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Article(id=1239184758400406113, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239184752507408921, articleNumber=null, orderNo=null, doi=10.16155/j.0254-1793.2024-0218, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1711900800000, receivedDateStr=2024-04-01, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773374269341, onlineDateStr=2026-03-13, pubDate=1735574400000, pubDateStr=2024-12-31, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773374269341, onlineIssueDateStr=2026-03-13, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773374269341, creator=13701087609, updateTime=1773374269341, updator=13701087609, issue=Issue{id=1239184752507408921, tenantId=1146029695717560320, journalId=1205117023404326918, year='2024', volume='44', issue='12', pageStart='2011', pageEnd='2188', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1773374267937, creator=13701087609, updateTime=1773374446543, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1239185501702377864, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239184752507408921, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1239185501702377865, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239184752507408921, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=2154, endPage=2163, ext={EN=ArticleExt(id=1239184758677230194, articleId=1239184758400406113, tenantId=1146029695717560320, journalId=1205117023404326918, language=EN, title=Research on the quality evaluation method of Alpiniae Officinarum Rhizoma based on quantitative analysis of multi-components by single marker method*, columnId=1206272758774821315, journalTitle=Chinese Journal of Pharmaceutical Analysis, columnName=Standard Deliberation, runingTitle=null, highlight=null, articleAbstract=
Objective:

To establish a quantitative analysis of multi-components by single marker (QAMS) method to simultaneously determine the contents of kalangin, diphenylheptane A, galangin, kaempferin and galangin-3-O-methyl ether.

Methods:

Hypersil ODS2 C18 (250 mm×4.6 mm, 5 μm) was used by high performance liquid chromatography (HPLC) and was eluted with 0.3% acetic acid in water (A) and acetonitrile (B) (0-2 min, 10%B→15%B；2-5 min, 15%B→20%B；5-20 min, 20%B→35%B；20-30 min, 35%B→40%B；30-55 min, 40%B；55-60 min, 40%B→100%B), the column temperature was 30 ℃, the volume flow rate was 0.8 mL·min-1, and the detection wavelength was 254 nm. The relative correction factors of each chemical component were calculated with gingerin as the internal reference, and the content was determined, which was compared with the results of the external standard method, and the quality of galangal from different origins was evaluated by chemical pattern recognition.

Results:

Kaempferol, diphenylheptane A, galangin, kaempferin and galangin-3-O-methyl ether had a good linear relationship in the ranges of 0.005 5-0.110 0, 0.140 0-2.800 0, 0.149 6-2.992 0, 0.021 5-0.430 0 and 0.022 2-0.444 0 μg, respectively, and the average sample recoveries were 100.7%, 101.4%, 99.9%, 100.9% and 101.7%, respectively. The RSDs were 1.3%, 2.8%, 0.83%, 1.4% and 1.8%, respectively. Quantitative analysis of multicomponents by single marker method and external standard method was no significant difference in the results.

Conclusion:

This method is rapid, accurate and specific, which can provide a reference for the quality control of galangal.

, correspAuthors=Yu DONG, 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=Hui WANG, Xiao-ling ZHU, Guo-yuan SUN, Jin-yang HU, Guang-jun XIANG, Yu DONG), CN=ArticleExt(id=1239184764008190719, articleId=1239184758400406113, tenantId=1146029695717560320, journalId=1205117023404326918, language=CN, title=基于一测多评法的高良姜质量评价方法研究*, columnId=1206272758971953622, journalTitle=药物分析杂志, columnName=标准研讨, runingTitle=null, highlight=null, articleAbstract=
目的：

建立一测多评法同时测定高良姜水提物中山柰酚、二苯基庚烷A、高良姜素、山柰素和高良姜素-3-O-甲醚的含量。

方法：

采用高效液相色谱法（HPLC）测定，色谱柱为Hypersil ODS2 C18(250 mm×4.6 mm，5 μm)，以0.3%乙酸水溶液（A）-乙腈（B）为流动相，梯度洗脱（0~2 min，10%B→15%B；2~5 min，15%B→20%B；5~20 min，20%B→35%B；20~30 min，35%B→40%B；30~55 min，40%B；55~60 min，40%B→100%B），柱温30 ℃，体积流量0.8 mL·min-1，检测波长254 nm。以高良姜素为内参物，计算各化学成分的相对校正因子，并进行含量测定，与外标法测定结果进行比较，并结合化学模式识别评价不同产地高良姜的质量。

结果：

山柰酚、二苯基庚烷A、高良姜素、山柰素和高良姜素-3-O-甲醚进样量分别在0.005 5~0.110 0、0.140 0~2.800 0、0.149 6~2.992 0、0.021 5~0.430 0和0.022 2~0.444 0 μg范围内线性关系良好，平均加样回收率分别为100.7%、101.4%、99.9%、100.9%和101.7%，RSD分别为1.3%、2.8%、0.83%、1.4%和1.8%。一测多评法与外标法所测结果无明显差异。

结论：

该方法快速准确且专属性强，可为高良姜的质量控制提供参考依据。

, correspAuthors=董玉, authorNote=null, correspAuthorsNote=
**Tel：（0471）6653081；E-mail：
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Tel：（0471）6653081；E-mail：

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Guiyang：Guizhou University，2016, articleTitle=Optimization of Pilot Process and Hypoglycemic Activity of Kaemphara, refAbstract=null), Reference(id=1239218786126057950, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, doi=null, pmid=null, pmcid=null, year=2022, volume=33, issue=11, pageStart=2612, pageEnd=null, url=null, language=null, rfNumber=[13], rfOrder=21, authorNames=秦华珍, 牛新迈, 谢旭格, journalName=时珍国医国药, refType=null, unstructuredReference=秦华珍，牛新迈，谢旭格，等. 高良姜、大高良姜黄酮类成分对胃溃疡寒证大鼠胃组织PGE2、EGF和血清IL-8、TNF-α等指标的影响[J]. 时珍国医国药，2022，33(11)：2612, articleTitle=高良姜、大高良姜黄酮类成分对胃溃疡寒证大鼠胃组织PGE2、EGF和血清IL-8、TNF-α等指标的影响, refAbstract=null), Reference(id=1239218786222526946, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, doi=null, pmid=null, pmcid=null, year=2022, volume=33, issue=11, pageStart=2612, pageEnd=null, url=null, language=null, rfNumber=[13], rfOrder=22, authorNames=QIN HZ, NIU XM, XIE XG, journalName=Lishizhen Med Mater Med Res, refType=null, unstructuredReference=QIN HZ，NIU XM，XIE XG，et al. 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Biomed Pharmacother，2017，89：845, articleTitle=Galangin potentiates human breast cancer to apoptosis induced by TRAIL through activating AMPK, refAbstract=null)], funds=[Fund(id=1239218783324262765, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, awardId=82060773, language=CN, fundingSource=*国家自然科学基金项目(82060773), fundOrder=null, country=null), Fund(id=1239218783445897585, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, awardId=2020GG0117, language=CN, fundingSource=内蒙古自治区科技成果转化项目(2020GG0117), fundOrder=null, country=null), Fund(id=1239218783554949494, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, awardId=NMGIRT2226, language=CN, fundingSource=内蒙古自治区高等学校青年科技人才发展计划项目(NMGIRT2226), fundOrder=null, country=null), Fund(id=1239218783689167227, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, awardId=2019ZD16, language=CN, fundingSource=内蒙古自治区自然科学基金重点项目(2019ZD16), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1239218772981109702, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, xref=1., ext=[AuthorCompanyExt(id=1239218772989498312, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, companyId=1239218772981109702, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.School of Pharmacy, Inner Mongolia Medical University, Hohhot 010110, China), AuthorCompanyExt(id=1239218773098550222, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, companyId=1239218772981109702, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.内蒙古医科大学药学院，呼和浩特 010110)]), AuthorCompany(id=1239218773186630618, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, xref=2, ext=[AuthorCompanyExt(id=1239218773195019225, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, companyId=1239218773186630618, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 Engineering Technology Research Center for Medicinal Substances and Quality Control of Mongolian Medicines, Inner Mongolia Autonomous Region, Hohhot 010110, China), AuthorCompanyExt(id=1239218773199213531, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, companyId=1239218773186630618, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.内蒙古自治区蒙药药效物质与质量控制工程技术研究中心，呼和浩特 010110)]), AuthorCompany(id=1239218773308265446, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, xref=3, ext=[AuthorCompanyExt(id=1239218773320848360, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, companyId=1239218773308265446, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3 Department of Pharmacology, Inner Mongolia International Mongolian Medicine Hospital, Hohhot 010065, China), AuthorCompanyExt(id=1239218773325042665, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, companyId=1239218773308265446, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3.内蒙古自治区国际蒙医医院药学部，呼和浩特 010065)])], figs=[ArticleFig(id=1239218778718916823, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Fig.1, caption=HPLC chromatograms of Alpiniae Officinarum Rhizoma test sample(A) and mixed referece substances(B), figureFileSmall=2ITkEZjp/+Ys4UfcbAN/Eg==, figureFileBig=VRWMLziTIYALzNy/Ctg3JA==, tableContent=null), ArticleFig(id=1239218778827968734, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=图1, caption=高良姜样品（A）及混合对照品（B）的高效液相色谱图

1.山柰酚（kaempferol）　2.二苯基庚烷A（diphenylheptane A）　3.高良姜素（galangin）　4.山柰素（kaempferin）　5.高良姜素-3-O-甲醚（galangin-3-O-methyl ether）

, figureFileSmall=2ITkEZjp/+Ys4UfcbAN/Eg==, figureFileBig=VRWMLziTIYALzNy/Ctg3JA==, tableContent=null), ArticleFig(id=1239218779973013729, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Fig.2, caption=Dendrogram of cluster analysis of 13 batches of Alpiniae Officinarum Rhizoma samples, figureFileSmall=vHIQR5X3a2nPYSdK6ohTRQ==, figureFileBig=YLPrGUCFo9/Hl1l5xQCBHA==, tableContent=null), ArticleFig(id=1239218780094648549, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=图2, caption=13批高良姜样品聚类分析树状图, figureFileSmall=vHIQR5X3a2nPYSdK6ohTRQ==, figureFileBig=YLPrGUCFo9/Hl1l5xQCBHA==, tableContent=null), ArticleFig(id=1239218780207894759, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Fig.3, caption=OPLS-DA score plot of 13 batches of Alpiniae Officinarum Rhizoma samples, figureFileSmall=0L+wv1Y5alT8Nws4nYepZg==, figureFileBig=dug0TzW6U73NEz8gveVuHg==, tableContent=null), ArticleFig(id=1239218780325335276, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=图3, caption=13批高良姜样品OPLS-DA得分图, figureFileSmall=0L+wv1Y5alT8Nws4nYepZg==, figureFileBig=dug0TzW6U73NEz8gveVuHg==, tableContent=null), ArticleFig(id=1239218780438581489, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Fig.4, caption=OPLS-DA displacement test diagram of 13 batches of Alpiniae Officinarum Rhizoma samples, figureFileSmall=JXHa5MZ78AzzsuROm1G/CQ==, figureFileBig=o2kyT6wYEfogSTYtM0N/LQ==, tableContent=null), ArticleFig(id=1239218780535050484, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=图4, caption=13批高良姜样品OPLS-DA置换检验图, figureFileSmall=JXHa5MZ78AzzsuROm1G/CQ==, figureFileBig=o2kyT6wYEfogSTYtM0N/LQ==, tableContent=null), ArticleFig(id=1239218780623130874, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Fig.5, caption=VIP diagram of 13 batches of Alpiniae Officinarum Rhizoma samples, figureFileSmall=L0dypoDYBFS2YdWCtpdGwA==, figureFileBig=6CtQceRtMiBvEEbldnjCDw==, tableContent=null), ArticleFig(id=1239218780765737213, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=图5, caption=13批高良姜样品VIP图, figureFileSmall=L0dypoDYBFS2YdWCtpdGwA==, figureFileBig=6CtQceRtMiBvEEbldnjCDw==, tableContent=null), ArticleFig(id=1239218780891566337, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Tab.1, caption=

Sources of Alpiniae Officinarum Rhizoma medicinal materials

, figureFileSmall=null, figureFileBig=null, tableContent=
批号
（batch No.）		编号
（sample No.）		产地
（habitat）
202001S1广东徐闻曲界(Xuwen Qu’jie，Guangdong)
202002S2广东徐闻海安(Xuwen Hai’an，Guangdong)
202003S3广东徐闻龙塘(Xuwen Longtang，Guangdong)
202004S4广东海康(Haikang，Guangdong)
202005S5广东徐闻城北(North of Xuwen City，Guangdong)
202006S6广东惠阳(Huiyang，Guangdong)
202007S7广东徐闻仙桥(Xuwen xian Bridge，Guangdong)
202008S8广东徐闻前山(Xuwen qian Mountain，Guangdong)
202009S9广东徐闻(Xuwen，Guangdong)
202010S10广东徐闻南山(Xuwen Nanshan，Guangdong)
21120603S11广西(Guangxi)
202011S12广西百色(Baise，Guangxi)
202012S13广西陆川(Luchuan，Guangxi)
), ArticleFig(id=1239218781004812548, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=表1, caption=

高良姜药材来源

, figureFileSmall=null, figureFileBig=null, tableContent=
批号
（batch No.）		编号
（sample No.）		产地
（habitat）
202001S1广东徐闻曲界(Xuwen Qu’jie，Guangdong)
202002S2广东徐闻海安(Xuwen Hai’an，Guangdong)
202003S3广东徐闻龙塘(Xuwen Longtang，Guangdong)
202004S4广东海康(Haikang，Guangdong)
202005S5广东徐闻城北(North of Xuwen City，Guangdong)
202006S6广东惠阳(Huiyang，Guangdong)
202007S7广东徐闻仙桥(Xuwen xian Bridge，Guangdong)
202008S8广东徐闻前山(Xuwen qian Mountain，Guangdong)
202009S9广东徐闻(Xuwen，Guangdong)
202010S10广东徐闻南山(Xuwen Nanshan，Guangdong)
21120603S11广西(Guangxi)
202011S12广西百色(Baise，Guangxi)
202012S13广西陆川(Luchuan，Guangxi)
), ArticleFig(id=1239218781122253066, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Tab.2, caption=

Regression equations，correlation coefficients，and linear ranges

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)		回归方程
(regression equation)		 r线性范围
(linear range)/μg
山柰酚（kaempferol） Y=4 193X-0.265 30.999 90.005 5~0.110 0
二苯基庚烷A（diphenylheptane A） Y=238.2X+1.3720.999 90.140 0~2.800 0
高良姜素（galangin） Y=4 865X+17.930.999 90.149 6~2.992 0
山柰素（kaempferin） Y=4 585X-0.919 00.999 90.021 5~0.430 0
高良姜素-3-O-甲醚（galangal-3-O-methyl ether） Y=5 396X+2.1340.999 90.022 2~0.444 0
), ArticleFig(id=1239218781227110669, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=表2, caption=

回归方程、相关系数和线性范围

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)		回归方程
(regression equation)		 r线性范围
(linear range)/μg
山柰酚（kaempferol） Y=4 193X-0.265 30.999 90.005 5~0.110 0
二苯基庚烷A（diphenylheptane A） Y=238.2X+1.3720.999 90.140 0~2.800 0
高良姜素（galangin） Y=4 865X+17.930.999 90.149 6~2.992 0
山柰素（kaempferin） Y=4 585X-0.919 00.999 90.021 5~0.430 0
高良姜素-3-O-甲醚（galangal-3-O-methyl ether） Y=5 396X+2.1340.999 90.022 2~0.444 0
), ArticleFig(id=1239218781331968273, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Tab.3, caption=

Results of sample recovery test

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		样品含量
（content in sample）/μg		加入量
（added content）/μg		测得量
（measured content）/μg		回收率
（recovery）/%		平均回收率
（average recovery）/%		RSD/%
山柰酚（kaempferol）3.177 43.136 06.333 8100.7100.71.3
3.177 73.136 06.381 7102.2
3.177 83.136 06.290 499.3
3.178 33.136 06.371 4101.8
3.178 43.136 06.360 7101.5
3.177 73.136 06.284 099.1
二苯基庚烷A
（diphenylheptane A）		230.595 5231.000 0458.523 798.7101.42.8
230.617 6231.000 0461.384 899.9
230.629 5231.000 0472.602 8104.8
230.660 8231.000 0469.909 5103.6
230.670 9231.000 0470.067 0103.6
230.621 2231.000 0457.285 298.1
高良姜素（galangin）105.791 9106.000 0211.964 4100.299.90.83
105.802 0106.000 0212.437 2100.6
105.807 5106.000 0210.433 098.7
105.821 8106.000 0212.399 5100.5
105.826 5106.000 0212.119 5100.3
105.803 7106.000 0210.679 098.9
山柰素（kaempferin）25.729 926.000 052.187 0101.8100.91.4
25.732 326.000 052.266 2102.1
25.733 726.000 051.466 599.0
25.737 226.000 052.169 0101.7
25.738 326.000 052.168 6101.7
25.732 826.000 051.515 199.2
高良姜-3-O-甲醚（galangal-3-O-methyl ether）15.450 715.500 030.982 5100.2101.71.8
15.452 215.500 030.972 5100.1
15.453 015.500 031.393 0102.8
15.455 115.500 030.975 0100.1
15.455 815.500 031.628 2104.3
15.452 515.500 031.337 6102.5
), ArticleFig(id=1239218781432631573, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=表3, caption=

加样回收率试验结果（n=6）

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		样品含量
（content in sample）/μg		加入量
（added content）/μg		测得量
（measured content）/μg		回收率
（recovery）/%		平均回收率
（average recovery）/%		RSD/%
山柰酚（kaempferol）3.177 43.136 06.333 8100.7100.71.3
3.177 73.136 06.381 7102.2
3.177 83.136 06.290 499.3
3.178 33.136 06.371 4101.8
3.178 43.136 06.360 7101.5
3.177 73.136 06.284 099.1
二苯基庚烷A
（diphenylheptane A）		230.595 5231.000 0458.523 798.7101.42.8
230.617 6231.000 0461.384 899.9
230.629 5231.000 0472.602 8104.8
230.660 8231.000 0469.909 5103.6
230.670 9231.000 0470.067 0103.6
230.621 2231.000 0457.285 298.1
高良姜素（galangin）105.791 9106.000 0211.964 4100.299.90.83
105.802 0106.000 0212.437 2100.6
105.807 5106.000 0210.433 098.7
105.821 8106.000 0212.399 5100.5
105.826 5106.000 0212.119 5100.3
105.803 7106.000 0210.679 098.9
山柰素（kaempferin）25.729 926.000 052.187 0101.8100.91.4
25.732 326.000 052.266 2102.1
25.733 726.000 051.466 599.0
25.737 226.000 052.169 0101.7
25.738 326.000 052.168 6101.7
25.732 826.000 051.515 199.2
高良姜-3-O-甲醚（galangal-3-O-methyl ether）15.450 715.500 030.982 5100.2101.71.8
15.452 215.500 030.972 5100.1
15.453 015.500 031.393 0102.8
15.455 115.500 030.975 0100.1
15.455 815.500 031.628 2104.3
15.452 515.500 031.337 6102.5
), ArticleFig(id=1239218781558460700, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Tab.4, caption=

fs/i for the four components

, figureFileSmall=null, figureFileBig=null, tableContent=
进样量
（injection volume）/μL		 fs/i
山柰酚
（kaempferol）		二苯基庚烷A
（diphenylheptane A）		山柰素
（kaempferin）		高良姜素-3-O-甲醚
（galangal-3-O-methyl ether）
11.189 321.308 31.139 50.893 1
21.191 719.722 71.048 50.902 3
51.167 620.177 71.062 50.902 6
101.164 320.496 21.067 60.904 2
151.164 020.422 01.071 10.904 9
201.162320.387 31.058 80.900 1
平均值（mean）1.173 220.419 01.074 70.901 2
RSD/%1.22.53.00.48
), ArticleFig(id=1239218781680095522, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=表4, caption=

4个化学成分的fs/i

, figureFileSmall=null, figureFileBig=null, tableContent=
进样量
（injection volume）/μL		 fs/i
山柰酚
（kaempferol）		二苯基庚烷A
（diphenylheptane A）		山柰素
（kaempferin）		高良姜素-3-O-甲醚
（galangal-3-O-methyl ether）
11.189 321.308 31.139 50.893 1
21.191 719.722 71.048 50.902 3
51.167 620.177 71.062 50.902 6
101.164 320.496 21.067 60.904 2
151.164 020.422 01.071 10.904 9
201.162320.387 31.058 80.900 1
平均值（mean）1.173 220.419 01.074 70.901 2
RSD/%1.22.53.00.48
), ArticleFig(id=1239218781793341732, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Tab.5, caption=

fs/i measured by different instruments and columns

, figureFileSmall=null, figureFileBig=null, tableContent=
仪器
（instrument）		色谱柱
（column）		 fs/i
山柰酚
（kaempferol）		二苯基庚烷A
（diphenylheptane A）		山柰素
（kaempferin）		高良姜素-3-O-甲醚
（galangal-3-O-methyl ether）
Agilent 1260Agilent Eclipse Plus C181.169 420.942 81.082 50.941 2
Hypersil ODS21.162 320.387 31.058 80.900 1
Shimadzu Shim-pack GIST1.187 120.943 71.089 20.907 6
ShimadzuAgilent Eclipse Plus C181.101 120.345 81.044 50.903 3
Hypersil ODS21.124 720.060 61.030 00.877 2
Shimadzu Shim-pack GIST1.126 720.360 91.060 40.908 4
平均值（mean）1.145 220.506 81.060 90.906 3
RSD/%2.91.72.12.3
), ArticleFig(id=1239218781889810729, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=表5, caption=

不同仪器及色谱柱测得的fs/i

, figureFileSmall=null, figureFileBig=null, tableContent=
仪器
（instrument）		色谱柱
（column）		 fs/i
山柰酚
（kaempferol）		二苯基庚烷A
（diphenylheptane A）		山柰素
（kaempferin）		高良姜素-3-O-甲醚
（galangal-3-O-methyl ether）
Agilent 1260Agilent Eclipse Plus C181.169 420.942 81.082 50.941 2
Hypersil ODS21.162 320.387 31.058 80.900 1
Shimadzu Shim-pack GIST1.187 120.943 71.089 20.907 6
ShimadzuAgilent Eclipse Plus C181.101 120.345 81.044 50.903 3
Hypersil ODS21.124 720.060 61.030 00.877 2
Shimadzu Shim-pack GIST1.126 720.360 91.060 40.908 4
平均值（mean）1.145 220.506 81.060 90.906 3
RSD/%2.91.72.12.3
), ArticleFig(id=1239218782024028463, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Tab.6, caption=

Effect of different flow rates on fs/i

, figureFileSmall=null, figureFileBig=null, tableContent=
流速
（flow rate）/(mL·min-1)		 fs/i
山柰酚
（kaempferol）		二苯基庚烷A
（diphenylheptane A）		山柰素
（kaempferin）		高良姜素-3-O-甲醚
（galangal-3-O-methyl ether）
0.71.204 320.924 51.064 80.893 2
0.81.162 320.387 31.058 80.900 1
0.91.167 121.068 61.063 30.897 1
平均值（mean）1.177 920.793 51.062 30.896 8
RSD/%2.01.70.290.38
), ArticleFig(id=1239218782116303158, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=表6, caption=

不同流速对fs/i的影响

, figureFileSmall=null, figureFileBig=null, tableContent=
流速
（flow rate）/(mL·min-1)		 fs/i
山柰酚
（kaempferol）		二苯基庚烷A
（diphenylheptane A）		山柰素
（kaempferin）		高良姜素-3-O-甲醚
（galangal-3-O-methyl ether）
0.71.204 320.924 51.064 80.893 2
0.81.162 320.387 31.058 80.900 1
0.91.167 121.068 61.063 30.897 1
平均值（mean）1.177 920.793 51.062 30.896 8
RSD/%2.01.70.290.38
), ArticleFig(id=1239218782246326587, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Tab.7, caption=

Effect of different column temperatures on the fs/i

, figureFileSmall=null, figureFileBig=null, tableContent=
柱温
（column temperatures）/℃		 fs/i
山柰酚
（kaempferol）		二苯基庚烷A
（diphenylheptane A）		山柰素
（kaempferin）		高良姜-3-O-甲醚
（galangal-3-O-methyl ether）
251.146 421.032 21.073 30.895 0
301.162 320.387 31.058 80.900 1
351.187 521.147 81.054 30.896 4
平均值（mean）1.165 420.855 71.062 10.897 1
RSD/%1.82.00.930.29
), ArticleFig(id=1239218782367961404, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=表7, caption=

不同柱温对fs/i的影响

, figureFileSmall=null, figureFileBig=null, tableContent=
柱温
（column temperatures）/℃		 fs/i
山柰酚
（kaempferol）		二苯基庚烷A
（diphenylheptane A）		山柰素
（kaempferin）		高良姜-3-O-甲醚
（galangal-3-O-methyl ether）
251.146 421.032 21.073 30.895 0
301.162 320.387 31.058 80.900 1
351.187 521.147 81.054 30.896 4
平均值（mean）1.165 420.855 71.062 10.897 1
RSD/%1.82.00.930.29
), ArticleFig(id=1239218782472819010, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Tab.8, caption=

Relative retention time of each component

, figureFileSmall=null, figureFileBig=null, tableContent=
仪器
（instrument）		色谱柱
（column）		 ri/s
山柰酚
（kaempferol）		二苯基庚烷A
（diphenylheptane A）		山柰素
（kaempferin）		高良姜素-3-O-甲醚
（galangal-3-O-methyl ether）
Agilent1260Agilent Eclipse Plus C180.577 40.850 91.032 81.137 9
Hypersil ODS20.656 80.881 81.038 21.080 0
Shimadzu Shim-pack GIST0.593 10.813 21.044 41.119 4
ShimadzuAgilent Eclipse Plus C180.609 00.852 51.028 51.125 3
Hypersil ODS20.638 20.868 01.034 41.088 2
Shimadzu Shim-pack GIST0.621 20.824 01.039 91.108 1
平均值（mean）0.615 90.848 41.036 41.109 8
RSD/%4.73.10.542.0
), ArticleFig(id=1239218782607036742, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=表8, caption=

各成分相对保留时间

, figureFileSmall=null, figureFileBig=null, tableContent=
仪器
（instrument）		色谱柱
（column）		 ri/s
山柰酚
（kaempferol）		二苯基庚烷A
（diphenylheptane A）		山柰素
（kaempferin）		高良姜素-3-O-甲醚
（galangal-3-O-methyl ether）
Agilent1260Agilent Eclipse Plus C180.577 40.850 91.032 81.137 9
Hypersil ODS20.656 80.881 81.038 21.080 0
Shimadzu Shim-pack GIST0.593 10.813 21.044 41.119 4
ShimadzuAgilent Eclipse Plus C180.609 00.852 51.028 51.125 3
Hypersil ODS20.638 20.868 01.034 41.088 2
Shimadzu Shim-pack GIST0.621 20.824 01.039 91.108 1
平均值（mean）0.615 90.848 41.036 41.109 8
RSD/%4.73.10.542.0
), ArticleFig(id=1239218782737060174, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Tab.9, caption=

Determination results of five components in Alpiniae Officinarum Rhizoma

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
（sample No.）		含量（content）/（mg·g-1）
高良姜素
（galangin）		山柰酚
（kaempferol）		二苯基庚烷A
（diphenylheptane A）		山柰素
（kaempferin）		高良姜素-3-O-甲醚
（galangal-3-O-methyl ether）
ESMQAMSESMRSD/%QAMSESMRSD/%QAMSESMRSD/%QAMSESMRSD/%
S10.555 80.018 20.018 10.661.078 21.076 50.110.126 80.124 91.00.072 40.072 30.14
S20.563 50.021 40.021 30.0930.877 10.875 80.110.120 00.118 21.10.103 90.103 80.10
S30.446 50.019 70.019 50.661.027 21.025 60.110.082 70.081 51.10.061 20.061 10.16
S40.262 80.007 60.007 50.670.610 30.609 40.110.059 20.058 31.00.040 90.040 80.090
S50.409 50.018 80.018 70.640.969 90.968 40.110.083 70.082 51.10.071 10.071 00.14
S60.201 00.007 60.007 50.670.527 10.526 30.110.039 60.039 01.00.036 80.036 80.090
S70.650 00.011 40.011 30.621.229 91.227 90.110.119 50.117 81.10.057 10.057 10.18
S80.322 30.009 90.009 80.711.561 71.559 30.110.118 00.116 21.00.130 80.130 60.77
S90.537 30.020 80.020 60.681.201 51.199 60.110.118 10.116 31.00.082 50.082 40.12
S100.468 40.023 40.023 20.641.108 41.106 70.110.097 00.095 61.00.071 30.071 30.14
S110.286 50.006 80.006 70.590.705 50.704 40.110.060 10.059 21.00.041 60.041 50.090
S120.278 30.008 30.008 30.600.525 80.525 00.110.051 40.050 61.00.041 70.041 60.090
S130.241 10.007 70.007 60.650.676 20.675 20.110.049 80.049 11.00.045 00.044 90.090
), ArticleFig(id=1239218782917415254, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=表9, caption=

高良姜中5个成分的含量测定结果

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
（sample No.）		含量（content）/（mg·g-1）
高良姜素
（galangin）		山柰酚
（kaempferol）		二苯基庚烷A
（diphenylheptane A）		山柰素
（kaempferin）		高良姜素-3-O-甲醚
（galangal-3-O-methyl ether）
ESMQAMSESMRSD/%QAMSESMRSD/%QAMSESMRSD/%QAMSESMRSD/%
S10.555 80.018 20.018 10.661.078 21.076 50.110.126 80.124 91.00.072 40.072 30.14
S20.563 50.021 40.021 30.0930.877 10.875 80.110.120 00.118 21.10.103 90.103 80.10
S30.446 50.019 70.019 50.661.027 21.025 60.110.082 70.081 51.10.061 20.061 10.16
S40.262 80.007 60.007 50.670.610 30.609 40.110.059 20.058 31.00.040 90.040 80.090
S50.409 50.018 80.018 70.640.969 90.968 40.110.083 70.082 51.10.071 10.071 00.14
S60.201 00.007 60.007 50.670.527 10.526 30.110.039 60.039 01.00.036 80.036 80.090
S70.650 00.011 40.011 30.621.229 91.227 90.110.119 50.117 81.10.057 10.057 10.18
S80.322 30.009 90.009 80.711.561 71.559 30.110.118 00.116 21.00.130 80.130 60.77
S90.537 30.020 80.020 60.681.201 51.199 60.110.118 10.116 31.00.082 50.082 40.12
S100.468 40.023 40.023 20.641.108 41.106 70.110.097 00.095 61.00.071 30.071 30.14
S110.286 50.006 80.006 70.590.705 50.704 40.110.060 10.059 21.00.041 60.041 50.090
S120.278 30.008 30.008 30.600.525 80.525 00.110.051 40.050 61.00.041 70.041 60.090
S130.241 10.007 70.007 60.650.676 20.675 20.110.049 80.049 11.00.045 00.044 90.090
), ArticleFig(id=1239218783013884253, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=EN, label=Tab.10, caption=

Eigenvalues and variance contribution rates of the five principal components

, figureFileSmall=null, figureFileBig=null, tableContent=
主成分
（principal component）		特征值
（eigenvalue）		方差贡献率
（variance contribution rate）/%		累计方差贡献率
（cumulative variance contribution rate）/%
13.67473.47373.473
20.77515.49688.969
30.3817.61696.585
40.1523.04999.635
50.0180.365100.000
), ArticleFig(id=1239218783106158946, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239184758400406113, language=CN, label=表10, caption=

5个主成分的特征值和方差贡献率

, figureFileSmall=null, figureFileBig=null, tableContent=
主成分
（principal component）		特征值
（eigenvalue）		方差贡献率
（variance contribution rate）/%		累计方差贡献率
（cumulative variance contribution rate）/%
13.67473.47373.473
20.77515.49688.969
30.3817.61696.585
40.1523.04999.635
50.0180.365100.000
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基于一测多评法的高良姜质量评价方法研究*
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王慧 1, 2 , 朱小玲 2, 3 , 孙国园 2, 3 , 胡锦阳 1, 2 , 向广军 1, 2 , 董玉 1, 2, **
药物分析杂志 | 标准研讨 2024,44(12): 2154-2163
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药物分析杂志 | 标准研讨 2024, 44(12): 2154-2163
基于一测多评法的高良姜质量评价方法研究*
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王慧1, 2 , 朱小玲2, 3, 孙国园2, 3, 胡锦阳1, 2, 向广军1, 2, 董玉1, 2, **
作者信息
  • 1.内蒙古医科大学药学院，呼和浩特 010110
  • 2.内蒙古自治区蒙药药效物质与质量控制工程技术研究中心，呼和浩特 010110
  • 3.内蒙古自治区国际蒙医医院药学部，呼和浩特 010065

    • Tel：（0471）6653081；E-mail：

通讯作者:

**Tel：（0471）6653081；E-mail：
Research on the quality evaluation method of Alpiniae Officinarum Rhizoma based on quantitative analysis of multi-components by single marker method*
Hui WANG1, 2 , Xiao-ling ZHU2, 3, Guo-yuan SUN2, 3, Jin-yang HU1, 2, Guang-jun XIANG1, 2, Yu DONG1, 2, **
Affiliations
  • 1.School of Pharmacy, Inner Mongolia Medical University, Hohhot 010110, China
  • 2 Engineering Technology Research Center for Medicinal Substances and Quality Control of Mongolian Medicines, Inner Mongolia Autonomous Region, Hohhot 010110, China
  • 3 Department of Pharmacology, Inner Mongolia International Mongolian Medicine Hospital, Hohhot 010065, China
出版时间: 2024-12-31 doi: 10.16155/j.0254-1793.2024-0218
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摘要
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目的：

建立一测多评法同时测定高良姜水提物中山柰酚、二苯基庚烷A、高良姜素、山柰素和高良姜素-3-O-甲醚的含量。

方法：

采用高效液相色谱法（HPLC）测定，色谱柱为Hypersil ODS2 C18(250 mm×4.6 mm，5 μm)，以0.3%乙酸水溶液（A）-乙腈（B）为流动相，梯度洗脱（0~2 min，10%B→15%B；2~5 min，15%B→20%B；5~20 min，20%B→35%B；20~30 min，35%B→40%B；30~55 min，40%B；55~60 min，40%B→100%B），柱温30 ℃，体积流量0.8 mL·min-1，检测波长254 nm。以高良姜素为内参物，计算各化学成分的相对校正因子，并进行含量测定，与外标法测定结果进行比较，并结合化学模式识别评价不同产地高良姜的质量。

结果：

山柰酚、二苯基庚烷A、高良姜素、山柰素和高良姜素-3-O-甲醚进样量分别在0.005 5~0.110 0、0.140 0~2.800 0、0.149 6~2.992 0、0.021 5~0.430 0和0.022 2~0.444 0 μg范围内线性关系良好，平均加样回收率分别为100.7%、101.4%、99.9%、100.9%和101.7%，RSD分别为1.3%、2.8%、0.83%、1.4%和1.8%。一测多评法与外标法所测结果无明显差异。

结论：

该方法快速准确且专属性强，可为高良姜的质量控制提供参考依据。

一测多评  /  高良姜  /  含量测定  /  聚类分析  /  质量评价
Objective:

To establish a quantitative analysis of multi-components by single marker (QAMS) method to simultaneously determine the contents of kalangin, diphenylheptane A, galangin, kaempferin and galangin-3-O-methyl ether.

Methods:

Hypersil ODS2 C18 (250 mm×4.6 mm, 5 μm) was used by high performance liquid chromatography (HPLC) and was eluted with 0.3% acetic acid in water (A) and acetonitrile (B) (0-2 min, 10%B→15%B；2-5 min, 15%B→20%B；5-20 min, 20%B→35%B；20-30 min, 35%B→40%B；30-55 min, 40%B；55-60 min, 40%B→100%B), the column temperature was 30 ℃, the volume flow rate was 0.8 mL·min-1, and the detection wavelength was 254 nm. The relative correction factors of each chemical component were calculated with gingerin as the internal reference, and the content was determined, which was compared with the results of the external standard method, and the quality of galangal from different origins was evaluated by chemical pattern recognition.

Results:

Kaempferol, diphenylheptane A, galangin, kaempferin and galangin-3-O-methyl ether had a good linear relationship in the ranges of 0.005 5-0.110 0, 0.140 0-2.800 0, 0.149 6-2.992 0, 0.021 5-0.430 0 and 0.022 2-0.444 0 μg, respectively, and the average sample recoveries were 100.7%, 101.4%, 99.9%, 100.9% and 101.7%, respectively. The RSDs were 1.3%, 2.8%, 0.83%, 1.4% and 1.8%, respectively. Quantitative analysis of multicomponents by single marker method and external standard method was no significant difference in the results.

Conclusion:

This method is rapid, accurate and specific, which can provide a reference for the quality control of galangal.

QAMS  /  galangal  /  content determination  /  cluster analysis  /  quality evaluation
王慧, 朱小玲, 孙国园, 胡锦阳, 向广军, 董玉. 基于一测多评法的高良姜质量评价方法研究*. 药物分析杂志, 2024 , 44 (12) : 2154 -2163 . DOI: 10.16155/j.0254-1793.2024-0218
Hui WANG, Xiao-ling ZHU, Guo-yuan SUN, Jin-yang HU, Guang-jun XIANG, Yu DONG. Research on the quality evaluation method of Alpiniae Officinarum Rhizoma based on quantitative analysis of multi-components by single marker method*[J]. Chinese Journal of Pharmaceutical Analysis, 2024 , 44 (12) : 2154 -2163 . DOI: 10.16155/j.0254-1793.2024-0218
正文
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高良姜是姜科山姜属植物高良姜Alpinia officinarum Hance的干燥根茎，呈圆柱形，外表皮棕红色至暗棕色，气香，味辛辣[1]。高良姜中含有的主要化学成分为挥发油类、黄酮类、二芳基庚烷类、苯丙素类、糖苷类等[2-3]，具有抗菌、抗病毒、抗氧化、抗肿瘤、抗溃疡和胃黏膜保护等药理作用[4-8]。高良姜的化学成分较多，有些对照品很难获取，有些化学性质不稳定容易变质，有些价格昂贵。一测多评（QAMS）是从量上阐述主要化学成分或药效成分间的相互关系[9]，解决对照品短缺的问题，为中药多指标成分的含量测定以及质量控制提供参考。
因此，本课题组尝试将QAMS法应用于高良姜中山柰酚、二苯基庚烷A、高良姜素、山柰素、高良姜素-3-O-甲醚5个化学成分的含量测定，为高良姜质量评价提供研究思路。
1　仪器与试药
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1.1　仪器
Agilent 1260高效液相色谱仪（安捷伦公司）和Shimadzu LC-16型二元高效液相色谱仪（岛津仪器有限公司）；CPA225D型十万分之一分析天平（赛多利斯科学仪器有限公司），KQ-250DE型数控超声波清洗仪（昆山市超声仪器有限公司）。
1.2　试药
对照品山柰酚（批号20221227001，纯度≥98%）、二苯基庚烷A（批号20210326001，纯度≥98%）、山柰素（批号20221120001，纯度≥98%）和高良姜素-3-O-甲醚（批号20210511001，纯度≥98%）购于上海鼓臣生物技术有限公司，高良姜素（批号111699-202204，纯度≥98%）购于中国食品药品检定研究院；HPLC级乙腈和甲醇购于Fisher公司，水为纯净水，其余试剂为分析纯。13个批次高良姜购买于内蒙古天力药业有限公司，经内蒙古医科大学药学院李骁副教授鉴定为姜科山姜属植物高良姜Alpinia officinarum Hance的干燥根茎，样品信息见表1。
2　方法和结果
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2.1　色谱条件
采用Hypersil ODS2 C18色谱柱（250 mm×4.6 mm，5 μm），以0.3%乙酸水溶液（A）-乙腈（B）为流动相，梯度洗脱（0~2 min，10%B→15%B；2~5 min，15%B→20%B；5~20 min，20%B→35%B；20~30 min，35%B→40%B；30~55 min，40%B；55~60 min，40%B→100%B），体积流量0.8 mL·min-1，检测波长254 nm，柱温30 ℃，进样量20 μL。色谱图如图1所示。
2.2　对照品溶液的制备
精密称取山柰酚对照品2.31 mg、高良姜素-3-O-甲醚对照品5.54 mg、山柰素对照品2.15 mg，分别置于10 mL量瓶中，加甲醇定容，摇匀，制成质量浓度分别为0.231 mg·mL-1的山柰酚储备液、0.554 mg·mL-1的高良姜素-3-O-甲醚储备液和0.215 mg·mL-1的山柰素储备液。精密称取高良姜素对照品3.74 mg，二苯基庚烷A对照品3.50 mg，置于25 mL量瓶中，并加入上述山柰酚储备液0.6 mL，高良姜素-3-O-甲醚储备液1 mL及山柰素2.5 mL，加甲醇定容，摇匀，制成山柰酚、二苯基庚烷A、高良姜素、山柰素、高良姜-3-O-甲醚质量浓度分别为0.005 5、0.140 0、0.149 6、0.021 5、0.022 2 mg·mL-1的混合对照品溶液。
2.3　供试品母液的制备
取过5目筛的高良姜药材粉末适量，置于圆底烧瓶中，加10倍量蒸馏水，采用水蒸气蒸馏法回流提取2次，第1次提取5 h，第2次提取1 h，趁热过滤合并滤液，真空浓缩即得。
2.4　线性关系考察
取“2.2”项混合对照品溶液，分别按“2.1”项下色谱条件进样1、2、5、10、15、20 μL，记录峰面积。以化学成分的进样量X为横坐标，峰面积Y为纵坐标，绘制标准曲线。结果见表2。
2.5　精密度试验
取“2.2”项混合对照品溶液，按“2.1”项下色谱条件连续进样测定6次，测得山柰酚、二苯基庚烷A、高良姜素、山柰素和高良姜素-3-O-甲醚峰面积的RSD(n=6)分别为0.95%、0.10%、0.12%、0.18%和0.17%，表明仪器精密度良好。
2.6　稳定性试验
取高良姜供试品溶液，按“2.1”项下色谱条件，分别在0、2、4、6、8、12、24 h时进样测定，计算得到山柰酚、二苯基庚烷A、高良姜素、山柰素、高良姜素-3-O-甲醚峰面积的RSD分别为2.4%、0.75%、0.45%、1.1%和0.63%，表明供试品溶液在24 h内稳定性良好。
2.7　重复性试验
取高良姜药材（S11）6份，每份约50.0 g，精密称定，按“2.3”项方法制备供试品母液，分别用水定容于250 mL量瓶中，精密吸取2 mL，用甲醇定容于10 mL量瓶中，超声（40 kHz，250 W）溶解15 min，定量滤纸过滤，取续滤液，过0.45 μm的有机微孔滤膜，取续滤液作为供试溶液。按“2.1”项下色谱条件分别进样分析，测得山柰酚、二苯基庚烷A、高良姜素、山柰素、高良姜素-3-O-甲醚的平均含量分别为0.015 8、1.149 3、0.527 3、0.128 2、0.077 0 mg·g-1，RSD分别为2.9%、1.5%、0.75%、1.9%和1.8%，符合方法学验证要求，表明该方法重复性良好。
2.8　加样回收率试验
取已知含量的高良姜药材（S11）6份，每份约25.0 g，精密称定，按“2.3”项下方法制备供试品母液，用水分别定容于250 mL量瓶中，精密吸取2 mL，且分别精密加入0.002 24 mg·mL-1的山柰酚对照品溶液1.4 mL、0.231 mg·mL-1的二苯基庚烷A对照品溶液1 mL、0.106 mg·mL-1的高良姜素对照品溶液1 mL、0.026 0 mg·mL-1的山柰素对照品溶液1 mL、0.015 5 mg·mL-1的高良姜素-3-O-甲醚对照品溶液1 mL，用甲醇定容于10 mL量瓶中，超声（40 kHz，250 W）溶解15 min，定量滤纸过滤，取续滤液，过0.45 μm的有机微孔滤膜，取续滤液作为供试溶液。按“2.1”项下色谱条件分别进样分析，计算山柰酚、二苯基庚烷A、高良姜素、山柰素、高良姜素-3-O-甲醚的平均加样回收率和RSD，结果见表3，表明方法的准确度良好。
2.9　QAMS法的研究
2.9.1　相对校正因子的计算
取“2.2”项混合对照品溶液，按“2.1”项下色谱条件分别进样 1、2、5、10、15、20 μL，记录峰面积，以高良姜素为内参物，计算相对校正因子（fs/i）=CiAs/CsAi，式中Ci为组分i的浓度，式中As为内标物s的峰面积，Cs为内标物s的浓度，Ai为组分i的峰面积。结果见表4。
2.9.2　不同仪器及色谱柱对fs/i的影响
取“2.2”项混合对照品溶液，考察了2种HPLC系统及3种不同品牌的色谱柱对fs/i的影响，结果表明均无显著性差异。见表5。
2.9.3　不同体积流量对fs/i的影响
取“2.2”项混合对照品溶液，采用Agilent 1260高效液相色谱仪系统，Hypersil ODS2 C18色谱柱，考察不同体积流量（0.7、0.8、0.9 mL·min-1）对各个化学成分fs/i的影响，各成分之间fs/i重复性良好，其RSD均<3.0%，表明不同体积流量对各成分fs/i无显著性影响。见表6。
2.9.4　不同柱温对fs/i的影响
取上述同一混合对照品溶液，采用Agilent 1260高效液相色谱仪系统，Hypersil ODS2 C18色谱柱，考察不同柱温（25、30、35 ℃）条件下的各个化学成分fs/i，结果显示各成分之间fs/i的RSD均<3.0%，表明柱温对各成分的fs/i无显著性影响。见表7。
2.9.5　待测成分色谱峰定位
取“2.2”项混合对照品溶液，按“2.1”项下色谱条件进样测定，分别计算各个化学成分的相对保留时间（ri/s），结果见表8，RSD<5.0%，表明可利用相对保留时间对各成分进行定位。
2.9.6　样品含量测定
取13批样品，分别按“2.3”项下方法制备供试品母液，定容于100 mL量瓶中，精密量取4 mL，置于10 mL量瓶中，加甲醇定容，超声（40 kHz，250 W）溶解15 min，摇匀，滤纸过滤，取续滤液，再经0.45 μm微孔滤膜滤过，取续滤液即得供试品溶液。按“2.1”项下色谱条件进样测定，结果显示，QAMS法和外标法（ESM）所测结果无显著差异，见表9，表明QAMS法可用于高良姜药材的含量测定。
2.10　化学模式识别分析
2.10.1　聚类分析
采用SIMCA 14.1分析软件对“2.9”项QAMS法测定的13批高良姜5个成分含量数据进行聚类分析。如图2所示，可将13批样品分为3类：S1、S2、S3、S5、S7、S9、S10聚为1类，S8聚为1类，S4、S6、S11、S12、S13聚为1类。由表1可知，S1、S2、S3、S5、S7、S8、S9、S10采集于广东徐闻，但S8采集于广东徐闻前山，该地属于热带季风气候，气候温暖，雨量充沛，山柰酚、二苯基庚烷A、高良姜素-3-O-甲醚的含量与其他产地差异明显，故单独聚为1类。第3类采集于广东海康、广东惠阳、广西等地，此类高良姜含量间并无明显差异，故归为1类。
2.10.2　主成分分析
采用SPSS 25.0分析软件对QAMS法测定的13批高良姜中5个成分含量数据进行主成分分析。由总方差结果看出，前2个主成分特征值分别为73.473%、15.496%，累计贡献率88.969%。因此，前2个成分即可代表高良姜88.969%的信息量，其中，第一主成分反映了山柰酚的信息，第二主成分反映了二苯基庚烷A的信息。见表10。
2.10.3　正交偏最小二乘-判别分析
采用SIMCA 14.1分析软件对QAMS法测定的13批高良姜5个化学成分含量数据进行正交偏最小二乘-判别分析（OPLS-DA）分析，其中，模型参数分别为R2X=0.89，R2Y=0.953，预测指数Q2=0.854，表明所建立的模型较为稳定可靠，可以用来区分不同批次的药材，见图3。对构建的OPLS-DA进行置换检验200次，结果显示，R2截距值为0.059 4（<0.3），所建立的模型稳定可靠，Q2截距值为-0.555（<0），说明所建立的模型稳定可靠，未过度拟合。可用于13批样品质量差异的有效判别。见图4。以变量重要性投影（variableimportanceinprojection，VIP）>1为标准，筛选出高良姜素-3-O-甲醚、高良姜素、二苯基庚烷A，这3个化学成分可能是高良姜药材的标志性成分。见图5。
3　讨论
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3.1　提取方法考察
本试验采用的提取溶剂为水，为后续配方颗粒的研究提供了参考，采用正交实验分别考察了提取次数、提取时间、加水体积及粉碎粒度，以所检测到高良姜中5个化学成分的含量为指标，最终确定的最佳提取工艺为提取2次，第1次提取5 h，第2次提取1 h，加10倍量的水，粉碎粒度为5目。
3.2　液相色谱条件的考察
采用二极管阵列检测器在200~400 nm范围内扫描得到光谱图，结果显示5个化学成分在254 nm波长处均有较大吸收。流动相分别比较了乙腈-水、乙腈-0.1%磷酸水、乙腈-0.3%乙酸水、甲醇-水、甲醇-0.1%磷酸水溶液；柱温比较了25、30和35 ℃。结果表明，柱温为30 ℃，波长为254 nm，流动相为乙腈-0.3%乙酸水溶液梯度洗脱时，待测成分的峰形较好，且分离度高，可用于高良姜中5个化学成分的含量测定。
3.3　指标性成分的选择
山柰酚、高良姜素、山柰素、高良姜素-3-O-甲醚具有抗炎、抗肿瘤、抗氧化、抗病毒、免疫调节、预防心血管疾病等药理作用[10-13]。二苯基庚烷A在抗炎、抗氧化、抗菌、抗病毒、抗肿瘤等方面也表现出较好的药理活性[14-15]。高良姜中黄酮类和二苯基庚烷类是主要的活性成分[2]，因此本文选择4个黄酮类和1个二苯基庚烷类作为指标性成分进行研究。
3.4　内参物的选择
高良姜素在高良姜中的含量较其他4个成分高，是主要的药理活性成分，且化学性质稳定，对照品价格较便宜，并且容易获得，保留时间适中，有助于其他化学成分色谱峰的相对保留时间的计算，故选择高良姜素为内参物。
3.5　小结
本研究建立了以高良姜素为内参物，同时测定高良姜药材中山柰酚、二苯基庚烷A、高良姜素、山柰素、高良姜素-3-O-甲醚5个成分含量的QAMS法，该方法检测简便，耐用性好，准确度高，成本较低，与各成分单独采用ESM测定含量比较，分析结果差异较小。同时，在试验过程中消耗的有机溶剂更少，在降低成本的同时减少了环境污染。通过QAMS法和ESM分析比对13批样品，并结合化学模式识别分析了影响药材质量标志性成分。QAMS法具有较好的精密度和准确度，方法学考察结果良好，可为高良姜药材的质量评价及标准制订提供依据。
基金
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  • *国家自然科学基金项目(82060773)
  • 内蒙古自治区科技成果转化项目(2020GG0117)
  • 内蒙古自治区高等学校青年科技人才发展计划项目(NMGIRT2226)
  • 内蒙古自治区自然科学基金重点项目(2019ZD16)
文献
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2024年第44卷第12期
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doi: 10.16155/j.0254-1793.2024-0218
  • 接收时间：2024-04-01
  • 首发时间：2026-03-13
  • 出版时间：2024-12-31
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  • 收稿日期：2024-04-01
基金
*国家自然科学基金项目(82060773)
内蒙古自治区科技成果转化项目(2020GG0117)
内蒙古自治区高等学校青年科技人才发展计划项目(NMGIRT2226)
内蒙古自治区自然科学基金重点项目(2019ZD16)
作者信息
    1.内蒙古医科大学药学院，呼和浩特 010110
    2.内蒙古自治区蒙药药效物质与质量控制工程技术研究中心，呼和浩特 010110
    3.内蒙古自治区国际蒙医医院药学部，呼和浩特 010065

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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
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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
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