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Article(id=1241779364476551508, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1241779355555266850, articleNumber=null, orderNo=null, doi=10.16155/j.0254-1793.2024.05.12, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1686412800000, receivedDateStr=2023-06-11, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773992871636, onlineDateStr=2026-03-20, pubDate=1717084800000, pubDateStr=2024-05-31, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773992871636, onlineIssueDateStr=2026-03-20, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773992871636, creator=13701087609, updateTime=1773992871636, updator=13701087609, issue=Issue{id=1241779355555266850, tenantId=1146029695717560320, journalId=1205117023404326918, year='2024', volume='44', issue='5', pageStart='737', pageEnd='920', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773992869509, creator=13701087609, updateTime=1773992925624, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241779590985749489, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1241779355555266850, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241779590985749490, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1241779355555266850, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=841, endPage=850, ext={EN=ArticleExt(id=1241779364891787619, articleId=1241779364476551508, tenantId=1146029695717560320, journalId=1205117023404326918, language=EN, title=Study on pharmacokinetics and bioavailability of four lignans in Acanthopanacis Senticosi Radix et Rhizoma Seu Caulis*, columnId=1239184757519602223, journalTitle=Chinese Journal of Pharmaceutical Analysis, columnName=Metabolism Analysis, runingTitle=null, highlight=null, articleAbstract=
Objective:

To establish a ultra-high performance liquid chromatography-mass spectrum in series method for the quantification of 7-hydroxycoumarin，fraxetin，isofraxidin and scopoletin in the aqueous extract of Acanthopanacis Senticosi Radix et Rhizoma Seu Caulis in rat plasma，and to evaluate the pharmacokinetic behavior and bioavailability in rats.

Methods:

The chromatography was performed on Thermo Scientific Hypersil GOLD aQ（100 mm×2.1 mm，1.9 μm）column with 0.1% aqueous formic acid -0.1% acetonitrile formic acid solution (82：18) as the mobile phase at the flow rate of 0.30 mL·min-1，and column temperature of 40 ℃. Mass spectrometry positive ion mode scan was used，and sample size was 5 μL. Healthy SD rats were selected for a single gavage of 10 mL·kg-1 of Acanthopanacis Senticosi Radix et Rhizoma Seu Caulis water extract (equivalent to the dose of 1 g·kg-1 of the original drug). Plasma concentration of the substances was determined at different time intervals after administration，and the pharmacokinetic parameters were calculated using DAS software by non-atrioventricular model fitting.

Results:

The methodological results showed that 7-hydroxycoumarin (r=0.999 4)，fraxetin (r=0.998 9)，isofraxidin (r=0.999 3) and scopoletin (r=0.998 4) had good linearity in the range of 0.05-55 μg·mL-1，and RSDs of precision of the four substances were all less than 15%. The recovery was 85%-115%. The absolute bioavailability ranged from 59% to 78%，and the relative bioavailability ranged from 80% to 87%. The extraction recovery，matrix effect and stability met the relevant requirements.

Conclusions:

After a single gavage of the aqueous extract of Acanthopanacis Senticosi Radix et Rhizoma Seu Caulis in rats，the four substances to be tested are absorbed and eliminated by rats. The method validation results are in line with the guiding principles of biological sample analysis methods，and can be applied to evaluate the pharmacokinetic behavior and bioavailability of the aqueous extract of Acanthopanacis Senticosi Radix et Rhizoma Seu Caulis in rats.

, correspAuthors=Chang-hai SUN, 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=Jin-yu ZHANG, Yan-cui LI, Chang-hai SUN), CN=ArticleExt(id=1241779368477917638, articleId=1241779364476551508, tenantId=1146029695717560320, journalId=1205117023404326918, language=CN, title=刺五加中4个木脂素成分的药代动力学及生物利用度研究*, columnId=1239184757708345914, journalTitle=药物分析杂志, columnName=代谢分析, runingTitle=null, highlight=null, articleAbstract=
目的：

建立超高效液相色谱-串联质谱（UPLC-MS/MS）方法测定大鼠血浆中刺五加提取液中7-羟基香豆素、秦皮素、异嗪皮啶、东莨菪内酯4个成分的含量，评价大鼠体内的药代动力学行为和生物利用度。

方法：

采用Thermo Scientific Hypersil GOLD aQ色谱柱（100 mm×2.1 mm，1.9 μm），以0.1%甲酸-水（A）和0.1%甲酸-乙腈（B）（82：18）为流动相，流速0.30 mL·min-1，柱温40 ℃；质谱正离子模式扫描，进样量5 μL；选取健康SD大鼠，单次灌胃10 mL·kg-1（相当于原药1 g·kg-1剂量）的刺五加提取液，测定给药后不同时间间隔的待测物质血浆浓度，利用DAS软件，经非房室模型拟合计算药代动力学参数。

结果：

7-羟基香豆素(r=0.999 4)、秦皮素(r=0.998 9)、异嗪皮啶(r=0.999 3)、东莨菪内酯(r=0.998 4)质量浓度在0.05~55 μg·mL-1范围内线性关系良好，精密度RSD均<15%，回收率均在85%~115%。绝对生物利用度均在59%~78%，相对生物利用度均在80%~87%。提取回收率、基质效应和稳定性均满足相关要求。

结论：

大鼠单次灌胃刺五加提取液后，4个待测物质均被大鼠吸收和消除，方法验证结果符合生物样本分析方法指导原则，可用于评价刺五加提取液在大鼠体内的药代动力学行为和生物利用度。

, correspAuthors=孙长海, authorNote=null, correspAuthorsNote=
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Tel：（0454）15765369662；E-mail：

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Chin J Pharm Anal，2006，26(6)：741, articleTitle=RP-HPLC determination of pharmacokinetics of eleutherococcuss eleutheroside E and eleutheroside B in rats plasma and tissues, refAbstract=null)], funds=[Fund(id=1241779380935000963, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, awardId=JDXKTD-2019005, language=CN, fundingSource=*黑龙江省佳木斯大学北药与功能食品(JDXKTD-2019005), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1241779368784101842, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, xref=null, ext=[AuthorCompanyExt(id=1241779368788296147, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, companyId=1241779368784101842, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=College of Pharmacy, Jiamusi University, Jiamusi 154007, China), AuthorCompanyExt(id=1241779368796684756, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, companyId=1241779368784101842, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=佳木斯大学药学院，佳木斯 154007)])], figs=[ArticleFig(id=1241779373905347256, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Fig.1, caption=UPLC-ESI-Q-Orbitrap ion chromatograms of blank plasma (A)，plasma mixed reference substance(B)，plasma sample（C）, figureFileSmall=1CGlmBxVxtDhvSnM2GNjOg==, figureFileBig=ZraCiYxJX2ppY/svWTmIZw==, tableContent=null), ArticleFig(id=1241779374035370689, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=图1, caption=空白血浆（A）、对照品血浆（B）、血浆样品（C）UPLC-LC-MS/MS提取离子色谱图

1. 7-羟基香豆素（7-hydroxycoumarin）　2.秦皮素（fraxetin）　3.牡荆素（isofraxidin）　4.异嗪皮啶（isofraxidin）　5.东莨菪内酯（scopoletin）

, figureFileSmall=1CGlmBxVxtDhvSnM2GNjOg==, figureFileBig=ZraCiYxJX2ppY/svWTmIZw==, tableContent=null), ArticleFig(id=1241779374308000468, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Fig.2, caption=The drug time curves of Acanthopanacis Senticosi Radix et Rhizoma Seu Caulis extract ig 7-hydroxycoumarin (A)，fraxetin (B)，isofraxidin (C)，and scopoletin (D), figureFileSmall=fnQjPZXb6j30EsrJHkCfeg==, figureFileBig=J+PWfDOSUhbkljd0pt7jXA==, tableContent=null), ArticleFig(id=1241779374429635290, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=图2, caption=刺五加提取液ig 7-羟基香豆素（A）、秦皮素（B）、异嗪皮啶（C）、东莨菪内酯（D）的药时曲线图, figureFileSmall=fnQjPZXb6j30EsrJHkCfeg==, figureFileBig=J+PWfDOSUhbkljd0pt7jXA==, tableContent=null), ArticleFig(id=1241779374534492898, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Fig.3, caption=Cleavage mechanism of 7-hydroxycoumarin, figureFileSmall=TlEhmVmSOLZc59hA3ynduQ==, figureFileBig=ny2NEw6rkuHgK2ge5H6UPQ==, tableContent=null), ArticleFig(id=1241779376077996778, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=图3, caption=7-羟基香豆素裂解机理, figureFileSmall=TlEhmVmSOLZc59hA3ynduQ==, figureFileBig=ny2NEw6rkuHgK2ge5H6UPQ==, tableContent=null), ArticleFig(id=1241779376212214513, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Fig.4, caption=Cracking mechanism of fraxetin, figureFileSmall=sRyxoX8chDwq4WsszFx2ng==, figureFileBig=wiAcnZk2pSvCYPAgCifBmQ==, tableContent=null), ArticleFig(id=1241779376359015162, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=图4, caption=秦皮素裂解机理, figureFileSmall=sRyxoX8chDwq4WsszFx2ng==, figureFileBig=wiAcnZk2pSvCYPAgCifBmQ==, tableContent=null), ArticleFig(id=1241779376468067073, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Fig.5, caption=Cleavage mechanism of isoazinpyridine, figureFileSmall=cTM7KXsufHBusxiYWEhHIg==, figureFileBig=Byvtfz5EAZIwnm0K7jI52Q==, tableContent=null), ArticleFig(id=1241779376602284809, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=图5, caption=异嗪皮啶裂解机理, figureFileSmall=cTM7KXsufHBusxiYWEhHIg==, figureFileBig=Byvtfz5EAZIwnm0K7jI52Q==, tableContent=null), ArticleFig(id=1241779376686170895, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Fig.6, caption=Cracking mechanism of scopolide, figureFileSmall=tHtNtQgtoow8S9xlaBWfdw==, figureFileBig=guDl7GrlPcJk6X4F1uJHNQ==, tableContent=null), ArticleFig(id=1241779376786834196, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=图6, caption=东莨菪内酯裂解机理, figureFileSmall=tHtNtQgtoow8S9xlaBWfdw==, figureFileBig=guDl7GrlPcJk6X4F1uJHNQ==, tableContent=null), ArticleFig(id=1241779376895886107, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Tab.1, caption=

Stability results

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		静置稳定性（static stability）冻融稳定性（freezing and melting stability）
mean±SDRSD/%mean±SDRSD/%
7-羟基香豆素（7-hydroxycoumarin）2 449 511±81 8143.32 521 586±130 2145.2
秦皮素（fraxetin）2 264 221±78 7953.52 341 584±115 6824.9
异嗪皮啶（isofraxidin）2 311 022±93 5964.12 332 574±159 8756.9
东莨菪内酯（scopoletin）1 107 610±54 1624.91 102 548±70 2156.4
), ArticleFig(id=1241779377009132322, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=表1, caption=

稳定性结果

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		静置稳定性（static stability）冻融稳定性（freezing and melting stability）
mean±SDRSD/%mean±SDRSD/%
7-羟基香豆素（7-hydroxycoumarin）2 449 511±81 8143.32 521 586±130 2145.2
秦皮素（fraxetin）2 264 221±78 7953.52 341 584±115 6824.9
异嗪皮啶（isofraxidin）2 311 022±93 5964.12 332 574±159 8756.9
东莨菪内酯（scopoletin）1 107 610±54 1624.91 102 548±70 2156.4
), ArticleFig(id=1241779377109795623, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Tab.2, caption=

Results of matrix effects

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		低浓度（low concentration）中浓度（medium concentration）高浓度（high concentration）
基质效应
（matrix effect）/%		RSD/%基质效应
（matrix effect）/%		RSD/%基质效应
（matrix effect）/%		RSD/%
7-羟基香豆素（7-hydroxycoumarin）99.11.698.60.92102.51.9
秦皮素（fraxetin）98.31.497.91.9101.31.99
异嗪皮啶（isofraxidin）98.21.1102.31.499.11.4
东莨菪内酯（scopoletin）97.91.699.51.2101.22.0
), ArticleFig(id=1241779377210458924, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=表2, caption=

基质效应结果(n=6)

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		低浓度（low concentration）中浓度（medium concentration）高浓度（high concentration）
基质效应
（matrix effect）/%		RSD/%基质效应
（matrix effect）/%		RSD/%基质效应
（matrix effect）/%		RSD/%
7-羟基香豆素（7-hydroxycoumarin）99.11.698.60.92102.51.9
秦皮素（fraxetin）98.31.497.91.9101.31.99
异嗪皮啶（isofraxidin）98.21.1102.31.499.11.4
东莨菪内酯（scopoletin）97.91.699.51.2101.22.0
), ArticleFig(id=1241779377315316529, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Tab.3, caption=

Results of in-batch precision

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		低浓度（low concentration）中浓度（medium concentration）高浓度（high concentration）
峰面积
（peak area）		RSD/%峰面积
（peak area）		RSD/%峰面积
（peak area）		RSD/%
7-羟基香豆素（7-hydroxycoumarin）15 563±8965.830 573 791±1 002 8203.3315 949 990±12 006 0703.8
秦皮素（fraxetin）46 995±2 4815.36 230 974±214 3463.470 542 675±1 664 8072.4
异嗪皮啶（isofraxidin）11 169±6315.71 841 688±55 4353.014 494 448±478 3173.3
东莨菪内酯（scopoletin）39 015±1 7674.56 346 375±152 9482.470 416 652±1 654 7912.4
), ArticleFig(id=1241779377474700089, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=表3, caption=

批内精密度结果（n=6）

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		低浓度（low concentration）中浓度（medium concentration）高浓度（high concentration）
峰面积
（peak area）		RSD/%峰面积
（peak area）		RSD/%峰面积
（peak area）		RSD/%
7-羟基香豆素（7-hydroxycoumarin）15 563±8965.830 573 791±1 002 8203.3315 949 990±12 006 0703.8
秦皮素（fraxetin）46 995±2 4815.36 230 974±214 3463.470 542 675±1 664 8072.4
异嗪皮啶（isofraxidin）11 169±6315.71 841 688±55 4353.014 494 448±478 3173.3
东莨菪内酯（scopoletin）39 015±1 7674.56 346 375±152 9482.470 416 652±1 654 7912.4
), ArticleFig(id=1241779377600529216, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Tab.4, caption=

Inter-lot precision results

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		低浓度（low concentration）中浓度（medium concentration）高浓度（high concentration）
峰面积
（peak area）		RSD/%峰面积
（peak area）		RSD/%峰面积
（peak area）		RSD/%
7-羟基香豆素（7-hydroxycoumarin）15 108±7965.331 258 671±1 012 5873.2312 357 848±11 898 5453.8
秦皮素（fraxetin）43 525±2 2455.26 055 874±223 4843.771 200 548±1 598 7422.2
异嗪皮啶（isofraxidin）10 859±6115.61 359 888±53 2483.912 345 865±487 1253.9
东莨菪内酯（scopoletin）37 585±1 3583.66 235 789±151 2382.471 204 489±1 531 5872.2
), ArticleFig(id=1241779377747329860, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=表4, caption=

批间精密度结果（n=6）

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		低浓度（low concentration）中浓度（medium concentration）高浓度（high concentration）
峰面积
（peak area）		RSD/%峰面积
（peak area）		RSD/%峰面积
（peak area）		RSD/%
7-羟基香豆素（7-hydroxycoumarin）15 108±7965.331 258 671±1 012 5873.2312 357 848±11 898 5453.8
秦皮素（fraxetin）43 525±2 2455.26 055 874±223 4843.771 200 548±1 598 7422.2
异嗪皮啶（isofraxidin）10 859±6115.61 359 888±53 2483.912 345 865±487 1253.9
东莨菪内酯（scopoletin）37 585±1 3583.66 235 789±151 2382.471 204 489±1 531 5872.2
), ArticleFig(id=1241779377931879242, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Tab.5, caption=

Results of linear relation

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		回归方程
（regression equation）		r线性范围
（linear range）/（μg·mL-1）		LOD/ngLOQ/ngRSD/%
7-羟基香豆素（7-hydroxycoumarin）Y=0.029 1X-0.162 50.999 40.050 00~51.250.198 00.660 22.8
秦皮素（fraxetin）Y=0.006 5X-0.061 30.998 90.054 10~55.500.333 01.1103.3
异嗪皮啶（isofraxidin）Y=0.001 3X+0.022 20.999 30.050 00~51.250.486 01.6202.5
东莨菪内酯（scopoletin）Y=0.006 5X-0.074 20.998 40.051 50~52.750.693 02.3102.7
), ArticleFig(id=1241779378032542542, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=表5, caption=

线性关系结果

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		回归方程
（regression equation）		r线性范围
（linear range）/（μg·mL-1）		LOD/ngLOQ/ngRSD/%
7-羟基香豆素（7-hydroxycoumarin）Y=0.029 1X-0.162 50.999 40.050 00~51.250.198 00.660 22.8
秦皮素（fraxetin）Y=0.006 5X-0.061 30.998 90.054 10~55.500.333 01.1103.3
异嗪皮啶（isofraxidin）Y=0.001 3X+0.022 20.999 30.050 00~51.250.486 01.6202.5
东莨菪内酯（scopoletin）Y=0.006 5X-0.074 20.998 40.051 50~52.750.693 02.3102.7
), ArticleFig(id=1241779378133205843, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Tab.6, caption=

Results of recovery rate

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		本底量
（the background quantity)/μg		加入量
（added）/μg		实测值
（measured value）/μg mean±SD		回收率
（recovery）/%		RSD/%
7-羟基香豆素（7-hydroxycoumarin）8.446.75215.52±0.21104.81.4
8.4416.61±0.2596.81.5
10.1319.12±0.24105.41.2
秦皮素（fraxetin）5.2604.2089.11±0.0991.40.97
5.2610.23±0.0994.40.85
6.31211.49±0.1398.71.2
异嗪皮啶（isofraxidin）21.8717.537.46±0.5189.11.4
21.8742.78±0.5195.61.2
26.2448.66±0.51102.11.0
东莨菪内酯（scopoletin）2.5702.0564.490±0.0493.20.94
2.575.230±0.08103.61.4
3.0845.830±0.08105.81.4
), ArticleFig(id=1241779378410029913, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=表6, caption=

回收率结果（n=6）

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		本底量
（the background quantity)/μg		加入量
（added）/μg		实测值
（measured value）/μg mean±SD		回收率
（recovery）/%		RSD/%
7-羟基香豆素（7-hydroxycoumarin）8.446.75215.52±0.21104.81.4
8.4416.61±0.2596.81.5
10.1319.12±0.24105.41.2
秦皮素（fraxetin）5.2604.2089.11±0.0991.40.97
5.2610.23±0.0994.40.85
6.31211.49±0.1398.71.2
异嗪皮啶（isofraxidin）21.8717.537.46±0.5189.11.4
21.8742.78±0.5195.61.2
26.2448.66±0.51102.11.0
东莨菪内酯（scopoletin）2.5702.0564.490±0.0493.20.94
2.575.230±0.08103.61.4
3.0845.830±0.08105.81.4
), ArticleFig(id=1241779378544247648, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Tab.7, caption=

Results of pharmacokinetic parameters

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		AUC（0-t）/（mg·h·L-1）AUC（0-∞）/（mg·h·L-1）Tmax/hCmax/（mg·L-1）t1/2/h（CL/F）/（L·kg-1）（V1/F）/（L·h-1·kg-1）
7-羟基香豆素（7-hydroxycoumarin）17.05±0.2317.05±0.140.500 0±0.0110.02±0.141.801±0.030.110 1±0.000.287 2±0.01
秦皮素（fraxetin）43.92±0.6550.58±0.581.500±0.014.882±0.067.801±0.110.063 2±0.000.714 1±0.02
异嗪皮啶（isofraxidin）26.86±0.3326.90±0.372.000±0.035.757±0.062.583±0.030.259 4±0.010.967±0.02
东莨菪内酯（scopoletin）54.21±0.5357.43±0.681.000±0.0111.61±0.116.140±0.050.055 3±0.000.488 4±0.01
), ArticleFig(id=1241779378682659685, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=表7, caption=

药代动力学参数结果

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		AUC（0-t）/（mg·h·L-1）AUC（0-∞）/（mg·h·L-1）Tmax/hCmax/（mg·L-1）t1/2/h（CL/F）/（L·kg-1）（V1/F）/（L·h-1·kg-1）
7-羟基香豆素（7-hydroxycoumarin）17.05±0.2317.05±0.140.500 0±0.0110.02±0.141.801±0.030.110 1±0.000.287 2±0.01
秦皮素（fraxetin）43.92±0.6550.58±0.581.500±0.014.882±0.067.801±0.110.063 2±0.000.714 1±0.02
异嗪皮啶（isofraxidin）26.86±0.3326.90±0.372.000±0.035.757±0.062.583±0.030.259 4±0.010.967±0.02
东莨菪内酯（scopoletin）54.21±0.5357.43±0.681.000±0.0111.61±0.116.140±0.050.055 3±0.000.488 4±0.01
), ArticleFig(id=1241779378800100201, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Tab.8, caption=

Results of individual differences

, figureFileSmall=null, figureFileBig=null, tableContent=
大鼠编号
（rat number）		P
独立样本结果
（independent sample result）		单样本结果
（independent sample result）
10.330.25
20.280.35
30.340.21
40.240.39
50.310.21
60.180.22
), ArticleFig(id=1241779378925929328, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=表8, caption=

个体差异性结果（n=6）

, figureFileSmall=null, figureFileBig=null, tableContent=
大鼠编号
（rat number）		P
独立样本结果
（independent sample result）		单样本结果
（independent sample result）
10.330.25
20.280.35
30.340.21
40.240.39
50.310.21
60.180.22
), ArticleFig(id=1241779379030786931, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Tab.9, caption=

Results of AUC

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		提取液ig组
（extract ig group）		提取液iv组
（extract iv group）		注射液ig组
（injection ig group）
7-羟基香豆素（7-hydroxycoumarin）19.24±0.4330.26±0.5622.64±0.34
秦皮素（fraxetin）42.81±0.5155.41±1.3750.89±0.71
异嗪皮啶（isofraxidin）26.73±0.4040.26±0.5531.57±0.55
东莨菪内酯（scopoletin）54.21±1.2769.80±1.2965.42±1.04
), ArticleFig(id=1241779380603650936, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=表9, caption=

AUC(mg·h·L-1)结果

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		提取液ig组
（extract ig group）		提取液iv组
（extract iv group）		注射液ig组
（injection ig group）
7-羟基香豆素（7-hydroxycoumarin）19.24±0.4330.26±0.5622.64±0.34
秦皮素（fraxetin）42.81±0.5155.41±1.3750.89±0.71
异嗪皮啶（isofraxidin）26.73±0.4040.26±0.5531.57±0.55
东莨菪内酯（scopoletin）54.21±1.2769.80±1.2965.42±1.04
), ArticleFig(id=1241779380670759803, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=EN, label=Tab.10, caption=

Results of bioavailability

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		相对生物利用度
（relative bioavailability）/%		绝对生物利用度
（absolute bioavailability）/%
7-羟基香豆素（7-hydroxycoumarin）84.963.58
秦皮素（fraxetin）84.177.26
异嗪皮啶（isofraxidin）84.666.39
东莨菪内酯（scopoletin）82.877.66
), ArticleFig(id=1241779380784006015, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1241779364476551508, language=CN, label=表10, caption=

生物利用度结果

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
（component）		相对生物利用度
（relative bioavailability）/%		绝对生物利用度
（absolute bioavailability）/%
7-羟基香豆素（7-hydroxycoumarin）84.963.58
秦皮素（fraxetin）84.177.26
异嗪皮啶（isofraxidin）84.666.39
东莨菪内酯（scopoletin）82.877.66
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刺五加中4个木脂素成分的药代动力学及生物利用度研究*
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张锦钰 , 李艳翠 , 孙长海 **
药物分析杂志 | 代谢分析 2024,44(5): 841-850
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药物分析杂志 | 代谢分析 2024, 44(5): 841-850
刺五加中4个木脂素成分的药代动力学及生物利用度研究*
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张锦钰 , 李艳翠, 孙长海**
作者信息
  • 佳木斯大学药学院，佳木斯 154007

    • Tel：（0454）15765369662；E-mail：

通讯作者:

** Tel：（0454）15904544250；E-mail：
Study on pharmacokinetics and bioavailability of four lignans in Acanthopanacis Senticosi Radix et Rhizoma Seu Caulis*
Jin-yu ZHANG , Yan-cui LI, Chang-hai SUN**
Affiliations
  • College of Pharmacy, Jiamusi University, Jiamusi 154007, China
出版时间: 2024-05-31 doi: 10.16155/j.0254-1793.2024.05.12
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摘要
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目的：

建立超高效液相色谱-串联质谱（UPLC-MS/MS）方法测定大鼠血浆中刺五加提取液中7-羟基香豆素、秦皮素、异嗪皮啶、东莨菪内酯4个成分的含量，评价大鼠体内的药代动力学行为和生物利用度。

方法：

采用Thermo Scientific Hypersil GOLD aQ色谱柱（100 mm×2.1 mm，1.9 μm），以0.1%甲酸-水（A）和0.1%甲酸-乙腈（B）（82：18）为流动相，流速0.30 mL·min-1，柱温40 ℃；质谱正离子模式扫描，进样量5 μL；选取健康SD大鼠，单次灌胃10 mL·kg-1（相当于原药1 g·kg-1剂量）的刺五加提取液，测定给药后不同时间间隔的待测物质血浆浓度，利用DAS软件，经非房室模型拟合计算药代动力学参数。

结果：

7-羟基香豆素(r=0.999 4)、秦皮素(r=0.998 9)、异嗪皮啶(r=0.999 3)、东莨菪内酯(r=0.998 4)质量浓度在0.05~55 μg·mL-1范围内线性关系良好，精密度RSD均<15%，回收率均在85%~115%。绝对生物利用度均在59%~78%，相对生物利用度均在80%~87%。提取回收率、基质效应和稳定性均满足相关要求。

结论：

大鼠单次灌胃刺五加提取液后，4个待测物质均被大鼠吸收和消除，方法验证结果符合生物样本分析方法指导原则，可用于评价刺五加提取液在大鼠体内的药代动力学行为和生物利用度。

刺五加  /  药物代谢动力学  /  生物利用度  /  7 -羟基香豆素  /  秦皮素  /  异嗪皮啶  /  东莨菪内酯  /  统计矩量法  /  超高效液相色谱-串联质谱
Objective:

To establish a ultra-high performance liquid chromatography-mass spectrum in series method for the quantification of 7-hydroxycoumarin，fraxetin，isofraxidin and scopoletin in the aqueous extract of Acanthopanacis Senticosi Radix et Rhizoma Seu Caulis in rat plasma，and to evaluate the pharmacokinetic behavior and bioavailability in rats.

Methods:

The chromatography was performed on Thermo Scientific Hypersil GOLD aQ（100 mm×2.1 mm，1.9 μm）column with 0.1% aqueous formic acid -0.1% acetonitrile formic acid solution (82：18) as the mobile phase at the flow rate of 0.30 mL·min-1，and column temperature of 40 ℃. Mass spectrometry positive ion mode scan was used，and sample size was 5 μL. Healthy SD rats were selected for a single gavage of 10 mL·kg-1 of Acanthopanacis Senticosi Radix et Rhizoma Seu Caulis water extract (equivalent to the dose of 1 g·kg-1 of the original drug). Plasma concentration of the substances was determined at different time intervals after administration，and the pharmacokinetic parameters were calculated using DAS software by non-atrioventricular model fitting.

Results:

The methodological results showed that 7-hydroxycoumarin (r=0.999 4)，fraxetin (r=0.998 9)，isofraxidin (r=0.999 3) and scopoletin (r=0.998 4) had good linearity in the range of 0.05-55 μg·mL-1，and RSDs of precision of the four substances were all less than 15%. The recovery was 85%-115%. The absolute bioavailability ranged from 59% to 78%，and the relative bioavailability ranged from 80% to 87%. The extraction recovery，matrix effect and stability met the relevant requirements.

Conclusions:

After a single gavage of the aqueous extract of Acanthopanacis Senticosi Radix et Rhizoma Seu Caulis in rats，the four substances to be tested are absorbed and eliminated by rats. The method validation results are in line with the guiding principles of biological sample analysis methods，and can be applied to evaluate the pharmacokinetic behavior and bioavailability of the aqueous extract of Acanthopanacis Senticosi Radix et Rhizoma Seu Caulis in rats.

Acanthopanacis Senticosi Radix et Rhizoma Seu Caulis  /  pharmacokinetics  /  bioavailability  /  7-hydroxycoumarin  /  fraxetin  /  isofraxidin  /  scopoletin  /  statistical method of moments  /  UPLC-MS/MS
张锦钰, 李艳翠, 孙长海. 刺五加中4个木脂素成分的药代动力学及生物利用度研究*. 药物分析杂志, 2024 , 44 (5) : 841 -850 . DOI: 10.16155/j.0254-1793.2024.05.12
Jin-yu ZHANG, Yan-cui LI, Chang-hai SUN. Study on pharmacokinetics and bioavailability of four lignans in Acanthopanacis Senticosi Radix et Rhizoma Seu Caulis*[J]. Chinese Journal of Pharmaceutical Analysis, 2024 , 44 (5) : 841 -850 . DOI: 10.16155/j.0254-1793.2024.05.12
正文
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刺五加为五加科植物刺五加[Acanthopanax seuticosus (Rupr.et Maxim.) Harms]的干燥根和根茎或茎，生长地区广泛[1-3]。临床证明，刺五加具有扩张人体大脑血管[4]，镇静安神[5]，增强机体抗疲劳能力[6]，降低血小板凝结[7-9]，促进蛋白质合成，降低组织耗氧量，扩张血管从而降低脑血栓形成等作用[10]，可用于冠心病、脑梗死及脑梗死后抑郁、老年功能性失眠和更年期综合征等疾病的治疗[11]。
实验表明，刺五加的上百个成分中，至少有40个成分可以被吸收，有着广阔的研究前景。但目前对刺五加的研究主要集中在刺五加苷E、紫丁香苷、金丝桃苷、绿原酸的大鼠体内药代动力学[12]，对于其他化学成分研究较少，例如具有抗肿瘤、降血压等药理作用的木脂素类化合物的药代动力学研究，至今还未有相关报道[13-15]。本文对刺五加中7-羟基香豆素、秦皮素、异嗪皮啶、东莨菪内酯4个木脂素成分的药代动力学及生物利用度进行研究，以期为后续刺五加的临床使用提供参考。
1　仪器与试药
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1.1　仪器
Dionex Ultimate 3000 RSLC高效液相色谱仪、Thermo Scientific Q Exactive Series质谱仪，Thermo Fisher Scientific公司；TGL-16G台式离心机，无锡莱浦仪器设备有限公司；HESI-II型离子源，Thermo Fisher Scientific公司；KQ-250型医用数控超声波清洗机，昆山超声仪器有限公司；Sartorius BP211D十万分之一电子分析天平，赛多利斯股份有限公司；FW100高速粉碎机，天津泰斯特公司；Master Touch-S 15超纯水系统，上海HHitech公司。
1.2　试药
甲醇、甲酸、乙腈（Thermo Fisher Scientific公司），水为实验制超纯水。对照品秦皮素（批号MUST-20103019，纯度≥99%）、异嗪皮啶（批号MUST-19041707，纯度≥98%）、东莨菪内酯（批号MUST-21032415，纯度≥99%）、7-羟基香豆素（批号DSTDQ006601，纯度≥98%），均购自中国食品药品检定研究院；牡荆素对照品（内标，批号20121112，纯度≥99%），购自天津一方科技有限公司。刺五加根茎采自佳木斯市四丰山野生植物区，经佳木斯大学药学院宗希明高级实验员鉴定。刺五加注射液来自佳木斯市多多药业有限公司，对应化合物质量浓度为7-羟基香豆素0.188 2 mg·mL-1，秦皮素0.321 3 mg·mL-1，异嗪皮啶0.693 8 mg·mL-1，东莨菪内酯0.316 2 mg·mL-1。
SPF级雄性SD大鼠6只，体质量180~220 g，长春市亿斯实验动物技术有限公司，许可证号SCXK（吉）-2021-0002。
2　方法与结果
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2.1　刺五加提取液的制备
采集刺五加样品，置于烘箱中，80 ℃下干燥1 h，粉碎后过80目筛，随后在80 ℃的烘箱中烘烤2 h，干燥至恒重。将所得样品以料液比1：10的比例加入超纯水，置于锥形瓶中浸泡12 h，40 ℃条件下超声（650 W，40 kHz）提取2 h，提取液置于1.5 mL离心管中，3 000 r·min-1离心15 min，取上清液，即得（对应化合物质量浓度为7-羟基香豆素0.146 8 mg·mL-1，秦皮素0.251 2 mg·mL-1，异嗪皮啶0.542 4 mg·mL-1，东莨菪内酯0.246 7 mg·mL-1）。
2.2　动物分组与给药
6只大鼠适应性喂养14 d，试验前禁食不禁水12 h，按照10 mL·kg-1给药刺五加提取液（相当于给药剂量为7-羟基香豆素0.293 6 mg·kg-1，秦皮素0.502 4 mg·kg-1，异嗪皮啶1.084 8 mg·kg-1，东莨菪内酯0.493 4 mg·kg-1）和刺五加注射液（相当于给药剂量为7-羟基香豆素0.376 3 mg·kg-1，秦皮素0.642 6 mg·kg-1，异嗪皮啶1.387 5 mg·kg-1，东莨菪内酯0.632 3 mg·kg-1），分别于给药后5、15、30、45、60、90、120、180、240、360、480、600、720、1 440 min眼眶取血约0.5 mL，将全血置于肝素钠管中，低温离心（4 ℃，3 000 r·min-1，15 min），取上清，即得血浆样品，于-80 ℃保存待测。
2.3　混合对照品溶液的制备
精密称取对照品7-羟基香豆素10.25 mg、秦皮素11.10 mg、异嗪皮啶10.25 mg、东莨菪内酯10.55 mg，分别置于10 mL量瓶中，用甲醇溶解并定容至刻度，摇匀，得混合对照品储备液，用甲醇稀释至不同浓度（7-羟基香豆素0.05、1、2.5、5、10、25、51.25 μg·mL-1，秦皮素0.05、1、2.5、5、10、25、55.50 μg·mL-1，异嗪皮啶0.05、1、2.5、5、10、25、51.25 μg·mL-1，东莨菪内酯0.05、1、2.5、5、10、25、52.75 μg·mL-1），即得。
精密称取牡荆素对照品2.00 mg，用甲醇配制成质量浓度为20 μg·mL-1的内标溶液。
2.4　对照品血浆的制备及处理
精密吸取空白大鼠血浆100 μL，置1.5 mL EP管中，加入不同浓度混合对照品溶液10 μL及内标溶液10 μL，混匀，加甲醇380 μL，涡旋30 s，静置30 min，离心（4 ℃，13 000 r·min-1，15 min），取上清过0.22 μm微孔滤膜，置进样瓶中，待测。
2.5　血浆样品处理
取大鼠血浆100 μL，置1.5 mL EP管中，加入内标溶液10 μL，混匀，加入甲醇390 μL，按照“2.4”项方法操作，即得。
2.6　UPLC-MS测试条件
高分辨质量光谱参数：鞘气压力为0.206 8 MPa，辅助气体压力为0.068 9 MPa，吹扫气压力为0 MPa；毛细管电压正离子模式为3.5 kV，负离子模式为3.2 kV；离子传输管温度为320 ℃；AUX气体加热温度为350 ℃；碰撞气体为高纯氮气（99.999 9%）；归一化碰撞能量为10、40、70 eV；s-lens透镜振幅为60.0；扫描模式：平行监测扫描触发二级质谱扫描，监测离子扫描质量锁定为m/z 163.039 08、m/z 209.044 51、m/z 223.060 15、m/z 193.049 18、m/z 433.112 88。特异性丢失扫描质量锁定为m/z 135.044 14、m/z 194.020 78、m/z 255.029 69、m/z 178.025 82。分子量特异性丢失误差范围设置为500×10-6（parts per million）。一级质谱分辨率为70 000 FWHM，二级质谱分辨率为17 500 FWHM；离子扫描范围为m/z 50~1 500；微扫描次数为3次；四级隔离窗为m/z 1.5；动态排除时间为5 s。
色谱条件：采用Thermo Scientific Hypersil GOLD aQ色谱柱（100 min×2.1 mm，1.9 μm），流动相为0.1%甲酸-水（A）和0.1%甲酸-乙腈（B），等度洗脱（0~8 min，82：18），流速0.30 mL·min-1，柱温40 ℃，进样量5 μL。
2.7　体内分析方法的建立
2.7.1　稳定性考察
将血浆样品在4 ℃下放置0、2、4、6、8、10、12、24 h后分别进样，考察静置稳定性，结果见表1，目标成分峰面积的RSD均<6%，表明血浆样品在24 h内稳定性良好。将血浆样品置于-80 ℃下冻融循环3次，分别进样，考察冻融稳定性，结果目标成分峰面积的RSD均<8%，表明血浆样品冻融稳定性良好。
2.7.2　专属性考察
对大鼠空白血浆、对照品血浆、血浆样品分别进样分析，检验方法专属性，结果见图1。除目标组分外，无其他杂峰及假阳性离子峰的干扰，说明该方法能够准确检测目标成分且无干扰，检测专属性良好。
2.7.3　基质效应考察
取大鼠空白血浆100 μL，按照“2.4”项方法操作，配制成低、中、高3个浓度（7-羟基香豆素0.05、5、51.25 μg·mL-1，秦皮素0.05、5、55.50 μg·mL-1，异嗪皮啶0.05、5、51.25 μg·mL-1，东莨菪内酯0.05、5、52.75 μg·mL-1）的质控溶液，作为基质溶液。将10 μL对照品溶液（低、中、高）与10 μL内标溶液、480 μL甲醇混匀，作为无基质溶液，每份溶液平行测定6次，根据峰面积计算RSD。以基质溶液与无基质溶液响应值的比值检验基质效应，结果（表2）基质效应均在96.6%~102.4%，表明基质效应对实验结果的影响较小，符合试验要求；平行测定6次峰面积的RSD均<3%，表明试验数据可靠。
2.7.4　精密度试验
对低、中、高3个浓度溶液分别测定6次，根据峰面积计算批内精密度；对低、中、高3个浓度溶液平行配制5份溶液进样分析，根据峰面积计算批间精密度。结果见表3、表4，精密度RSD均<6%，表明方法精密度良好。
2.7.5　线性关系考察
对样品用内标法进行定量检测。以药物浓度X（μg·mL-1）为横坐标，样品与内标的峰面积比值Y为纵坐标，进行加权线性回归。以绝对进样量3倍于信噪比的比值为检测限，绝对进样量10倍于信噪比的比值为定量限，结果见表5。r均>0.997，表明回归方程相关性良好，定量限RSD均<5%。
2.7.6　回收率试验
对血浆样品加入已知浓度的对照品溶液进样分析，计算回收率，结果见表6，回收率均在88%~109%，表明方法准确度良好。
2.8　药代动力学及生物利用度研究
2.8.1　药代动力学参数结果
以统计矩方法计算药动学参数，结果见表7。刺五加提取液ig药时曲线图见图2。
2.8.2　个体差异结果
采用SPSS软件对6只大鼠血浆样品数据进行独立个体差异性分析，以大鼠编号为分组变量，总离子流图相对丰度为检验变量，设置置信区间百分比为95%，每组数据与其他组数据单循环检验后取均值，P均>0.05，表明独立样本之间没有显著性差异。对每只大鼠的血浆样品与总样品均值进行单样本差异性检验，设置置信区间百分比为95%，P均>0.05，表明单样本与总样本量均值没有显著性差异，表8列出了个体差异性详细结果，表明大鼠之间的个体性差异在实验可接受范围内，研究数据有效，可用于后续研究参考。
2.8.3　绝对和相对生物利用度
根据刺五加提取液ig血药浓度-时间曲线图，计算血管外AUC；根据刺五加提取液iv（给药剂量为7-羟基香豆素0.293 6 mg·kg-1、秦皮素0.502 4 mg·kg-1、异嗪皮啶1.084 8 mg·kg-1、东莨菪内酯0.493 4 mg·kg-1），计算血管内AUC。根据刺五加提取液ig血药浓度-时间曲线图，计算试验制剂AUC；根据刺五加注射液ig血药浓度-时间曲线图，计算参比制剂AUC。通过个体差异检验后每组实验结果取均值，详细结果见表9，生物利用度结果见表10。
2.9　质谱裂解研究结果
经Xcalibur软件处理，在刺五加提取液和大鼠血浆的MS图中均发现m/z 163.039 08的准分子离子峰，设定正负扫描模式质量校正误差范围为5×10-6，根据软件分析，在[M+H]模式下锁定1种加和离子化学式，在m/z 163.039 08的MS2光谱图下显示了1个信号强度为4×107的m/z 163.039 08的前体离子，校正误差为-0.671×10-6，质谱图结果显示，前体离子在20能量下丢失羰基基团，在更高的能量下逐渐丢失16、12、12的碎片，这与7-羟基香豆素的苯环开裂丢失CO，在最优能量55的碰撞下，与苯环逐渐丢失O、C、C原子的相对分子质量吻合，初步鉴定该化合物为7-羟基香豆素。
结合mzVault和Thermo Scientific OTCML本地数据库，给出该化合物匹配分数为93.3，数据库的二级光谱图下在m/z 135.044 05、119.049 35、107.049 48处出现了与实验数据相同的特征碎片峰，文献报道该化合物计算化学参数中的不饱和度为6.5，与软件计算结果一致，经与mzCloud光谱数据库比对，匹配率高达90.5%，确定该化合物为7-羟基香豆素，裂解途径见图3。
经Xcalibur软件处理，发现在刺五加提取液和大鼠血浆的MS图中均出现m/z 209.044 51的准分子离子峰，设定正负模式质量校正误差范围为5×10-6，根据软件分析，在[M+H]模式下锁定1种加和离子化学式，在m/z 209.044 51的MS2光谱图下显示了1个信号强度为3×106的m/z 209.044 51的前体离子，校正误差为0.288×10-6，后续在低能量下观察到碎片信息为m/z 194.020 78、149.023 21、121.028 48，此结构经过与数据库比对分析，为陆续丢失甲基基团、羧基基团、羰基基团形成；在高能量下观察到m/z 181.049 32、163.038 71、135.043 98、107.049 40的碎片，该碎片形成为丢失羰基基团、水分子、接着苯环连续断裂丢失2个羰基基团，最终形成苯甲醛结构，为苯环的氢被醛基取代后的化合物，此裂解规律符合秦皮素质谱数据，因此初步鉴定该化合物为秦皮素。
结合mzVault和Thermo Scientific OTCML本地数据库，给出该化合物匹配分数为91.8，数据库的二级光谱图下，在m/z 194.020 78、163.038 71、149.023 21、135.043 98、107.049 40处出现了与实验数据相同的特征碎片峰，文献报道该化合物计算化学参数中的不饱和度为6.5，与软件计算结果一致，经过与mzCloud光谱数据库比对，匹配率高达89.4%，确定该化合物为秦皮素，裂解途径见图4。
经Xcalibur软件处理，发现在刺五加提取液和大鼠血浆的MS图中均出现m/z 223.060 15的准分子离子峰，设定正负模式质量校正误差范围为5×10-6，根据软件分析，在[M+H]模式下锁定1种加和离子化学式，在m/z 223.060 15的MS2光谱图下显示了1个信号强度为1×108的m/z 223.060 15的前体离子，校正误差为-0.403×10-6，经过分析质谱图，发现该化合物的裂解规律与秦皮素大同小异，不同之处在于低能量下首先发生去甲基基团，随后发生的裂解都一致，最终生成醛基取代苯环的氢形成的苯甲醛结构，与秦皮素结构拟合后，初步鉴定该化合物为异嗪皮啶。
结合mzVault和Thermo Scientific OTCML本地数据库给出该化合物匹配分数为92.8，数据库的二级光谱图下在m/z 208.036 32、194.020 80、190.025 85、162.030 96、135.044 02、107.049 42处出现了与实验数据相同的特征碎片峰，文献报道该化合物计算化学参数中的不饱和度为6.5，与软件计算结果一致，经过与mzCloud光谱数据库比对，匹配率高达92.2%，经上述鉴定，该化合物为异嗪皮啶，裂解途径见图5。
经Xcalibur软件处理，发现在刺五加提取液和大鼠血浆的MS图中均出现m/z 193.049 18的准分子离子峰，设定正负模式质量校正误差范围为5×10-6，根据软件分析，在[M+H]模式下锁定1种加和离子化学式，在m/z 193.049 18的MS2光谱图下显示了1个信号强度为6×105的m/z 193.049 18的前体离子，校正误差为-0.286×10-6，经过对数据裂解分析，20能量下发现4个碎片离子m/z 178.025 82、150.031 01、122.036 30、105.033 91，经过分析为陆续丢失甲基基团、羧基基团、羰基基团和羟基基团；在60能量下又发现3个碎片离子m/z 165.054 35、137.059 60、133.028 35，为丢失2个羰基和甲基基团所形成，该裂解模式与秦皮素裂解规律和异嗪皮啶的去甲基化后续裂解规律类似，结合化学式初步鉴定该化合物为东莨菪内酯或异莨菪亭。它们均为苯丙素类化合物，最终碎片都为苯环被不同基团所取代的结构。东莨菪内酯与异莨菪亭属于同分异构体，其区别在于香豆素结构的6号位和7号位取代基的顺序，东莨菪内酯为羟基取代7号位，甲氧基取代6号位；而异莨菪亭为羟基取代6号位，甲氧基取代7号位。但由于质谱无法区分，因此选择与对照品保留时间比对，最终鉴定为东莨菪内酯。
结合mzVault和Thermo Scientific OTCML本地数据库给出该化合物匹配分数为95.9，数据库的二级光谱图下在m/z 178.025 82、165.054 35、133.028 35、122.036 30处出现了与实验数据相同的特征碎片峰，文献报道该化合物计算化学参数中的不饱和度为6.5，与软件计算结果一致，经过与mzCloud光谱数据库比对，匹配率高达93.7%，经上述鉴定，该化合物为东莨菪内酯，裂解途径见图6。
3　结论
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本研究根据LC-MS/MS裂解规律，定性刺五加在大鼠体内入血的4种木脂素成分并建立了1种体内分析方法，计算血浆中4个化学成分的药代动力学参数，包括达峰时间、达峰浓度、半衰期、药时曲线下面积、清除率、表观分布容积。统计结果显示，各组间差异的P均>0.05，说明个体间的差异在实验可接受的误差范围内。4个化合物的绝对生物利用度为63%~78%，相对生物利用度为82%~85%，说明刺五加水提物的生物利用度较好，本研究有助于为刺五加的临床应用提供参考。
基金
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  • *黑龙江省佳木斯大学北药与功能食品(JDXKTD-2019005)
文献
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2024年第44卷第5期
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doi: 10.16155/j.0254-1793.2024.05.12
  • 接收时间：2023-06-11
  • 首发时间：2026-03-20
  • 出版时间：2024-05-31
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  • 收稿日期：2023-06-11
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*黑龙江省佳木斯大学北药与功能食品(JDXKTD-2019005)
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    佳木斯大学药学院，佳木斯 154007

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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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