Phenomenex公司、Agilent EC-C18 (150 mm × 4.6 mm, 4 μm), 美国Agilent公司; 对照品槲皮苷(批号: 111538-202007, 纯度93.5%)、木犀草素(批号: 111520-201605, 纯度99.6%)、芹菜素(批号: 111901-202004, 纯度99.4%)、芫花素(批号: 111899-201202, 纯度94.9%), 均购自中国食品药品检定研究院; 芹菜素-7-葡萄糖醛酸(批号: lot#21-API-23-48, 纯度99.48%)、芫根苷(批号: lot#21-YUA-06-25, 纯度96.8%)、羟基芫花素(批号: lot#21-HYD-15-07, 纯度99.54%) 均购自美国Pharmaceutical Chemistry Laboratory公司; 甲醇为色谱纯(美国Fisher试剂公司); 超纯水由MILLI-Q超纯水制备仪制备(美国Millipore公司); 其他试剂均为分析纯。
实验材料  10批祛痰止咳颗粒(编号S1-S10)、紫花杜鹃阴性对照以及芫花阴性对照均由广州花城药业有限公司生产。
色谱条件  采用Agilent EC-C18 (150 mm × 4.6 mm, 4 μm) 色谱柱, 以甲醇(A)-0.15%磷酸水溶液(B) 为流动相, 梯度洗脱程序为0~5 min, 20%~30% A; 5~10 min, 30%~30% A; 10~35 min, 30%~50% A; 35~45 min, 50%~80% A; 45~50 min, 80%~20% A。流速为1.0 mL·min-1, 检测波长为338 nm, 柱温25 ℃, 进样量10 μL。
混合对照品溶液制备  精密称取芹菜素等7种对照品适量, 加甲醇溶液制成每1 mL分别含芹菜素-7-葡萄糖醛酸1 741.300 μg、槲皮苷135.500 μg、芫根苷173.600 μg、木犀草素32.400 μg、芹菜素166.000 μg、羟基芫花素139.400 μg、芫花素189.200 μg的溶液作为混合对照品溶液。
供试品溶液制备  取装量差异项下的本品, 混匀, 研细, 取约10 g, 精密称定, 置具塞锥形瓶中, 精密加入甲醇50 mL, 称定重量, 超声处理(功率300 W, 频率37 kHz) 30 min, 放冷, 再称定重量, 用甲醇补足减失的重量, 滤过, 取续滤液25 mL, 蒸干, 残渣加75%甲醇溶解, 转移至5 mL量瓶中, 加75%甲醇稀释至刻度, 摇匀, 滤过, 取续滤液, 即得。
阴性对照溶液的制备  按照祛痰止咳颗粒质量标准的处方和制法, 分别制备紫花杜鹃阴性对照和芫花阴性对照样品, 并按“供试品溶液制备”项下方法分别制备相应的阴性对照溶液。
专属性  取混合对照品溶液、供试品溶液, 紫花杜鹃阴性对照溶液和芫花阴性对照溶液分别进行测定, 比较色谱图。
线性关系  精密吸取混合对照品溶液0.2、0.4、0.6、0.8、1.0、1.5、2.0 mL, 分别置10 mL量瓶中, 加甲醇稀释至刻度, 分别进样10 μL。以芹菜素-7-葡萄糖醛酸、槲皮苷、芫根苷、木犀草素、芹菜素、羟基芫花素、芫花素进样浓度(x, μg·min-1) 与峰面积(Y) 作标准曲线, 计算回归方程。
精密度  精密吸取混合对照品溶液1.0 mL, 置10 mL量瓶中, 加甲醇稀释至刻度, 按色谱条件测定6次, 测定峰面积, 计算7种成分峰面积的RSD。
稳定性  取同一批供试品溶液, 于0、4、8、12、24 h按色谱条件进行测定。记录峰面积, 计算7种成分峰面积的RSD。
重复性  取同一批样品(编号S1), 按“供试品溶液制备”方法平行制备6份供试品溶液, 按色谱条件进样测定, 计算供试品中7种成分的平均含量及其RSD。
加样回收率  分别取芹菜素-7-葡萄糖醛酸、槲皮苷、芫根苷、木犀草素、芹菜素、羟基芫花素、芫花素对照品适量, 精密称定, 加甲醇制成每1 mL各含160.120、13.620、18.350、3.150、16.230、13.760和16.380 μg的混合对照品溶液, 作为加样回收用储备液。取同一批已知含量样品(编号S1) 6份, 每份约5 g, 精密称定, 置具塞锥形瓶中, 精密加入上述加样回收用储备液5 mL和甲醇45 mL, 按“供试品溶液制备”方法制备供试品溶液, 按色谱条件进样测定, 计算回收率。
相对校正因子的测定  相对校正因子(f) 计算公式为f = (As/Cs)/(Ai/Ci), 其中As和Cs为内参物峰面积和浓度; Ai和Ci为待测成分i的峰面积和浓度。将“线性关系”项下的系列对照品溶液各进样10 μL, 按色谱条件测定各成分的峰面积, 以芹菜素为内参物, 计算不同进样浓度下其他6种成分的相对校正因子的平均值, 比较RSD值。
不同仪器、色谱柱对相对校正因子的影响  分别考察不同仪器(Agilent1260 Ⅱ型、Waters2695型, Shimadzu LC-20AT高效液相色谱仪) 和3种色谱柱Thermo BDS Hypersil C18 (100 mm × 4.6 mm, 2.4 μm)、Phenomenex Kinetex C18 (100 mm × 4.6 mm, 2.6 μm)、Agilent EC-C18 (150 mm × 4.6 mm, 4 μm) 对相对校正因子的影响, 计算相对校正因子的平均值, 并比较RSD值。
色谱峰的定位  取线性关系项下的中浓度混合对照品溶液, 按色谱条件在不同型号仪器(Agilent1260 Ⅱ型、Waters2695型, Shimadzu LC-20AT高效液相色谱仪) 和色谱柱Thermo BDS Hypersil C18 (100 mm × 4.6 mm, 2.4 μm)、Phenomenex Kinetex C18 (100 mm × 4.6 mm, 2.6 μm)、Agilent EC-C18 (150 mm × 4.6 mm, 4 μm) 进样测定。采用相对保留时间法, 以芹菜素为内参物S, 计算其余6种化合物的相对保留时间及RSD值; 采用两点校正法, 以内参物芹菜素和另一种常见、价格便宜易获取的槲皮苷在Agilent1260 Ⅱ仪器上使用Agilent EC-C18色谱柱所得保留时间为横坐标(x), 其他仪器、色谱柱所得保留时间为纵坐标(Y) 进行回归, 绘制校正曲线, 再以Agilent EC-C18所得标准保留时间代入校正曲线, 即可计算各成分预测出峰时间, 并计算预测保留时间和实测保留时间的相对误差(relative error, RE)。
样品含量测定  取不同批次的祛痰止咳颗粒样品, 按供试品溶液制备方法制备供试品溶液, 按色谱条件进行测定, 分别采用一测多评法和外标法(external standard method, ESM) 计算祛痰止咳颗粒中芹菜素、木犀草素、槲皮苷、羟基芫花素、芫根苷、芫花素、芹菜素-7-葡萄糖醛酸的含量, 并用RE进行评价。
结果
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1 方法学考察
1.1 系统适应性
7个成分与相邻成分之间分离度均大于1.5, 芫花阴性对照在样品色谱相应位置上干扰峰峰面积低于5%, 紫花杜鹃阴性无干扰, 见图 1。
1.2 线性关系
各成分在各自范围内线性关系良好, 结果见表 1。
1.3 精密度
芹菜素-7-葡萄糖醛酸、槲皮苷、芫根苷、木犀草素、芹菜素、羟基芫花素、芫花素的RSD分别为0.912%、0.916%、1.110%、1.121%、1.109%、1.102%和1.112%, 均小于2%, 表明方法的精密度良好。
1.4 稳定性
芹菜素-7-葡萄糖醛酸、槲皮苷、芫根苷、木犀草素、芹菜素、羟基芫花素、芫花素的RSD分别为0.605%、0.812%、0.515%、0.625%、0.541%、0.625%和0.532%, 均小于3%, 表明供试品溶液在制备后24 h内稳定性良好。
1.5 重复性
芹菜素-7-葡萄糖醛酸、槲皮苷、芫根苷、木犀草素、芹菜素、羟基芫花素、芫花素7个成分的平均含量分别为155.102、13.151、17.114、3.588、17.751、12.098和16.168 μg·g-1, RSD分别为2.377%、2.005%、2.322%、1.479%、1.638%、1.853%和1.460%, 表明方法重复性良好。
1.6 加样回收率
芹菜素-7-葡萄糖醛酸、槲皮苷、芫根苷、木犀草素、芹菜素、羟基芫花素、芫花素的加样回收率分别为100.057%、94.091%、97.574%、95.260%、101.097%、100.811%和93.442%, RSD分别为2.478%、2.462%、1.538%、2.478%、2.564%、2.131%和2.768%, 表明该方法准确度高。
2 一测多评法
2.1 相对校正因子的测定
以芹菜素为内参物, 芹菜素-7-葡萄糖醛酸、槲皮苷、芫根苷、木犀草素、羟基芫花素、芫花素的相对校正因子分别为1.762 8、2.310 4、1.898 4、1.282 8、1.191 3和1.066 9, RSD值均小于2%。
2.2 不同仪器、色谱柱对相对校正因子影响
不同高效色谱仪和色谱柱条件下, 计算芹菜素-7-葡萄糖醛酸、槲皮苷、芫根苷、木犀草素、羟基芫花素、芫花素的相对校正因子平均值, 分别为1.762 3、2.305 1、1.877 1、1.285 6、1.182 1和1.048 9, RSD值均小于3%, 表明不同高效液相色谱仪和色谱柱对相对校正因子没有显著影响, 建立的相对校正因子重现性较好。
2.3 待测成分色谱峰的定位
利用相对保留时间法, 结果见表 2, 芫根苷、木犀草素、羟基芫花素、芫花素相对保留值在不同仪器和不同色谱柱上重现性良好, RSD < 5%。由于3个品牌色谱柱的内径和长度规格不一致, 并且槲皮苷和芹菜素-7-葡萄糖醛酸距离内参物芹菜素较远, 导致相对保留时间RSD稍微偏大。
由于槲皮苷和芹菜素-7-葡萄糖醛酸的相对保留时间RSD > 5%, 难以对二者进行准确定位, 本实验进一步采用两点校正法。结果见表 3, 芹菜素-7-葡萄糖醛酸和槲皮苷采用两点校正法的预测保留时间和实测保留时间的RE绝对值较低(< 2%), 且非常接近。因此, 芹菜素-7-葡萄糖醛酸和槲皮苷可采用两点校正法定位, 其余4个待测成分采用相对保留时间进行定位, 两者相结合可以更加准确定位色谱峰。
3 外标法和一测多评法含量测定比较
外标法和一测多评法测定结果见表 4, 结果显示, 10批样品中均能检出7种有效成分, 两种方法测得并以RE为参数, 对2种方法所得结果进行比较, RE值在-5%~5%, 提示建立的方法具有较好的可信度。
讨论
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本实验考察了不同提取方法(超声、回流提取)、不同提取溶剂(纯水、纯甲醇、50%甲醇、75%甲醇及乙醇)、不同料液比(1∶5、1∶10、1∶15) 以及提取时间(15、30、45、60 min) 下, 以7个成分(木犀草素、槲皮苷、羟基芫花素、芫根苷、芫花素、芹菜素-7-葡萄糖醛酸、芹菜素) 的提取效率为指标。最终确定料液比为1∶5、溶剂为纯甲醇、超声提取30 min。
检测波长的选择, 本实验所选的7个指标性成分, 化学结构母核相似, 采用二极管阵列检测器对7个成分进行光谱扫描, 7个成分最大吸收波长也相近。综合考虑, 选择338 nm为检测波长, 在此波长下, 色谱图基线平稳, 7个成分分离效果好, 且各成分响应值也较高。
本研究建立了祛痰止咳颗粒中有效成分及指标性成分的一测多评方法, 成品中芹菜素含量较高, 且峰型较好、保留时间适中, 故选择芹菜素作为内参物, 测定了木犀草素、槲皮苷、羟基芫花素、芫根苷、芫花素以及芹菜素-7-葡萄糖醛酸的相对校正因子。所测得的相对校正因子在不同色谱柱以及不同仪器上重现性良好, 并且分别用一测多评法和外标法测定10批祛痰止咳颗粒样品中7个成分的含量, 两者结果无显著差异, 这说明本实验所建立的相对校正因子可信度高。
色谱峰定位, 目前文献[15-17]报道一测多评法色谱峰定位方法主要有相对保留时间、保留时间差以及两点校正法。本实验前期摸索色谱条件时, 采用常规色谱(250 mm × 4.6 mm, 5 μm) 分离效果不理想, 采集时间长达100 min, 进一步采用Agilent EC-C18 (150 mm × 4.6 mm, 4 μm) 小粒径短柱, 分离效果好, 时间缩短一半。后续考察了不同规格小粒径短柱和不同色谱仪器对7个待测成分保留时间的影响, 结果采用相对保留时间定位色谱峰时, 芫根苷、木犀草素、羟基芫花素、芫花素4个成分的相对保留时间RSD均小于5%。采用两点校正法时, 芹菜素-7-葡萄糖醛酸、槲皮苷两个成分RE均小于2%。故一测多评的定位若结合相对保留时间法和两点校正法, 可以实现准确定位, 尤其适合待测成分数量较多, 且相邻近色谱峰较多的情况。
作者贡献: 陈家仪设计实验和数据采集处理以及撰写论文; 李镜友负责收集样品; 栗建明、顾利红和侯惠婵负责修改论文。
利益冲突: 无利益冲突。
基金
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  • 国家药典委员会2021年国家药品标准提高(2021Z031)
文献
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2022年第57卷第11期
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doi: 10.16438/j.0513-4870.2022-0811
  • 接收时间：2022-07-02
  • 首发时间：2025-12-24
  • 出版时间：2022-11-12
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  • 收稿日期：2022-07-02
  • 修回日期：2022-09-05
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国家药典委员会2021年国家药品标准提高(2021Z031)
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    1.广州市药品检验所, 国家药品监督管理局中成药质量评价重点实验室, 广东 广州 510160
    2.广州花城药业有限公司, 广东 广州 510555

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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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