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Article(id=1239250710890598576, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239250701583446236, articleNumber=null, orderNo=null, doi=10.16155/j.0254-1793.2024.04.03, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1689609600000, receivedDateStr=2023-07-18, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773389993641, onlineDateStr=2026-03-13, pubDate=1714406400000, pubDateStr=2024-04-30, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773389993641, onlineIssueDateStr=2026-03-13, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773389993641, creator=13701087609, updateTime=1773389993641, updator=13701087609, issue=Issue{id=1239250701583446236, tenantId=1146029695717560320, journalId=1205117023404326918, year='2024', volume='44', issue='4', pageStart='553', pageEnd='736', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773389991422, creator=13701087609, updateTime=1773390513217, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1239252890213209050, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239250701583446236, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1239252890213209051, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239250701583446236, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=567, endPage=576, ext={EN=ArticleExt(id=1239250711322611906, articleId=1239250710890598576, tenantId=1146029695717560320, journalId=1205117023404326918, language=EN, title=Simultaneous determination of 11 components in Hongwushen capsules by UPLC-MS/MS*, columnId=1206272756333736276, journalTitle=Chinese Journal of Pharmaceutical Analysis, columnName=Ingredient Analysis, runingTitle=null, highlight=null, articleAbstract=
Objective:

To establish an UPLC-MS/MS method for simultaneous determination of 11 components(caffeic acid, afzelin, gallic acid, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, salidroside, eleutheroside B, ginsenoside Re, ginsenoside Rg1, ginsenoside Rd) in Hongwushen capsules.

Methods:

A Shim-pack GIST C18 chromatographic column(100 mm×2.1 mm, 2 μm) was used. The mobile phase was composed of acetonitrile -0.1% acetic acid -1 mmol·L-1 ammonium acetate aqueous solution and the gradient elution was applied. The flow rate was 0.3 mL·min-1, the column temperature was 30 ℃, and the injection volume was 1 μL. Electrospray ionization (ESI) source and multiple reaction monitoring (MRM) mode in both positive and negative were used for ion detections.

Results:

The linear relationship of 11 components was good in the concentration range, and the linear correlation coefficients were all above 0.999 0. The RSD values of precision were less than 3%. The repeatability and stability were good, and the RSD values were less than 5%. The average recoveries were in the range of 97.1%-101.5% with RSDs≤3.7%. The contents of caffeic acid, afzelin, gallic acid, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, salidroside, eleutheroside B, ginsenoside Re, ginsenoside Rg1 and ginsenoside Rd in 10 batches of Hongwushen capsules were 0.010-0.013 mg·g-1, 0.000 7-0.001 4 mg·g-1, 0.035-0.038 mg·g-1, 0.312-0.315 mg·g-1, 0.413-0.417 mg·g-1, 0.411-0.416 mg·g-1, 4.355-4.358 mg·g-1, 0.030-0.032 mg·g-1, 0.993-0.999 mg·g-1, 1.120-1.124 mg·g-1 and 2.536-2.538 mg·g-1, respectively.

Conclusions:

The method is accurate, sensitive, stable and reproducible, and can be used for the quality control of Hongwushen capsules.

, correspAuthors=Xin-guo WANG, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, 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=Shuai SUN, Xiang WANG, Le GAO, Wen-chao XIE, Chen-nan LIU, Li-ying NIU, Xin-guo WANG), CN=ArticleExt(id=1239250712153084168, articleId=1239250710890598576, tenantId=1146029695717560320, journalId=1205117023404326918, language=CN, title=UPLC-MS/MS法同时测定红五参胶囊中11个成分的含量*, columnId=1206272756476342615, journalTitle=药物分析杂志, columnName=成分分析, runingTitle=null, highlight=null, articleAbstract=
目的：

建立UPLC-MS/MS同时测定红五参胶囊中11个成分(咖啡酸、阿福豆苷、没食子酸、新绿原酸、绿原酸、隐绿原酸、红景天苷、紫丁香苷、人参皂苷Re、人参皂苷Rg1、人参皂苷Rd)含量的方法。

方法：

采用Shim-pack GIST C18(100 mm×2.1 mm，2 μm)色谱柱，以乙腈-0.1%乙酸-1 mmol·L-1乙酸铵水溶液为流动相，梯度洗脱，流速0.3 mL·min-1，柱温30 ℃，进样量为1 μL；采用电喷雾电离源(ESI源)，多反应监测(MRM)模式进行正负离子检测。

结果：

11个成分在测定浓度范围内线性关系良好，线性相关系数r均>0.999 0；精密度RSD均<3%；重复性和稳定性良好，RSD值均<5%；平均加样回收率为97.1%~101.5%，RSD≤3.7%。10批红五参胶囊中咖啡酸、阿福豆苷、没食子酸、新绿原酸、绿原酸、隐绿原酸、红景天苷、紫丁香苷、人参皂苷Re、人参皂苷Rg1、人参皂苷Rd含量分别为0.010~0.013、0.000 7~0.001 4、0.035~0.038、0.312~0.315、0.413~0.417、0.411~0.416、4.355~4.358、0.030~0.032、0.993~0.999、1.120~1.124、2.536~2.538 mg·g-1。

结论：

本方法准确灵敏，稳定性和重复性良好，可用于红五参胶囊的质量控制。

, correspAuthors=王鑫国, authorNote=null, correspAuthorsNote=
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J Univ Vet Med，2019，55(8)：81, articleTitle=Study on anti-fatigue effect of protopanaxadiol-type Ginseng and protopanaxatriol-type Ginseng stem and leave saponin, refAbstract=null)], funds=[Fund(id=1239250722932445938, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, awardId=23372502D, language=CN, fundingSource=*河北省省级科技计划项目(23372502D), fundOrder=null, country=null), Fund(id=1239250723016332024, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, awardId=H2022423341, language=CN, fundingSource=河北省自然科学基金项目(H2022423341), fundOrder=null, country=null), Fund(id=1239250723121189631, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, awardId=H2022423335, language=CN, fundingSource=河北省自然科学基金项目(H2022423335), fundOrder=null, country=null), Fund(id=1239250723209270020, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, awardId=202214432020, language=CN, fundingSource=国家级大学生创新创业训练计划项目(202214432020), fundOrder=null, country=null), Fund(id=1239250723272184586, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, awardId=2022107, language=CN, fundingSource=河北中医药管理局项目(2022107), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1239250712366993696, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, xref=1., ext=[AuthorCompanyExt(id=1239250712375382306, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, companyId=1239250712366993696, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.Hebei University of Chinese Medicine, Hebei Traditional Chinese Medicine Formula Granule Engineering & Technology Innovate Center, Quality Evaluation & Standardization Hebei Province Engineering Research Center of Traditional Chinese Medicine, Shijiazhuang 050091, China), AuthorCompanyExt(id=1239250712383770916, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, companyId=1239250712366993696, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.河北中医药大学 河北省中药配方颗粒技术创新中心 中药材品质评价与标准化河北省工程研究中心，石家庄050091)]), AuthorCompany(id=1239250712501211441, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, xref=2., ext=[AuthorCompanyExt(id=1239250712505405747, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, companyId=1239250712501211441, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.NCPC Hebei Huawei Health Industry Co., Ltd., Shijiazhuang 052165, China), AuthorCompanyExt(id=1239250712513794356, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, companyId=1239250712501211441, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.华北制药河北华维健康产业有限公司，石家庄 052165)])], figs=[ArticleFig(id=1239250719920935578, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, language=EN, label=Fig.1, caption=Ion chromatograms in positive ion mode(A) and ion chromatograms in negative ion mode (B), figureFileSmall=4b1QobP6hhlg+K/mstJtTA==, figureFileBig=dJvckzmDgTLo49IVVl1Obg==, tableContent=null), ArticleFig(id=1239250720013210274, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, language=CN, label=图1, caption=正离子模式下离子流图(A)和负离子模式下离子流图(B)

1.咖啡酸(caffeic acid)　2.阿福豆苷(afzelin)　3.没食子酸(gallic acid)　4.新绿原酸(neochlorogenic acid))　5.绿原酸(chlorogenic acid)　6.隐绿原酸(xryptochlorogenic acid)　7.红景天苷(salidroside)　8.紫丁香苷(eleutheroside B)　9.人参皂苷Re(ginsenoside Re)　10.人参皂苷Rg1(ginsenoside Rg1)　11.人参皂苷Rd(ginsenoside Rd)

, figureFileSmall=4b1QobP6hhlg+K/mstJtTA==, figureFileBig=dJvckzmDgTLo49IVVl1Obg==, tableContent=null), ArticleFig(id=1239250720218731179, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, language=EN, label=Fig.2, caption=MRM chromatograms of mixed reference substances(A) and Hongwushen capsules(B), figureFileSmall=ZOmfGX2nie1jf9ewDkot4g==, figureFileBig=fpjP0f9K7e2ARO0aAMCWEg==, tableContent=null), ArticleFig(id=1239250720285840052, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, language=CN, label=图2, caption=混合对照品(A)和红五参胶囊供试品(B)的MRM色谱图

1.咖啡酸(caffeic acid)　2.阿福豆苷(afzelin)　3.没食子酸(gallic acid)　4.新绿原酸(neochlorogenic acid))　5.绿原酸(chlorogenic acid)　6.隐绿原酸(xryptochlorogenic acid)　7.红景天苷(salidroside)　8.紫丁香苷(eleutheroside B)　9.人参皂苷Re(ginsenoside Re)　10.人参皂苷Rg1(ginsenoside Rg1)　11.人参皂苷Rd(ginsenoside Rd)

, figureFileSmall=ZOmfGX2nie1jf9ewDkot4g==, figureFileBig=fpjP0f9K7e2ARO0aAMCWEg==, tableContent=null), ArticleFig(id=1239250720369726134, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, language=EN, label=Fig.3, caption=The contents of 11 components in the test solutions under different extraction methods, figureFileSmall=rtF4J7tzKEumMFLLQ/OhOQ==, figureFileBig=FSDRrgHw9skw30isIWQxxw==, tableContent=null), ArticleFig(id=1239250720457806525, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, language=CN, label=图3, caption=不同浓缩方式下供试品溶液中11个待测成分的含量

g1.常压浓缩-100 ℃(normal pressure condense -100 ℃)　g2.减压浓缩-40 ℃(decompression concentration -40 ℃)　g3.减压浓缩-50 ℃(decompression concentration -50 ℃)　g4.减压浓缩-60 ℃(decompression concentration -60 ℃) h1.咖啡酸(caffeic acid)　h2.阿福豆苷(afzelin)　h3.没食子酸(gallic acid)　h4.新绿原酸(neochlorogenic acid))　h5.绿原酸(chlorogenic acid)　h6.隐绿原酸(cryptochlorogenic acid)　h7.红景天苷(salidroside)　h8.紫丁香苷(eleutheroside B)　h9.人参皂苷Re(ginsenoside Re)　h10.人参皂苷Rg1(ginsenoside Rg1)　h11.人参皂苷Rd(ginsenoside Rd)

, figureFileSmall=rtF4J7tzKEumMFLLQ/OhOQ==, figureFileBig=FSDRrgHw9skw30isIWQxxw==, tableContent=null), ArticleFig(id=1239250720566858433, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, language=EN, label=Tab.1, caption=

Mass spectrometric parameters of 11 components in Hongwushen capsules

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)		相对分子质量
(relative molecular mass)		母离子
(parent ion) m/z		子离子
(daughter ion) m/z		解簇电压
(declustering potential)/V		碰撞能量
(collision energy)/eV
咖啡酸(caffeic acid)180.16179.0134.9-53.15-20.99
没食子酸(gallic acid)170.12168.8124.8-74.08-17.11
新绿原酸(neochlorogenic acid)354.31353.2190.9-41.02-30.44
绿原酸(chlorogenic acid)354.31353.2190.9-40.00-27.00
隐绿原酸(cryptochlorogenic acid)354.31353.3190.9-73.88-27.33
红景天苷(salidroside)300.30299.0119.0-92.41-19.26
人参皂苷Rg1(ginsenoside Rg1)801.01823.3643.5172.0966.30
人参皂苷Re(ginsenoside Re)947.17969.4789.6152.3357.87
人参皂苷Rd(ginsenoside Rd)947.15969.5789.7157.3667.21
紫丁香苷(eleutheroside B)372.37374.4312.393.1836.41
阿福豆苷(afzelin)432.38431.1285.099.2625.99
), ArticleFig(id=1239250720654938824, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, language=CN, label=表1, caption=

五参胶囊中11个成分的质谱参数

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)		相对分子质量
(relative molecular mass)		母离子
(parent ion) m/z		子离子
(daughter ion) m/z		解簇电压
(declustering potential)/V		碰撞能量
(collision energy)/eV
咖啡酸(caffeic acid)180.16179.0134.9-53.15-20.99
没食子酸(gallic acid)170.12168.8124.8-74.08-17.11
新绿原酸(neochlorogenic acid)354.31353.2190.9-41.02-30.44
绿原酸(chlorogenic acid)354.31353.2190.9-40.00-27.00
隐绿原酸(cryptochlorogenic acid)354.31353.3190.9-73.88-27.33
红景天苷(salidroside)300.30299.0119.0-92.41-19.26
人参皂苷Rg1(ginsenoside Rg1)801.01823.3643.5172.0966.30
人参皂苷Re(ginsenoside Re)947.17969.4789.6152.3357.87
人参皂苷Rd(ginsenoside Rd)947.15969.5789.7157.3667.21
紫丁香苷(eleutheroside B)372.37374.4312.393.1836.41
阿福豆苷(afzelin)432.38431.1285.099.2625.99
), ArticleFig(id=1239250720768185034, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, language=EN, label=Tab.2, caption=

Results of regression equation，LOD and LOQ

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)		回归方程
(regression equation)		r线性范围
(linear range)/(ng·μL-1)		LOD/(ng·μL-1)LOQ/(ng·μL-1)
咖啡酸(caffeic acid)Y=2.51×109X+9.01×1050.999 50.529~10.5870.110.33
阿福豆苷(afzelin)Y=5.29×108X+3.58×1040.999 00.028~0.5640.010.02
没食子酸(gallic acid)Y=6.07×108X+4.09×1060.999 12.890~57.7920.400.80
新绿原酸(neochlorogenic acid)Y=4.36×108X+1.68×1060.999 16.212~124.2363.794.38
绿原酸(chlorogenic acid)Y=5.86×105X+4.45×1060.999 48.283~165.6681.295.16
隐绿原酸(cryptochlorogenic acid)Y=1.19×108X+6.50×1050.999 17.377~147.5333.426.84
红景天苷(salidroside)Y=2.70×107X+1.38×1060.999 255.751~1 115.0244.3617.44
紫丁香苷(eleutheroside B)Y=1.38×107X+2.54×1050.999 84.754~95.0901.063.18
人参皂苷Re(ginsenoside Re)Y=2.39×106X+7.07×1040.999 59.104~182.0740.842.52
人参皂苷Rg1(ginsenoside Rg1)Y=8.05×105X+2.76×1040.999 45.827~116.5380.460.92
人参皂苷Rd(ginsenoside Rd)Y=3.21×106X+3.88×1050.999 131.786~635.71215.3523.03
), ArticleFig(id=1239250720889819859, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, language=CN, label=表2, caption=

回归方程、LOD和LOQ

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)		回归方程
(regression equation)		r线性范围
(linear range)/(ng·μL-1)		LOD/(ng·μL-1)LOQ/(ng·μL-1)
咖啡酸(caffeic acid)Y=2.51×109X+9.01×1050.999 50.529~10.5870.110.33
阿福豆苷(afzelin)Y=5.29×108X+3.58×1040.999 00.028~0.5640.010.02
没食子酸(gallic acid)Y=6.07×108X+4.09×1060.999 12.890~57.7920.400.80
新绿原酸(neochlorogenic acid)Y=4.36×108X+1.68×1060.999 16.212~124.2363.794.38
绿原酸(chlorogenic acid)Y=5.86×105X+4.45×1060.999 48.283~165.6681.295.16
隐绿原酸(cryptochlorogenic acid)Y=1.19×108X+6.50×1050.999 17.377~147.5333.426.84
红景天苷(salidroside)Y=2.70×107X+1.38×1060.999 255.751~1 115.0244.3617.44
紫丁香苷(eleutheroside B)Y=1.38×107X+2.54×1050.999 84.754~95.0901.063.18
人参皂苷Re(ginsenoside Re)Y=2.39×106X+7.07×1040.999 59.104~182.0740.842.52
人参皂苷Rg1(ginsenoside Rg1)Y=8.05×105X+2.76×1040.999 45.827~116.5380.460.92
人参皂苷Rd(ginsenoside Rd)Y=3.21×106X+3.88×1050.999 131.786~635.71215.3523.03
), ArticleFig(id=1239250721024037590, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, language=EN, label=Tab.3, caption=

Experimental results of sample recovery rate

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)		原有量
(original)/μg		加入量
(added)/μg		测得量
(detected)/μg		回收率
(recovery)/%		平均回收率
(mean)/%		RSD/%
咖啡酸(caffeic acid)8.628 58.469 817.209 6101.399.32.7
8.638 816.838 796.8
8.633 116.798 996.4
8.626 217.369 0103.2
8.631 916.968 298.4
8.635 417.085 299.8
阿福豆苷(afzelin)0.750 30.740 91.484 898.298.73.7
0.751 21.450 593.5
0.750 71.515 5102.3
0.750 11.496 699.8
0.750 61.517 9102.6
0.750 91.465 995.6
没食子酸(gallic acid)27.010 826.006 453.376 9101.4101.51.6
27.043 254.128 4104.2
27.025 253.325 5101.1
27.003 653.057 8100.2
27.021 652.975 599.8
27.032 453.685 7102.5
新绿原酸(neochlorogenic acid)234.468 8232.942 5473.782 6102.798.02.7
234.750 0456.287 195.1
234.593 8464.136 898.5
234.406 3462.506 597.9
234.562 5459.110 196.4
234.656 3461.283 897.3
绿原酸(chlorogenic acid)313.102 2310.627 5609.060 595.397.83.7
313.475 8611.515 496.0
313.267 1619.840 998.7
313.016 7611.195 296.0
313.225 4619.733 3104.8
313.350 6612.476 196.3
隐绿原酸(cryptochlorogenic acid)309.573 8306.130 6611.327 998.697.11.0
309.945 1609.234 297.8
309.738 8605.570 496.6
309.491 3605.570 496.7
309.697 6607.664 097.3
309.821 3602.953 395.8
红景天苷(salidroside)3 268.757 03 233.569 66 557.991 9101.799.71.9
3 272.677 96 395.679 096.6
3 270.499 66 525.529 3100.7
3 267.885 76 495.385 599.8
3 270.064 06 530.166 8100.8
3 271.370 96 458.285 498.6
紫丁香苷(eleutheroside B)23.109 223.772 446.118 196.899.13.2
23.137 046.572 398.7
23.121 648.071 2105.0
23.103 146.027 396.4
23.118 546.935 7100.2
23.127 746.390 697.9
人参皂苷Re(ginsenoside Re)747.148 7741.949 91 463.778 696.699.22.6
748.045 01 490.154 5100.0
747.547 11 456.205 395.5
746.949 61 501.122 7101.7
767.447 51 502.950 8101.8
747.746 21 485.976 199.5
人参皂苷Rg1(ginsenoside Rg1)842.136 7844.897 61 652.171 595.9101.33.1
843.146 91 690.982 6100.4
842.585 71 722.031 5104.1
841.912 21 690.982 6100.5
842.473 41 722.031 5104.1
842.810 21 714.269 3103.1
人参皂苷Rd(ginsenoside Rd)1 902.760 81 907.136 03 786.672 398.899.91.0
1 905.043 23 794.450 799.1
1 903.775 23 821.675 3100.6
1 902.253 63 825.564 5100.9
1 903.521 63 825.564 5100.8
1 904.282 43 794.450 799.1
), ArticleFig(id=1239250721179226845, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, language=CN, label=表3, caption=

加样回收率试验结果

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)		原有量
(original)/μg		加入量
(added)/μg		测得量
(detected)/μg		回收率
(recovery)/%		平均回收率
(mean)/%		RSD/%
咖啡酸(caffeic acid)8.628 58.469 817.209 6101.399.32.7
8.638 816.838 796.8
8.633 116.798 996.4
8.626 217.369 0103.2
8.631 916.968 298.4
8.635 417.085 299.8
阿福豆苷(afzelin)0.750 30.740 91.484 898.298.73.7
0.751 21.450 593.5
0.750 71.515 5102.3
0.750 11.496 699.8
0.750 61.517 9102.6
0.750 91.465 995.6
没食子酸(gallic acid)27.010 826.006 453.376 9101.4101.51.6
27.043 254.128 4104.2
27.025 253.325 5101.1
27.003 653.057 8100.2
27.021 652.975 599.8
27.032 453.685 7102.5
新绿原酸(neochlorogenic acid)234.468 8232.942 5473.782 6102.798.02.7
234.750 0456.287 195.1
234.593 8464.136 898.5
234.406 3462.506 597.9
234.562 5459.110 196.4
234.656 3461.283 897.3
绿原酸(chlorogenic acid)313.102 2310.627 5609.060 595.397.83.7
313.475 8611.515 496.0
313.267 1619.840 998.7
313.016 7611.195 296.0
313.225 4619.733 3104.8
313.350 6612.476 196.3
隐绿原酸(cryptochlorogenic acid)309.573 8306.130 6611.327 998.697.11.0
309.945 1609.234 297.8
309.738 8605.570 496.6
309.491 3605.570 496.7
309.697 6607.664 097.3
309.821 3602.953 395.8
红景天苷(salidroside)3 268.757 03 233.569 66 557.991 9101.799.71.9
3 272.677 96 395.679 096.6
3 270.499 66 525.529 3100.7
3 267.885 76 495.385 599.8
3 270.064 06 530.166 8100.8
3 271.370 96 458.285 498.6
紫丁香苷(eleutheroside B)23.109 223.772 446.118 196.899.13.2
23.137 046.572 398.7
23.121 648.071 2105.0
23.103 146.027 396.4
23.118 546.935 7100.2
23.127 746.390 697.9
人参皂苷Re(ginsenoside Re)747.148 7741.949 91 463.778 696.699.22.6
748.045 01 490.154 5100.0
747.547 11 456.205 395.5
746.949 61 501.122 7101.7
767.447 51 502.950 8101.8
747.746 21 485.976 199.5
人参皂苷Rg1(ginsenoside Rg1)842.136 7844.897 61 652.171 595.9101.33.1
843.146 91 690.982 6100.4
842.585 71 722.031 5104.1
841.912 21 690.982 6100.5
842.473 41 722.031 5104.1
842.810 21 714.269 3103.1
人参皂苷Rd(ginsenoside Rd)1 902.760 81 907.136 03 786.672 398.899.91.0
1 905.043 23 794.450 799.1
1 903.775 23 821.675 3100.6
1 902.253 63 825.564 5100.9
1 903.521 63 825.564 5100.8
1 904.282 43 794.450 799.1
), ArticleFig(id=1239250721292473060, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, language=EN, label=Tab.4, caption=

Content determination of 11 components in Hongwushen capsules

, figureFileSmall=null, figureFileBig=null, tableContent=
样品批号
(sample No.)		含量(content)/(mg·g-1)
咖啡酸
(caffeic acid)		阿福豆苷
(afzelin)		没食子酸
(gallic acid)		新绿原酸
(neochlorogenic acid)		绿原酸
(chlorogenic acid)		隐绿原酸
(cryptochlorogenic acid)		红景天苷
(salidroside)		紫丁香苷
(eleutheroside B)		人参皂苷Re
(ginsenoside Re)		人参皂苷Rg1
(ginsenoside Rg1)		人参皂苷Rd
(ginsenoside Rd)
202110010.011 50.000 80.036 00.312 50.417 30.412 64.357 40.030 80.995 81.121 42.536 0
202110020.010 40.000 90.037 10.311 60.416 70.413 84.356 30.031 00.994 91.122 42.537 2
202110030.012 30.001 00.036 80.312 30.413 70.414 94.355 70.031 60.996 01.122 02.536 1
202110040.011 10.000 90.038 20.314 40.413 30.415 54.356 00.030 90.995 21.123 52.535 7
202110050.010 50.001 20.035 80.315 20.417 40.410 64.356 60.031 80.994 41.121 62.535 8
202110060.013 30.001 00.036 40.312 60.413 90.412 74.358 10.032 10.995 71.123 82.537 6
202110070.012 00.000 70.037 70.313 90.412 80.411 74.355 90.030 60.993 41.121 82.536 9
202110080.011 40.001 10.036 20.315 10.416 10.412 84.356 70.031 40.995 91.120 42.538 2
202110090.013 40.001 40.034 90.314 90.415 80.415 34.355 60.030 30.996 71.121 22.537 8
202110100.013 10.001 10.036 70.312 40.412 60.411 54.354 80.031 50.998 51.122 52.536 5
), ArticleFig(id=1239250721393136359, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250710890598576, language=CN, label=表4, caption=

红五参胶囊中11个成分的含量测定(n=2)

, figureFileSmall=null, figureFileBig=null, tableContent=
样品批号
(sample No.)		含量(content)/(mg·g-1)
咖啡酸
(caffeic acid)		阿福豆苷
(afzelin)		没食子酸
(gallic acid)		新绿原酸
(neochlorogenic acid)		绿原酸
(chlorogenic acid)		隐绿原酸
(cryptochlorogenic acid)		红景天苷
(salidroside)		紫丁香苷
(eleutheroside B)		人参皂苷Re
(ginsenoside Re)		人参皂苷Rg1
(ginsenoside Rg1)		人参皂苷Rd
(ginsenoside Rd)
202110010.011 50.000 80.036 00.312 50.417 30.412 64.357 40.030 80.995 81.121 42.536 0
202110020.010 40.000 90.037 10.311 60.416 70.413 84.356 30.031 00.994 91.122 42.537 2
202110030.012 30.001 00.036 80.312 30.413 70.414 94.355 70.031 60.996 01.122 02.536 1
202110040.011 10.000 90.038 20.314 40.413 30.415 54.356 00.030 90.995 21.123 52.535 7
202110050.010 50.001 20.035 80.315 20.417 40.410 64.356 60.031 80.994 41.121 62.535 8
202110060.013 30.001 00.036 40.312 60.413 90.412 74.358 10.032 10.995 71.123 82.537 6
202110070.012 00.000 70.037 70.313 90.412 80.411 74.355 90.030 60.993 41.121 82.536 9
202110080.011 40.001 10.036 20.315 10.416 10.412 84.356 70.031 40.995 91.120 42.538 2
202110090.013 40.001 40.034 90.314 90.415 80.415 34.355 60.030 30.996 71.121 22.537 8
202110100.013 10.001 10.036 70.312 40.412 60.411 54.354 80.031 50.998 51.122 52.536 5
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UPLC-MS/MS法同时测定红五参胶囊中11个成分的含量*
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孙帅 1 , 王相 1 , 高乐 1 , 谢文超 2 , 刘宸男 1 , 牛丽颖 1 , 王鑫国 1, **
药物分析杂志 | 成分分析 2024,44(4): 567-576
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药物分析杂志 | 成分分析 2024, 44(4): 567-576
UPLC-MS/MS法同时测定红五参胶囊中11个成分的含量*
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孙帅1 , 王相1, 高乐1, 谢文超2, 刘宸男1, 牛丽颖1, 王鑫国1, **
作者信息
  • 1.河北中医药大学 河北省中药配方颗粒技术创新中心 中药材品质评价与标准化河北省工程研究中心，石家庄050091
  • 2.华北制药河北华维健康产业有限公司，石家庄 052165

    • Tel：(0311)89926890；E-mail：

通讯作者:

** Tel：(0311)89926548；E-mail：
Simultaneous determination of 11 components in Hongwushen capsules by UPLC-MS/MS*
Shuai SUN1 , Xiang WANG1, Le GAO1, Wen-chao XIE2, Chen-nan LIU1, Li-ying NIU1, Xin-guo WANG1, **
Affiliations
  • 1.Hebei University of Chinese Medicine, Hebei Traditional Chinese Medicine Formula Granule Engineering & Technology Innovate Center, Quality Evaluation & Standardization Hebei Province Engineering Research Center of Traditional Chinese Medicine, Shijiazhuang 050091, China
  • 2.NCPC Hebei Huawei Health Industry Co., Ltd., Shijiazhuang 052165, China
出版时间: 2024-04-30 doi: 10.16155/j.0254-1793.2024.04.03
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摘要
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目的：

建立UPLC-MS/MS同时测定红五参胶囊中11个成分(咖啡酸、阿福豆苷、没食子酸、新绿原酸、绿原酸、隐绿原酸、红景天苷、紫丁香苷、人参皂苷Re、人参皂苷Rg1、人参皂苷Rd)含量的方法。

方法：

采用Shim-pack GIST C18(100 mm×2.1 mm，2 μm)色谱柱，以乙腈-0.1%乙酸-1 mmol·L-1乙酸铵水溶液为流动相，梯度洗脱，流速0.3 mL·min-1，柱温30 ℃，进样量为1 μL；采用电喷雾电离源(ESI源)，多反应监测(MRM)模式进行正负离子检测。

结果：

11个成分在测定浓度范围内线性关系良好，线性相关系数r均>0.999 0；精密度RSD均<3%；重复性和稳定性良好，RSD值均<5%；平均加样回收率为97.1%~101.5%，RSD≤3.7%。10批红五参胶囊中咖啡酸、阿福豆苷、没食子酸、新绿原酸、绿原酸、隐绿原酸、红景天苷、紫丁香苷、人参皂苷Re、人参皂苷Rg1、人参皂苷Rd含量分别为0.010~0.013、0.000 7~0.001 4、0.035~0.038、0.312~0.315、0.413~0.417、0.411~0.416、4.355~4.358、0.030~0.032、0.993~0.999、1.120~1.124、2.536~2.538 mg·g-1。

结论：

本方法准确灵敏，稳定性和重复性良好，可用于红五参胶囊的质量控制。

红五参胶囊  /  红景天  /  刺五加  /  人参  /  大健康产品  /  红景天苷  /  人参皂苷Rd  /  超高效液相色谱-串联质谱  /  多重反应监测  /  多成分含量测定  /  质量控制
Objective:

To establish an UPLC-MS/MS method for simultaneous determination of 11 components(caffeic acid, afzelin, gallic acid, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, salidroside, eleutheroside B, ginsenoside Re, ginsenoside Rg1, ginsenoside Rd) in Hongwushen capsules.

Methods:

A Shim-pack GIST C18 chromatographic column(100 mm×2.1 mm, 2 μm) was used. The mobile phase was composed of acetonitrile -0.1% acetic acid -1 mmol·L-1 ammonium acetate aqueous solution and the gradient elution was applied. The flow rate was 0.3 mL·min-1, the column temperature was 30 ℃, and the injection volume was 1 μL. Electrospray ionization (ESI) source and multiple reaction monitoring (MRM) mode in both positive and negative were used for ion detections.

Results:

The linear relationship of 11 components was good in the concentration range, and the linear correlation coefficients were all above 0.999 0. The RSD values of precision were less than 3%. The repeatability and stability were good, and the RSD values were less than 5%. The average recoveries were in the range of 97.1%-101.5% with RSDs≤3.7%. The contents of caffeic acid, afzelin, gallic acid, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, salidroside, eleutheroside B, ginsenoside Re, ginsenoside Rg1 and ginsenoside Rd in 10 batches of Hongwushen capsules were 0.010-0.013 mg·g-1, 0.000 7-0.001 4 mg·g-1, 0.035-0.038 mg·g-1, 0.312-0.315 mg·g-1, 0.413-0.417 mg·g-1, 0.411-0.416 mg·g-1, 4.355-4.358 mg·g-1, 0.030-0.032 mg·g-1, 0.993-0.999 mg·g-1, 1.120-1.124 mg·g-1 and 2.536-2.538 mg·g-1, respectively.

Conclusions:

The method is accurate, sensitive, stable and reproducible, and can be used for the quality control of Hongwushen capsules.

Hongwushen capsule  /  Rhodiola crenulata  /  Acanthopanax senticosus  /  ginseng  /  big health products  /  salidroside  /  ginsenoside Rd  /  UPLC-MS/MS  /  multiple reaction monitoring  /  multi-component content determination  /  quality control
孙帅, 王相, 高乐, 谢文超, 刘宸男, 牛丽颖, 王鑫国. UPLC-MS/MS法同时测定红五参胶囊中11个成分的含量*. 药物分析杂志, 2024 , 44 (4) : 567 -576 . DOI: 10.16155/j.0254-1793.2024.04.03
Shuai SUN, Xiang WANG, Le GAO, Wen-chao XIE, Chen-nan LIU, Li-ying NIU, Xin-guo WANG. Simultaneous determination of 11 components in Hongwushen capsules by UPLC-MS/MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2024 , 44 (4) : 567 -576 . DOI: 10.16155/j.0254-1793.2024.04.03
正文
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红五参胶囊是一款大健康产品，由红景天、刺五加、人参茎叶3味中药组成。红景天，景天科植物大花红景天Rhodiola crenulata (Hook. f. et Thoms.) H. Ohba的干燥根和根茎，是亚洲地区公认滋补食材，素有“高原人参”和“雪山仙草”之称，可益气活血、通脉平喘；刺五加，五加科植物刺五加Acanthopanax senticosus (Rupr. et Maxim.) Harms的干燥根和根茎或茎，又名“五加参”，可益气健脾、补肾安神，具有免疫调节、抗疲劳、抗肿瘤、抗衰老、抗疲劳等作用[1-2]；人参茎叶，五加科植物人参Panax ginseng C. A. Mey.的干燥茎叶，可补气、益肺、祛暑、生津。3味中药合用能益气活血、补肺安中，缓解体力疲劳。
红五参胶囊质量控制中仅对红景天苷及总皂苷进行限度规定，其他药效成分暂未涉及，难以体现其质量控制的整体性。因此，建立一个高效、准确且能同时满足制剂中所有药味的质量控制方法尤为重要。试验前期已采用超高效液相色谱法对红五参胶囊中的成分进行含量测定，发现检测灵敏度较低，分析时间较长，多成分分离困难，且人参茎叶中的皂苷类成分难以被检测到，不能满足分析要求，难以对红五参胶囊进行质量控制。UPLC-MS/MS法专属性强，灵敏度高，可在短时间内完成多种成分的含量测定，也可以检出和测定含量较低的成分[3-6]。因此，本实验建立了UPLC-MS/MS方法同时测定红五参胶囊中红景天(红景天苷、阿福豆苷、没食子酸、咖啡酸)、刺五加(紫丁香苷、新绿原酸、绿原酸、隐绿原酸)和人参茎叶(人参皂苷Rg1、人参皂苷Re、人参皂苷Rd)中11个成分的含量，为红五参胶囊的质量控制提升提供依据。
1　仪器与试药
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Shimadzu LC-30A型超高效液相色谱仪(岛津公司)，4500 QTRAP三重四极杆线性离子阱质谱仪(SCIEX公司，ESI离子源)，Analyst® TF 1.6.3数据采集软件(SCIEX公司)，BSA224S-CW型万分之一、CPA225D型十万分之一电子分析天平(赛多利斯科学仪器北京有限公司)，KQ-250型超声波清洗器(昆山市超声仪器有限公司)，KD-98-IIA电热恒温水浴锅(天津市泰斯特仪器有限公司)。
对照品红景天苷(批号15120801，纯度≥97%)、人参皂苷Rd(批121115，纯度98%)，成都普菲德生物技术有限公司；没食子酸(批号110831-201906，纯度≥89.9%)、人参皂苷Rg1(批号110703-202235，纯度≥93.4%)、人参皂苷Re(批号110754-202330，纯度≥93.4%)、绿原酸(批号110753-202119，纯度≥98%)、咖啡酸(批号10885-201703，纯度≥95%)，中国食品药品检研究院；隐绿原酸(批号PS001110，纯度≥98%)、阿福豆苷(批号PS011206，纯度≥98%)、紫丁香苷(批号PS010261，纯度≥98%)，成都普思生物科技股份有限公司；新绿原酸(批号MUST-12113001，纯度≥98%)，成都曼思特生物科技有限公司。乙腈、甲醇为色谱纯，Merck公司；其他试剂均为分析纯，实验用水为屈臣氏蒸馏水。
红五参胶囊（批号20211001-20211010）由华北制药河北华维健康产业有限公司提供。
2　方法与结果
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2.1　色谱-质谱条件
2.1.1　色谱条件
采用Shim-pack GIST C18(100 mm×2.1 mm，2 μm)色谱柱，柱温30 ℃，以0.1%乙酸-1 mmol·L-1乙酸铵水溶液为流动相A，乙腈为流动相B，梯度洗脱(0~4 min，5%B→10%B；4~8 min，10%B→13%B；8~12 min，13%B→17%B；12~15 min，17%B→30%B；15~17 min，30%B→34%B；17~19 min，34%B；19~20 min，34%B→35%B；20~21 min，35%B→37%B；21~23 min，37%B；23~25 min，37%B→50%B；25~30 min，50%B→60%B；30~32 min，60%B→75%B；32~36 min，75%B)，每次进样前预平衡5 min，再进行梯度洗脱，流速0.3 mL·min-1，进样量1 μL。
2.1.2　质谱条件
采用多重反应监测(MRM)的扫描方式在正、负离子模式下同时监测，离子源为电喷雾离子源(ESI)，离子化电压(IS)为5 500 V和-4 500 V，离子源温度(TEM)为550 ℃，喷雾气(GS1，N2)为380 kPa，辅助气(GS2，N2)为380 kPa，接口持续加热，全程通入氮气，气帘气(CUR，N2)为242 kPa，碰撞气(CAD)压力为medium，每个离子对的滞留时间(dwelltime)为50 ms。每个待测化合物的监测离子对、解簇电压(DP)及碰撞能量(CE)见表1。
2.2　溶液制备
2.2.1　混合对照品溶液
分别精密称取对照品咖啡酸1.323 mg、阿福豆苷7.056 mg、没食子酸7.224 mg、新绿原酸1.553 mg、绿原酸2.071 mg、紫丁香苷1.189 mg，置5 mL量瓶中，加甲醇溶解、稀释并定容，得上述6个成分的对照品储备液；分别精密称取对照品隐绿原酸3.688 mg、红景天苷27.876 mg、人参皂苷Re 9.104 mg、人参皂苷Rg15.827 mg、人参皂苷Rd 15.893 mg，置10 mL量瓶中，加甲醇溶解、稀释并定容，得上述5个成分的对照品储备液。分别精密吸取各对照品储备液适量，置10 mL量瓶中，加甲醇稀释至刻度，摇匀，即得每1 mL含咖啡酸0.002 6 mg、阿福豆苷0.000 1 mg、没食子酸0.014 4 mg、新绿原酸0.031 1 mg、绿原酸0.041 42 mg、隐绿原酸0.036 9 mg、红景天苷0.278 8 mg、紫丁香苷0.023 8 mg、人参皂苷Re 0.045 5 mg、人参皂苷Rg1 0.029 1 mg和人参皂苷Rd 0.158 9 mg的混合对照品溶液。
2.2.2　供试品溶液
取胶囊内容物适量，研磨至细粉，精密称取1.5 g，置于50 mL具塞锥形瓶中，加入70%甲醇25 mL，密塞，精密称量，超声(功率250 W，频率40 kHz)处理30 min，取出放冷，再称量，用70%甲醇补足减失的量，摇匀，滤过，精密量取上清液10 mL至蒸发皿中，水浴加热(100 ℃)至干，放冷，用70%甲醇复溶，定容至5 mL，摇匀，取上清液，用0.22 μm微孔滤膜滤过，即得。
2.2.3　阴性溶液
取聚维酮K30和乳糖的混合物(1∶3)1.5 g，精密称定，置于50 mL具塞锥形瓶中，按“2.2.2”项方法操作，即得。
2.3　方法学考察
2.3.1　专属性考察
分别精密吸取阴性溶液、混合对照品溶液和供试品溶液各1 μL，按“2.1”项下条件进样分析得到正、负离子流图见图1。供试品溶液中待测的11个成分与11个对照品的保留时间相同，被测定成分分离效果良好，无阴性干扰，比较各对照品与样品的色谱图，见图2，二者一致，表明本法专属性良好。
2.3.2　线性关系考察及定量限和检测限测定
精密量取“2.2.1”项混合对照品溶液适量，用甲醇稀释2.5、5、10、12.5、16.6、50倍，得到11个成分的系列混合对照品溶液。分别精密吸取上述溶液1 μL，按“2.1”项下条件进样分析。以对照品进样浓度(X)为横坐标，以峰面积(Y)为纵坐标，绘制坐标曲线，计算得到各成分的回归方程和线性范围，见表2。结果显示，11个成分在各自的范围内呈良好的线性关系，表明本方法线性良好。将混合对照品溶液逐步稀释，以信噪比S/N=3和S/N=10分别计算11个成分的检测限(LOD)和定量限(LOQ)，结果见表2。
2.3.3　精密度试验
精密吸取“2.2.1”项下混合对照品溶液1 μL，按“2.1”项下条件，连续进样6次，测定峰面积，计算咖啡酸、阿福豆苷、没食子酸、新绿原酸、绿原酸、隐绿原酸、红景天苷、紫丁香苷、人参皂苷Re、人参皂苷Rg1、人参皂苷Rd峰面积的RSD分别为2.0%、2.5%、2.5%、2.9%、1.8%、1.5%、1.8%、2.0%、2.8%、2.5%、2.5%，均<3%，表明仪器精密度良好。
2.3.4　稳定性试验
取同一批次红五参胶囊样品(批号20211001)，按“2.2.2”项下方法制备供试品溶液，分别于0、2、6、12、18、24 h按“2.1”项下条件进样分析，测定峰面积。所得咖啡酸、阿福豆苷、没食子酸、新绿原酸、绿原酸、隐绿原酸、红景天苷、紫丁香苷、人参皂苷Re、人参皂苷Rg1、人参皂苷Rd峰面积的RSD(n=6)分别为1.6%、1.6%、1.0%、4.7%、2.0%、0.77%、4.5%、1.0%、2.8%、1.5%、1.8%，表明供试品溶液在24 h内稳定性良好。
2.3.5　重复性试验
取同一批次红五参胶囊(批号20211001)，分别精密称取低(0.75 g)、中(1.50 g)、高(2.25 g)3个水平样品量，每个水平3份样品，按“2.2.2”项下方法制备供试品溶液，精密吸取各供试品溶液1 μL，按“2.1”项下条件进样分析，测定峰面积，计算含量，结果咖啡酸、阿福豆苷、没食子酸、新绿原酸、绿原酸、隐绿原酸、红景天苷、紫丁香苷、人参皂苷Re、人参皂苷Rg1、人参皂苷Rd的平均质量分数(n=9)分别为0.012、0.001、0.036、0.313、0.417、0.413、4.357、0.031、0.996、1.122、2.536 mg·g-1，RSD分别为1.7%、3.2%、0.74%、4.8%、3.1%、3.5%、3.3%、4.7%、4.0%、4.8%、4.3%，表明该方法重复性良好。
2.3.6　加样回收率试验
取同一批次(批号20211001)已知含量的红五参胶囊内容物粉末6份，每份约0.75 g，精密称定，加入与样品中各成分的已知含有量相当的对照品溶液，按“2.2.2”项下方法制备供试溶液，精密吸取各供试溶液1 μL，按“2.1”项下条件进样分析，测定峰面积，分别计算11个成分的加样回收率。结果见表3，表明该方法准确度良好。
2.4　样品含量测定
精密称取10批红五参胶囊样品，按“2.2.2”项下方法制备供试品溶液，精密吸取供试品溶液1 μL，按“2.2.2”项下液质联用条件进样分析，测定峰面积，计算含量。结果见表4。
3　讨论
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为了实现被测成分的快速分离，试验中考察了不同流动相体系(甲醇-0.1%甲酸水溶液、乙腈-0.1%甲酸水溶液、乙腈-0.1%乙酸水溶液、乙腈-0.1%乙酸-0.5 mmol·L-1乙酸铵水溶液、乙腈-0.1%乙酸-1 mmo·L-1乙酸铵水溶液、乙腈-0.1%乙酸-2 mmo·L-1乙酸铵水溶液)进行梯度洗脱。结果发现乙腈的洗脱能力更强，有利于有效成分的分离检出；乙酸可以改善色谱峰的拖尾现象，使峰形更好；加入乙酸铵可以提高被测成分的质谱响应，因此选用乙腈-0.1%乙酸-1 mmol·L-1乙酸铵水溶液为流动相洗脱体系。
前期进行的红五参胶囊特征图谱试验中进行了提取溶剂(甲醇、70%甲醇、50%甲醇、乙醇、70%乙醇、50%乙醇)和提取时间(超声20 min、超声30 min、超声40 min、冷浸24 h)的考察，发现采用70%甲醇、超声30 min时待测成分含量较高，最终选取以70%甲醇为提取溶剂，超声30 min的提取方式提取有效成分。试验中发现将样品浓缩1倍，可以使更多的有效成分被检出，便于更好地进行质量控制。同时试验考察了不同浓缩方法及温度对待测成分的影响，包括常压浓缩(100 ℃)、减压浓缩(40、50、60 ℃)。不同处理方式下，待测成分的含量如图3，综合各成分的提取情况，常压浓缩(100 ℃)的方式所提取出的样品中成分含量相对较高，因此选取常压浓缩样品的提取方式。
质谱分析中同分异构体有相同的裂解行为，难以区分，因此通过调整流动相比例进行分离，试验中实现了新绿原酸、绿原酸、隐绿原酸以及人参皂苷Re和人参皂苷Rd 2对同分异构体的分离，能在较短时间快速分离和检测目标化合物。
红五参胶囊具有缓解疲劳的功效，试验中所检测的11个成分均有相关的药理活性。研究发现红景天苷可以减轻氧化应激损伤，从而实现缓解疲劳的作用[7-8]。研究表明黄酮类化合物可以降低羟基自由基和DPPH自由基的半抑制浓度[9-10]；有机酸类成分通过对DPPH自由基的较强清除，来实现缓解疲劳的功效[11]，因此黄酮类成分阿福豆苷、有机酸类成分没食子酸、咖啡酸、新绿原酸、绿原酸、隐绿原酸均具有较好的缓解疲劳作用。研究发现紫丁香苷可能是通过减少乳酸在肌肉中的积累，来保护肌肉组织从而发挥缓解疲劳作用[12-13]。
人参皂苷Rg1可加速调节线粒体生物合成的作用，通过PGC-1α途径最终达到缓解疲劳的效果[14]。人参皂苷Re可使下丘脑5-HT、Ach和GA-BA水平均显著性降低，DA含量则显著性上升[15-16]，起到缓解疲劳的作用。原人参二醇型皂苷人参皂苷Rd可以提高肌糖原和肝糖原含量、降低血清中LD含量及提高LDH活力[17]来缓解疲劳。本研究针对红五参胶囊中的每味药材均建立多成分的含量测定方法，且被测的11个成分均与缓解疲劳活性相关，对临床应用及评价控制红五参胶囊质量具有重要意义。
试验采用UPLC-MS/MS法测定了11个有效成分，该方法灵敏度高，专属性强，重复性良好，能够在36 min内快速实现对目标成分的分离和含量测定，具有高选择性、高灵敏度的特点。11个有效成分中红景天苷、阿福豆苷来源于红景天，紫丁香苷、新绿原酸、绿原酸和隐绿原酸来源于刺五加，人参皂苷Rg1、人参皂苷Re和人参皂苷Rd来源于人参茎叶，咖啡酸、没食子酸为红景天和刺五加共有。本实验对每一味药均进行质量控制，以期更全面地控制红五参胶囊的质量，为建立红五参胶囊的质量控制方法提供科学依据。
基金
收起
  • *河北省省级科技计划项目(23372502D)
  • 河北省自然科学基金项目(H2022423341)
  • 河北省自然科学基金项目(H2022423335)
  • 国家级大学生创新创业训练计划项目(202214432020)
  • 河北中医药管理局项目(2022107)
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2024年第44卷第4期
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doi: 10.16155/j.0254-1793.2024.04.03
  • 接收时间：2023-07-18
  • 首发时间：2026-03-13
  • 出版时间：2024-04-30
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  • 收稿日期：2023-07-18
基金
*河北省省级科技计划项目(23372502D)
河北省自然科学基金项目(H2022423341)
河北省自然科学基金项目(H2022423335)
国家级大学生创新创业训练计划项目(202214432020)
河北中医药管理局项目(2022107)
作者信息
    1.河北中医药大学 河北省中药配方颗粒技术创新中心 中药材品质评价与标准化河北省工程研究中心，石家庄050091
    2.华北制药河北华维健康产业有限公司，石家庄 052165

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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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