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Article(id=1218551232780751086, tenantId=1146029695717560320, journalId=1189982191388893191, issueId=1218551229794403031, articleNumber=null, orderNo=null, doi=10.16438/j.0513-4870.2018-0248, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1521561600000, receivedDateStr=2018-03-21, revisedDate=1525363200000, revisedDateStr=2018-05-04, acceptedDate=null, acceptedDateStr=null, onlineDate=1768454853481, onlineDateStr=2026-01-15, pubDate=1536681600000, pubDateStr=2018-09-12, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1768454853481, onlineIssueDateStr=2026-01-15, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1768454853481, creator=13701087609, updateTime=1768454853481, updator=13701087609, issue=Issue{id=1218551229794403031, tenantId=1146029695717560320, journalId=1189982191388893191, year='2018', volume='53', issue='9', pageStart='1387', pageEnd='1582', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1768454852770, creator=13701087609, updateTime=1768457118357, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1218560732426322043, tenantId=1146029695717560320, journalId=1189982191388893191, issueId=1218551229794403031, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1218560732426322044, tenantId=1146029695717560320, journalId=1189982191388893191, issueId=1218551229794403031, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=1532, endPage=1535, ext={EN=ArticleExt(id=1218551233397313840, articleId=1218551232780751086, tenantId=1146029695717560320, journalId=1189982191388893191, language=EN, title=Determination of ginkgolic acids in Yinxing Tongzhi Dropping Pills by mix-mode SPE-UHPLC/MS/MS, columnId=1190335348761793317, journalTitle=Acta Pharmaceutica Sinica, columnName=ORIGINAL ARTICLES, runingTitle=null, highlight=null, articleAbstract=

An analytical method was developed for determination of ginkgolic acids in Yinxing Tongzhi Dropping Pills by ultra high performance liquid chromatography-triple quadrupole mass spectrometry. The samples were purified by mix-mode anion exchange and reversed-phase SPE. A chromatographic column, Waters Cortecs T3 (50 mm×2.1 mm, 2.7 μm), was used with acetonitrile-methanol-1% acetic acid (44:44:12) as the mobile phase. The ginkgolic acids were detected by electrospray ionization mass spectrometry in negative mode with multiple reaction monitoring (MRM) mode. Ginkgolic acid C13:0, C15:1 and C17:1 possessed good linear correlation in the mass concentration range from 0.2 to 200 μg·L-1, 2 to 200 μg·L-1, 4 to 200 μg·L-1, respectively, with the correlation coefficients more than 0.999. The mean recoveries at spiked levels of 50, 250 and 600 μg·kg-1 were in the range of 70.8%-95.1%, and the RSDs were 0.7%-8.6%. The limits of quantification were 1, 10, 20 μg·kg-1, respectively. The method could be applied to the analysis of ginkgolic acids in complex matrix samples.

, correspAuthors=Shen JI, authorNote=null, correspAuthorsNote=null, copyrightStatement=Copyright ©2018 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=Jian SUN, Xue-yi ZHANG, Li-min LI, Qing HU, Yan-rong ZHU, Xiu-hong MAO, Shen JI), CN=ArticleExt(id=1218551235414774295, articleId=1218551232780751086, tenantId=1146029695717560320, journalId=1189982191388893191, language=CN, title=混合型固相萃取-UHPLC/MS/MS法测定银杏酮酯滴丸中银杏酸含量, columnId=1190335348896011050, journalTitle=药学学报, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=

建立了超高效液相色谱串联三重四极杆质谱测定银杏酮酯滴丸中银杏酸的方法。采用混合型强阴离子反相吸附固相萃取净化样品，Waters Cortecs T3色谱柱（50 mm×2.1 mm，2.7 μm），以乙腈-甲醇-1%冰醋酸溶液（44:44:12）为流动相，在电喷雾离子化负离子模式下，以多反应监测方式（MRM）检测。银杏酸C13:0、C15:1、C17:1分别在0.2~200、2~200和4~200 μg·L-1范围内成良好线性关系，相关系数均大于0.999；在50、250和600 μg·kg-1加标水平下的平均加样回收率为70.8%~95.1%，相对标准偏差（RSD）为0.7%~8.6%；定量限分别为1、10、20 μg·kg-1。本方法可应用于复杂基质样品的银杏酸测定。

, correspAuthors=季申, authorNote=null, correspAuthorsNote=
* 季申, Tel:86-21-50798195, E-mail:
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Effect of GBE50 on experi mental arrhythmias[J]. China J Chin Mater Med (中国中药杂志), 2010, 35: 199-203., articleTitle=null, refAbstract=null), Reference(id=1218970836606833252, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1218551232780751086, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[2], rfOrder=1, authorNames=null, journalName=null, refType=null, unstructuredReference=Liu PP, Pan SH. Advance in study of ginkgolic acid contained in Ginkgo biloba preparations[J]. China J Chin Mater Med (中国中药杂志), 2012, 37: 274-277., articleTitle=null, refAbstract=null), Reference(id=1218970836724273774, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1218551232780751086, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[3], rfOrder=2, authorNames=null, journalName=null, refType=null, unstructuredReference=Wu XY, Yang LQ, Chen J. Determination of ginkgolic acids in Ginkgo biloba extract and its preparations by high performance liquid chromatography[J]. Acta Pharm Sin (药学学报), 2003, 38: 846-849., articleTitle=null, refAbstract=null), Reference(id=1218970836816548474, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1218551232780751086, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[4], rfOrder=3, authorNames=null, journalName=null, refType=null, unstructuredReference=United Sates Pharmacopeial Convention. United States Pharmacopoeia, 41 Revision, Volume 3[S]. Baltimore: United Book Press, 2018: 4460-4663., articleTitle=null, refAbstract=null), Reference(id=1218970836913017478, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1218551232780751086, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[5], rfOrder=4, authorNames=null, journalName=null, refType=null, unstructuredReference=Sun J, Li LM, Hu Q, et al. Determination of ginkgolic acids in the Ginkgo biloba extract and its preparations by ultra high performance liquid chromatography-triple quadrupole mass spectrometry[J]. Chin J Chromatogr (色谱), 2016, 34: 184- 188., articleTitle=null, refAbstract=null), Reference(id=1218970837034652305, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1218551232780751086, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[6], rfOrder=5, authorNames=null, journalName=null, refType=null, unstructuredReference=Chen J, Chen C, Ren H, et al. Determination of ginkgolic acids in the ginkgo leaf [J]. Chin J Mod Appl Pharm (中国现代应用药学), 2018, 35: 72-75., articleTitle=null, refAbstract=null), Reference(id=1218970837181452954, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1218551232780751086, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[7], rfOrder=6, authorNames=null, journalName=null, refType=null, unstructuredReference=Yao X, Xue P, Yu DH, et al. Determination of ginkgolic acids in ginkgo leaves extract from different manufacturers by UPLC-MS/MS[J]. 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Chemical structures of ginkgolic acids

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MRM chromatograms of ginkgolic acids

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Ginkgolic acid Precursor ion (m/z) Product ion (m/z) CE/V
C13:0 319.2 275.2* 25
106.1 49
C15:1 345.2 301.2* 21
119.0 49
C17:1 373.3 329.3* 29
106.0 49
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Monitoring ion pairs and CEs of ginkgolic acids. *Quantitative ion

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Ginkgolic acid Precursor ion (m/z) Product ion (m/z) CE/V
C13:0 319.2 275.2* 25
106.1 49
C15:1 345.2 301.2* 21
119.0 49
C17:1 373.3 329.3* 29
106.0 49
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Ginkgolic acid Spiked /mg·kg-1 Recovery /% RSD /% Correlation coefficient LOQ /μg·kg-1
C13:0 50 95.1 4.7 0.999 5 1
250 89.3 2.8
600 85.1 1.0
C15:1 50 83.9 7.6 0.999 6 10
250 82.1 8.6
600 78.7 3.8
C17:1 50 79.1 3.8 0.999 9 20
250 75.3 3.9
600 70.8 0.7
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Recoveries, precisions, correlation coefficients and LOQs of the three ginkgolic acids

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Ginkgolic acid Spiked /mg·kg-1 Recovery /% RSD /% Correlation coefficient LOQ /μg·kg-1
C13:0 50 95.1 4.7 0.999 5 1
250 89.3 2.8
600 85.1 1.0
C15:1 50 83.9 7.6 0.999 6 10
250 82.1 8.6
600 78.7 3.8
C17:1 50 79.1 3.8 0.999 9 20
250 75.3 3.9
600 70.8 0.7
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No. Content /μg per pill
1 0.06
2 0.10
3 0.07
4 0.04
5 0.03
6 0.02
7 0.06
8 0.03
9 0.03
10 0.02
11 0.02
12 0.03
13 0.03
14 0.04
15 0.04
16 0.04
17 0.03
18 0.03
19 0.03
20 0.03
21 0.02
22 0.02
23 0.02
24 0.02
25 0.02
26 0.02
27 0.02
28 0.02
29 0.02
30 0.02
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Detection results of the 30 Yinxing Tongzhi Dropping Pills. No. 1-10, 11-20 and 21-30 supplied by Manufacturer A, B and C, respectively

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No. Content /μg per pill
1 0.06
2 0.10
3 0.07
4 0.04
5 0.03
6 0.02
7 0.06
8 0.03
9 0.03
10 0.02
11 0.02
12 0.03
13 0.03
14 0.04
15 0.04
16 0.04
17 0.03
18 0.03
19 0.03
20 0.03
21 0.02
22 0.02
23 0.02
24 0.02
25 0.02
26 0.02
27 0.02
28 0.02
29 0.02
30 0.02
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混合型固相萃取-UHPLC/MS/MS法测定银杏酮酯滴丸中银杏酸含量
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孙健 1 , 张雪怡 2 , 李丽敏 1 , 胡青 1 , 诸艳蓉 1 , 毛秀红 1 , 季申 1, *
药学学报 | 研究论文 2018,53(9): 1532-1535
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药学学报 | 研究论文 2018, 53(9): 1532-1535
混合型固相萃取-UHPLC/MS/MS法测定银杏酮酯滴丸中银杏酸含量
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孙健1, 张雪怡2, 李丽敏1, 胡青1, 诸艳蓉1, 毛秀红1, 季申1, *
作者信息
  • 1.上海市食品药品检验所, 上海 201203
  • 2.上海上药杏灵科技药业股份有限公司, 上海 201703

通讯作者:

* 季申, Tel:86-21-50798195, E-mail:
Determination of ginkgolic acids in Yinxing Tongzhi Dropping Pills by mix-mode SPE-UHPLC/MS/MS
Jian SUN1, Xue-yi ZHANG2, Li-min LI1, Qing HU1, Yan-rong ZHU1, Xiu-hong MAO1, Shen JI1, *
Affiliations
  • 1. Shanghai Institute for Food and Drug Control, Shanghai 201203, China
  • 2. Shanghai Shangyao Xingling Technology Pharmaceutical Co., Ltd., Shanghai 201703, China
出版时间: 2018-09-12 doi: 10.16438/j.0513-4870.2018-0248
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摘要
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建立了超高效液相色谱串联三重四极杆质谱测定银杏酮酯滴丸中银杏酸的方法。采用混合型强阴离子反相吸附固相萃取净化样品，Waters Cortecs T3色谱柱（50 mm×2.1 mm，2.7 μm），以乙腈-甲醇-1%冰醋酸溶液（44:44:12）为流动相，在电喷雾离子化负离子模式下，以多反应监测方式（MRM）检测。银杏酸C13:0、C15:1、C17:1分别在0.2~200、2~200和4~200 μg·L-1范围内成良好线性关系，相关系数均大于0.999；在50、250和600 μg·kg-1加标水平下的平均加样回收率为70.8%~95.1%，相对标准偏差（RSD）为0.7%~8.6%；定量限分别为1、10、20 μg·kg-1。本方法可应用于复杂基质样品的银杏酸测定。

超高效液相色谱-三重四极杆质谱  /  混合型固相萃取  /  银杏酸  /  银杏酮酯滴丸

An analytical method was developed for determination of ginkgolic acids in Yinxing Tongzhi Dropping Pills by ultra high performance liquid chromatography-triple quadrupole mass spectrometry. The samples were purified by mix-mode anion exchange and reversed-phase SPE. A chromatographic column, Waters Cortecs T3 (50 mm×2.1 mm, 2.7 μm), was used with acetonitrile-methanol-1% acetic acid (44:44:12) as the mobile phase. The ginkgolic acids were detected by electrospray ionization mass spectrometry in negative mode with multiple reaction monitoring (MRM) mode. Ginkgolic acid C13:0, C15:1 and C17:1 possessed good linear correlation in the mass concentration range from 0.2 to 200 μg·L-1, 2 to 200 μg·L-1, 4 to 200 μg·L-1, respectively, with the correlation coefficients more than 0.999. The mean recoveries at spiked levels of 50, 250 and 600 μg·kg-1 were in the range of 70.8%-95.1%, and the RSDs were 0.7%-8.6%. The limits of quantification were 1, 10, 20 μg·kg-1, respectively. The method could be applied to the analysis of ginkgolic acids in complex matrix samples.

ultra high performance liquid chromatography-tandem mass spectrometry  /  mix-mode solidphase extraction  /  ginkgolic acid  /  Yinxing Tongzhi Dropping Pills
孙健, 张雪怡, 李丽敏, 胡青, 诸艳蓉, 毛秀红, 季申. 混合型固相萃取-UHPLC/MS/MS法测定银杏酮酯滴丸中银杏酸含量. 药学学报, 2018 , 53 (9) : 1532 -1535 . DOI: 10.16438/j.0513-4870.2018-0248
Jian SUN, Xue-yi ZHANG, Li-min LI, Qing HU, Yan-rong ZHU, Xiu-hong MAO, Shen JI. Determination of ginkgolic acids in Yinxing Tongzhi Dropping Pills by mix-mode SPE-UHPLC/MS/MS[J]. Acta Pharmaceutica Sinica, 2018 , 53 (9) : 1532 -1535 . DOI: 10.16438/j.0513-4870.2018-0248
正文
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银杏叶提取物为银杏科植物银杏的干燥叶经加工制成的提取物, 其主要功效为活血化瘀通络, 临床广泛用于冠心病、心绞痛等疾病。银杏酮酯是我国自主研发的新一代银杏叶提取物, 有效成分总黄酮和萜类内酯含量达到50%以上[1]。
银杏酸是银杏叶提取物中主要的毒性物质, 具有致敏性、胚胎毒性、细胞毒性及免疫毒性[2], 应当在提取生产工艺中有效去除。银杏酸主要包括银杏酸C13:0、C15:0、C15:1、C17:1、C17:2, 化学结构见图 1, 其中C13:0、C15:1、C17:1占总银杏酸的94%以上[3]。美国药典以该3种银杏酸含量之和作为总银杏酸含量[4]。作者研究组已针对银杏叶提取物及其片剂和胶囊剂开发了UHPLC/MS/MS法测定其中总银杏酸含量[5]。
银杏酮酯滴丸是指银杏酮酯原料与适宜的基质加热熔融混匀, 滴入冷凝介质中制成的球形制剂。所使用的基质主要为聚乙二醇6000、泊洛沙姆等高分子聚合物, 因其基质复杂, 无法使用银杏叶提取物测定方法[5]进行测定。文献[6, 7]同样多用甲醇直接超声提取后测定, 亦无法应用于复杂基质中。
因此, 复杂基质中银杏酸的测定存在方法空白, 必须采用专属性的前处理方法对复杂样品进行纯化后, 以三重四极杆质谱法测定其中银杏酸含量, 保障用药安全。
材料与方法
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仪器与试剂 Agilent 1290超高效液相色谱仪; Agilent 6495三重四极杆质谱; Waters Cortecs T3色谱柱(50 mm × 2.1 mm, 2.7 μm); Waters Oasis MAX固相萃取柱(规格60 mg/3 mL); 银杏酸C13:0对照品(中国食品药品检定研究院, 批号: 111690-200501)、银杏酸C15:1对照品(中国食品药品检定研究院, 批号: 111762-200601), 银杏酸C17:1对照品(同田生化公司, 纯度98.0%, 批号: 16040916);甲醇、乙腈、醋酸、甲酸均为色谱纯; 银杏酮酯滴丸(规格:每丸含银杏酮酯10 mg; 各生产企业提供)。
色谱和质谱条件 Waters Cortecs T3色谱柱(50 mm × 2.1 mm, 2.7 μm); 柱温为30 ℃, 流速为0.3 mL·min-1, 对照品溶液进样量1 μL, 供试品溶液进样量5 μL。流动相为乙腈-甲醇-1%冰醋酸溶液(44:44:12), 待测成分全部出峰后以乙腈-甲醇-1%冰醋酸溶液(49.5:49.5:1)充分清洗至少10倍柱体积。
电喷雾离子化(ESI)负离子模式; 干燥气(N2)流速15 L·min-1, 温度225 ℃; 雾化气(N2) 0.21 MPa; 鞘气(N2)流速11 L·min-1, 温度300 ℃; 毛细管电压3 000 V。采用多反应监测方式(MRM)检测, 监测离子、碰撞能量等参数见表 1。
对照品溶液制备方法 分别取银杏酸C13:0对照品、银杏酸C15:1对照品、银杏酸C17:1对照品适量, 精密称定, 加2%甲酸的乙腈溶液制成0.2~200、2~200、4~200μg·L-1的系列混合溶液, 作为对照品溶液。
供试品溶液制备方法 取本品200丸, 精密称定, 研细, 混匀, 取约2 g (约相当于银杏酮酯0.4 g), 精密称定, 置具塞锥形瓶中, 精密加入甲醇10 mL, 称定重量, 于40 ℃超声(功率180 W, 频率42 kHz) 30 min, 随时摇散, 放冷, 用甲醇补足减失的重量, 滤过, 精密取续滤液1 mL, 再精密加入水1 mL (可适当增加水量, 使单个银杏酸上样浓度低于60 μg·L-1), 混匀, 作为上样液。精密量取上样液1 mL, 加于Waters Oasis MAX固相萃取柱(规格60 mg/3 mL, 预先依次用甲醇1 mL和水1 mL活化)上, 依次用5%氨水和甲醇各2 mL清洗, 弃去洗液, 再用2%甲酸的乙腈溶液4 mL洗脱, 收集洗脱液并定容至5 mL, 滤过, 取续滤液, 即得。
方法学验证
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线性 取系列对照品溶液进样测定, 以各组分峰面积对质量浓度绘制曲线。
准确度 取银杏酮酯滴丸, 经检测银杏酸C13:0含量61.0 μg·kg-1、银杏酸C15:1含量195.5 μg·kg-1、银杏酸C17:1含量92.7 μg·kg-1, 分别添加低(50 μg·kg-1)、中(250 μg·kg-1)、高(600 μg·kg-1) 3个水平的对照品溶液, 每个水平做3个平行样, 共9份, 按上述供试品溶液制备方法和色谱质谱条件进行分析, 计算回收率和精密度。
稳定性 取供试品溶液, 分别于放置0、8、15 h时进样测定, 比较峰面积。
定量限 分析低水平添加溶液的信噪比, 以定量离子对计算定量限(信噪比为10)。
结果
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1 方法学验证
1.1 线性
银杏酸C13:0、C15:1和C17:1分别在0.2~200、2~200和4~200 μg·L-1内成良好线性关系, 相关系数均在0.999以上, 结果见表 2。
1.2 准确度
在50、250和600 μg·kg-1的加样水平下, 银杏酸C13:0的平均加样回收率为85.1%~95.1%, RSD为1.0%~4.7%;银杏酸C15:1的平均加样回收率为78.7%~83.9%, RSD为3.8%~8.6%;银杏酸C17:1的平均加样回收率为70.8%~79.1%, RSD为0.7%~3.9%。具体结果见表 2。
因银杏酸C17:1极性最小, 强保留于固相萃取柱上, 无法完全洗脱, 造成损失, 回收率较另2种银杏酸稍低。根据中国药典2015年版四部通则 <9101> , 样品中待测定成分含量为mg·kg-1级别时, 回收率要求为75%~120%, 重复性要求为不超过8%, 在基质复杂、组分含量低于0.01%及多成分等分析中, 回收率和精密度范围可适当放宽[8]。因此, 本次实验回收率和精密度符合要求。
1.3 稳定性
银杏酸C13:0、C15:1、C17:1峰面积RSD分别为4.2%、3.3%、3.5%, 在15 h内基本稳定。
1.4 定量限
银杏酸C13:0、C15:1、C17:1定量限分别为1、10、20 μg·kg-1 (表 2)。银杏酸C15:1、C17:1化学结构中脂肪碳链较C13:0更长, 且具双键, 基质中含有的同分异构体更多, 导致基线噪音较大, 因此定量限较银杏酸C13:0高。
原料银杏酮酯中总银杏酸限度为5 mg·kg-1, 制剂按处方量折算, 限度不得过1 000 μg·kg-1 (即每丸0.05 μg)。本方法的定量限可满足检测需求。
2 样品测定
本次研究测定了3家企业的共30批银杏酮酯滴丸的总银杏酸测定结果, 结果见表 3, 色谱图见图 2。限度按每丸0.05 μg计, 企业A的部分产品中总银杏酸含量超过限度。
现行银杏酮酯(原料)质量标准中总银杏酸测定方法为薄层扫描法, 前处理为正己烷索氏提取, 该方法提取效率低, 灵敏度低, 准确度差。企业A的部分制剂产品超过限度, 可能与原料质量未得到有效控制有关, 也可能与其工艺不稳定有关。因此, 有必要建立专属准确的原料及其制剂的总银杏酸测定方法, 从而有效控制产品质量, 保障用药安全。
讨论
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参照银杏叶提取物测定方法[5], 采用甲醇超声提取银杏酸。实验发现, 滴丸辅料特殊, 室温超声20 min时, 仍有部分样品结块。当采用40 ℃、超声30 min提取时, 样品能够全部溶解。
样品提取后采用: ①提取液直接进样测定; ②减缓流动相梯度以尽可能分离基质与待测物; ③反相固相萃取(Waters oasis HLB)净化等3种方式处理并进样测定, 但回收率均较差, 基质抑制或增强严重。因此, 使用混合型强阴离子交换反相吸附填料固相萃取(Waters oasis MAX)净化, 该固相萃取方法对弱酸性化合物具高度专属性, 回收率得到较大改善。但精密度较差, 具体分析数据为高浓度加样水平回收率较差, 原因为固相萃取柱规格较小, 高浓度样品过载所致, 故若含量过高时, 上样前需稀释。因各品牌的柱填料有细微差别, 使用其他品牌时清洗及洗脱溶剂的类别和酸度均应作相应调整。
流动相条件参照银杏叶提取物测定方法[5], 以甲醇-1%冰醋酸溶液(90:10)为流动相。但在大批次进样时, 发现部分样品重复性较差, 推测个别企业样品中存在部分保留极强残留于色谱柱中的成分, 与后续进样的供试品溶液共馏出产生基质增强效应, 以甲醇-1%冰醋酸溶液(99:1)也无法彻底洗脱。尝试将有机相换为洗脱能力更强的乙腈, 但峰形太差, 拖尾严重。故有机相采用甲醇+乙腈(1:1), 方能兼顾洗脱能力和峰形。因乙腈洗脱能力更强, 比例微调, 最终定为以乙腈-甲醇-1%冰醋酸溶液(44:44:12)为流动相, 待测成分全部出峰后以乙腈-甲醇-1%冰醋酸溶液(49.5:49.5:1)充分清洗至少10倍柱体积。
质谱条件同银杏叶提取物测定方法[5]。综上, 本研究建立了混合型固相萃取-UHPLC/ MS/MS法测定银杏酮酯滴丸中银杏酸, 方法专属, 解决了复杂基质中银杏酸测定的难题, 灵敏准确, 能够满足痕量银杏酸检测的需求。本方法可为银杏叶相关药品或保健食品中总银杏酸测定提供借鉴意义。
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doi: 10.16438/j.0513-4870.2018-0248
  • 接收时间：2018-03-21
  • 首发时间：2026-01-15
  • 出版时间：2018-09-12
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  • 收稿日期：2018-03-21
  • 修回日期：2018-05-04
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上海市科委技术平台专项(14DZ2294000)
作者信息
    1.上海市食品药品检验所, 上海 201203
    2.上海上药杏灵科技药业股份有限公司, 上海 201703

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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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