首页 期刊 论文 学科刊群 资讯 加盟 关于
EN
image
Article(id=1239250706637582709, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239250701583446236, articleNumber=null, orderNo=null, doi=10.16155/j.0254-1793.2024.04.09, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1687104000000, receivedDateStr=2023-06-19, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773389992626, onlineDateStr=2026-03-13, pubDate=1714406400000, pubDateStr=2024-04-30, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773389992626, onlineIssueDateStr=2026-03-13, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773389992626, creator=13701087609, updateTime=1773389992626, updator=13701087609, issue=Issue{id=1239250701583446236, tenantId=1146029695717560320, journalId=1205117023404326918, year='2024', volume='44', issue='4', pageStart='553', pageEnd='736', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773389991422, creator=13701087609, updateTime=1773390513217, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1239252890213209050, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239250701583446236, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1239252890213209051, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1239250701583446236, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=620, endPage=627, ext={EN=ArticleExt(id=1239250706872463757, articleId=1239250706637582709, tenantId=1146029695717560320, journalId=1205117023404326918, language=EN, title=Research on the detection method of Draconis Sanguis adulterated Resina Draconis in Zhenghonghua oil*, columnId=1206272757852074373, journalTitle=Chinese Journal of Pharmaceutical Analysis, columnName=Safety Monitoring, runingTitle=null, highlight=null, articleAbstract=
Objective:

To establish a screening method for the detection of adulteration of Draconis Sanguis in Zhenghonghua oil.

Methods:

To establish a thin layer chromatography (TLC) method with 7, 4’-dihydroxyflavone as an index for fast screen of the adulteration in Zhenghonghua oil. The suspected samples were screened by TLC and the quantification was performed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The chromatographic column was SuperLu C18 (2)(100 mm×2.1 mm, 1.8 μm), the mobile phase was acetonitrile-water (25∶75) at a flow rate of 0.3 mL·min-1 and the column temperature was 25 ℃. The detection ion pairs for 7, 4’-dihydroxyflavone were m/z 253.1→117.1 (quantitative) and m/z 253.1→91.0 (qualitative).

Results:

TLC method was specific and durable. The linear range of 7, 4’-dihydroxyflavone was 0.470-37.58 ng·mL-1 (r=0.999 7) by UPLC-MS/MS. The average recovery rate(n=6) was 96.1% and RSD was 3.2%. Thirty batches of Zhenghonghua oil were screened by TLC, and 24 batches were suspected to have 7, 4’-dihydroxyflavone. The suspected samples were verified by UPLC-MS/MS, 24 batches of Zhenghonghua oil exceeded the proposed limit, and the verification results were consistent with TLC method.

Conclusion:

This method is rapid, accurate and can be used for the screening and analysis of adulterated Zhenghonghua oil.

, correspAuthors=Zai-min CHEN, Yong WANG, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, authorCompany=null, fund=null, authors=null, authorsList=Yan-ting LIU, Zai-min CHEN, Yong WANG), CN=ArticleExt(id=1239250709636510225, articleId=1239250706637582709, tenantId=1146029695717560320, journalId=1205117023404326918, language=CN, title=正红花油中血竭掺伪龙血竭检查方法的研究*, columnId=1206272758036623764, journalTitle=药物分析杂志, columnName=安全监测, runingTitle=null, highlight=null, articleAbstract=
目的：

建立正红花油中血竭掺伪的检测方法。

方法：

以7，4’-二羟基黄酮为指标建立薄层色谱(TLC)法，快速筛查正红花油中掺伪的龙血竭。TLC筛查出可疑样品，用超高效液相色谱串联质谱(UPLC-MS/MS)法进行确证并定量分析，采用SuperLu C18(2)(100 mm×2.1 mm，1.8 μm)色谱柱，以乙腈-水(25∶75)为流动相，流速0.3 mL·min-1，柱温25 ℃，选择m/z 253.1→117.1(定量)和m/z 253.1→91.0(定性)作为7，4’-二羟基黄酮检测离子对。

结果：

TLC方法专属性、耐用性良好。采用UPLC-MS/MS法，7，4’-二羟基黄酮质量浓度在0.470~37.58 ng·mL-1范围内线性良好(r=0.999 7)，加样平均回收率(n=6)为96.1%，RSD为3.2%。对30批正红花油进行薄层初筛，结果有24批疑似检出7，4’-二羟基黄酮。疑似样品通过UPLC-MS/MS验证，有24批正红花油超出拟定的限度，验证结果与TLC方法一致。

结论：

本方法快速，结果准确，灵敏度高，可用于正红花油中掺伪龙血竭筛查与分析。

, correspAuthors=陈在敏, 王勇, authorNote=null, correspAuthorsNote=
** 陈在敏　Tel：(0591)87671677；E-mail：
王勇　Tel：18959193539；E-mail：
, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=BQVMhXc586UPpWa//8TtFA==, magXml=S06FhpZpfbZlN02gM1Q5iA==, pdfUrl=null, pdf=UgSMqorW3xaWgkB3gsh60w==, pdfFileSize=4738828, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=POE3cpFCvFB/2h6HLD52tQ==, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=5GwLY0kl7rLpn1nAES5KGg==, mapNumber=null, authorCompany=null, fund=null, authors=

Tel：18805903391；E-mail：

, authorsList=刘岩庭, 陈在敏, 王勇)}, authors=[Author(id=1239250710114660913, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, orderNo=0, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=522157067@qq.com, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1239250710215324214, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, authorId=1239250710114660913, language=EN, stringName=Yan-ting LIU, firstName=Yan-ting, middleName=null, lastName=LIU, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Fujian Institute for Food and Drug Quality Control, Fuzhou 350012, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1239250710353736258, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, authorId=1239250710114660913, language=CN, stringName=刘岩庭, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=福建省食品药品质量检验研究院，福州 350012, bio={"content":"

Tel：18805903391；E-mail：

"}, bioImg=null, bioContent=

Tel：18805903391；E-mail：

, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1239250710022386213, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, xref=null, ext=[AuthorCompanyExt(id=1239250710026580518, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, companyId=1239250710022386213, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Fujian Institute for Food and Drug Quality Control, Fuzhou 350012, China), AuthorCompanyExt(id=1239250710034969127, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, companyId=1239250710022386213, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=福建省食品药品质量检验研究院，福州 350012)])]), Author(id=1239250710441816646, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, orderNo=1, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=505109226@qq.com, emailSecond=null, emailThird=null, correspondingAuthor=1, authorType=1, ext={EN=AuthorExt(id=1239250710529897037, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, authorId=1239250710441816646, language=EN, stringName=Zai-min CHEN, firstName=Zai-min, middleName=null, lastName=CHEN, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=**, address=Fujian Institute for Food and Drug Quality Control, Fuzhou 350012, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1239250710613783123, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, authorId=1239250710441816646, language=CN, stringName=陈在敏, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=**, address=福建省食品药品质量检验研究院，福州 350012, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1239250710022386213, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, xref=null, ext=[AuthorCompanyExt(id=1239250710026580518, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, companyId=1239250710022386213, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Fujian Institute for Food and Drug Quality Control, Fuzhou 350012, China), AuthorCompanyExt(id=1239250710034969127, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, companyId=1239250710022386213, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=福建省食品药品质量检验研究院，福州 350012)])]), Author(id=1239250710710252122, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, orderNo=2, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=1767559645@qq.com, emailSecond=null, emailThird=null, correspondingAuthor=1, authorType=1, ext={EN=AuthorExt(id=1239250710802526818, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, authorId=1239250710710252122, language=EN, stringName=Yong WANG, firstName=Yong, middleName=null, lastName=WANG, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=**, address=Fujian Institute for Food and Drug Quality Control, Fuzhou 350012, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1239250710907384423, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, authorId=1239250710710252122, language=CN, stringName=王勇, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=**, address=福建省食品药品质量检验研究院，福州 350012, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1239250710022386213, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, xref=null, ext=[AuthorCompanyExt(id=1239250710026580518, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, companyId=1239250710022386213, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Fujian Institute for Food and Drug Quality Control, Fuzhou 350012, China), AuthorCompanyExt(id=1239250710034969127, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, companyId=1239250710022386213, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=福建省食品药品质量检验研究院，福州 350012)])])], keywords=[Keyword(id=1239250711020630636, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=EN, orderNo=1, keyword=Zhenghonghua oil), Keyword(id=1239250711079350898, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=EN, orderNo=2, keyword=7，4’-dihydroxyflavone), Keyword(id=1239250711163236986, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=EN, orderNo=3, keyword=adulteration), Keyword(id=1239250711263900285, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=EN, orderNo=4, keyword=Draconis Sanguis), Keyword(id=1239250711360369284, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=EN, orderNo=5, keyword=Resina Draconis), Keyword(id=1239250711486198411, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=EN, orderNo=6, keyword=TLC), Keyword(id=1239250711565890192, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=EN, orderNo=7, keyword=UPLC-MS/MS), Keyword(id=1239250711666553495, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=CN, orderNo=1, keyword=正红花油), Keyword(id=1239250711754633886, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=CN, orderNo=2, keyword=7，4’-二羟基黄酮), Keyword(id=1239250711842714275, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=CN, orderNo=3, keyword=掺伪), Keyword(id=1239250711930794664, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=CN, orderNo=4, keyword=血竭), Keyword(id=1239250712027263662, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=CN, orderNo=5, keyword=龙血竭), Keyword(id=1239250712090178227, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=CN, orderNo=6, keyword=薄层色谱法), Keyword(id=1239250712178258619, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=CN, orderNo=7, keyword=超高效液相-质谱联用)], refs=[Reference(id=1239250715307209504, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2020, volume=null, issue=null, pageStart=149, pageEnd=null, url=null, language=null, rfNumber=[1], rfOrder=0, authorNames=null, journalName=null, refType=null, unstructuredReference=中华人民共和国药典2020年版. 一部[S]. 2020：149, articleTitle=null, refAbstract=null), Reference(id=1239250715403678500, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2020, volume=null, issue=null, pageStart=149, pageEnd=null, url=null, language=null, rfNumber=[1], rfOrder=1, authorNames=null, journalName=null, refType=null, unstructuredReference=ChP 2020. Vol Ⅰ[S]. 2020：149, articleTitle=null, refAbstract=null), Reference(id=1239250715491758889, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2011, volume=24, issue=8, pageStart=17, pageEnd=null, url=null, language=null, rfNumber=[2], rfOrder=2, authorNames=赵江红, journalName=中医研究, refType=null, unstructuredReference=赵江红. 高效液相色谱法鉴定29批血竭中非法添加的3种化学成分[J]. 中医研究，2011，24(8)：17, articleTitle=高效液相色谱法鉴定29批血竭中非法添加的3种化学成分, refAbstract=null), Reference(id=1239250715588227888, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2011, volume=24, issue=8, pageStart=17, pageEnd=null, url=null, language=null, rfNumber=[2], rfOrder=3, authorNames=ZHAO JH, journalName=Tradit Chin Med Res, refType=null, unstructuredReference=ZHAO JH. Identification of three chemical components illegally added in 29 batches of Draconis Sanguis by high performance liquid chromatography[J]. Tradit Chin Med Res，2011，24(8)：17, articleTitle=Identification of three chemical components illegally added in 29 batches of Draconis Sanguis by high performance liquid chromatography, refAbstract=null), Reference(id=1239250715663725361, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2020, volume=40, issue=5, pageStart=865, pageEnd=null, url=null, language=null, rfNumber=[3], rfOrder=4, authorNames=冼小敏, 林蔚文, 陈伟康, journalName=药物分析杂志, refType=null, unstructuredReference=冼小敏，林蔚文，陈伟康，等. HPLC-DAD法测定血竭饮片中添加苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ及808猩红[J]. 药物分析杂志，2020，40(5)：865, articleTitle=HPLC-DAD法测定血竭饮片中添加苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ及808猩红, refAbstract=null), Reference(id=1239250715739222838, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2020, volume=40, issue=5, pageStart=865, pageEnd=null, url=null, language=null, rfNumber=[3], rfOrder=5, authorNames=XIAN XM, LIN WW, CHEN WK, journalName=Chin J Pharm Anal, refType=null, unstructuredReference=XIAN XM，LIN WW，CHEN WK，et al. Determination of Sudan scarlet added in Draconis Sanguis by HPLC-DAD[J]. Chin J Pharm Anal，2020，40(5)：865, articleTitle=Determination of Sudan scarlet added in Draconis Sanguis by HPLC-DAD, refAbstract=null), Reference(id=1239250715823108920, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2019, volume=54, issue=9, pageStart=695, pageEnd=null, url=null, language=null, rfNumber=[4], rfOrder=6, authorNames=廖嘉宝, 张鹏, 谭沛, journalName=浙江中医杂志, refType=null, unstructuredReference=廖嘉宝，张鹏，谭沛，等. 利用红外光谱法快速测定血竭中掺假松香的含量[J]. 浙江中医杂志，2019，54(9)：695, articleTitle=利用红外光谱法快速测定血竭中掺假松香的含量, refAbstract=null), Reference(id=1239250715911189311, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2019, volume=54, issue=9, pageStart=695, pageEnd=null, url=null, language=null, rfNumber=[4], rfOrder=7, authorNames=LIAO JB, ZHANG P, TAN P, journalName=Zhejiang J Tradit Chin Med, refType=null, unstructuredReference=LIAO JB，ZHANG P，TAN P，et al. The content of adulterated rosin in Draconis Sanguis was rapidly determined by infrared spectroscopy[J]. Zhejiang J Tradit Chin Med，2019，54(9)：695, articleTitle=The content of adulterated rosin in Draconis Sanguis was rapidly determined by infrared spectroscopy, refAbstract=null), Reference(id=1239250716032824131, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2020, volume=56, issue=12, pageStart=1267, pageEnd=null, url=null, language=null, rfNumber=[5], rfOrder=8, authorNames=张明童, 刘志荣, 李冬华, journalName=理化检验-化学分册, refType=null, unstructuredReference=张明童，刘志荣，李冬华，等. 薄层色谱法和高效液相色谱法鉴别掺伪龙血竭的血竭[J]. 理化检验-化学分册，2020，56(12)：1267, articleTitle=薄层色谱法和高效液相色谱法鉴别掺伪龙血竭的血竭, refAbstract=null), Reference(id=1239250716129293125, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2020, volume=56, issue=12, pageStart=1267, pageEnd=null, url=null, language=null, rfNumber=[5], rfOrder=9, authorNames=ZHANG MT, LIU ZR, LI DH, journalName=Phys Test Chem Anal Part B：Chem Anal, refType=null, unstructuredReference=ZHANG MT，LIU ZR，LI DH，et al. Identification of Draconis Sanguis adulterated with Resina Draconis by thin layer chromatography and HPLC[J]. Phys Test Chem Anal Part B：Chem Anal，2020，56(12)：1267, articleTitle=Identification of Draconis Sanguis adulterated with Resina Draconis by thin layer chromatography and HPLC, refAbstract=null), Reference(id=1239250716196401992, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2019, volume=19, issue=66, pageStart=36, pageEnd=null, url=null, language=null, rfNumber=[6], rfOrder=10, authorNames=薛恒跃, 邹亮, 秦峥, journalName=世界最新医学信息文摘, refType=null, unstructuredReference=薛恒跃，邹亮，秦峥. 含血竭中成药中掺杂龙血竭的鉴别研究[J]. 世界最新医学信息文摘，2019，19(66)：36, articleTitle=含血竭中成药中掺杂龙血竭的鉴别研究, refAbstract=null), Reference(id=1239250716255122251, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2019, volume=19, issue=66, pageStart=36, pageEnd=null, url=null, language=null, rfNumber=[6], rfOrder=11, authorNames=XUE HY, ZOU L, QIN Z, journalName=World Latest Med Inf, refType=null, unstructuredReference=XUE HY，ZOU L，QIN Z. Identification study of Resina Draconis mixed into traditional Chinese medicine containing Draconis Sanguis[J]. World Latest Med Inf，2019，19(66)：36, articleTitle=Identification study of Resina Draconis mixed into traditional Chinese medicine containing Draconis Sanguis, refAbstract=null), Reference(id=1239250716339008334, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2019, volume=36, issue=20, pageStart=2605, pageEnd=null, url=null, language=null, rfNumber=[7], rfOrder=12, authorNames=张丽, 王绪平, 黄孝闻, journalName=中国现代应用药学, refType=null, unstructuredReference=张丽，王绪平，黄孝闻，等. 血竭及龙血竭化学成分、药理作用研究进展[J]. 中国现代应用药学，2019，36(20)：2605, articleTitle=血竭及龙血竭化学成分、药理作用研究进展, refAbstract=null), Reference(id=1239250716456448850, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2019, volume=36, issue=20, pageStart=2605, pageEnd=null, url=null, language=null, rfNumber=[7], rfOrder=13, authorNames=ZHANG L, WANG XP, HUANG XW, journalName=Chin J Mod Appl Pharm, refType=null, unstructuredReference=ZHANG L，WANG XP，HUANG XW，et al. Advance of the chemical components and pharmacological effects of Draconis Sanguis and Resina Draconis[J]. Chin J Mod Appl Pharm，2019，36(20)：2605, articleTitle=Advance of the chemical components and pharmacological effects of Draconis Sanguis and Resina Draconis, refAbstract=null), Reference(id=1239250716557112151, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2020, volume=29, issue=6, pageStart=50, pageEnd=null, url=null, language=null, rfNumber=[8], rfOrder=14, authorNames=林忆龙, 文亦磊, 黄洪, journalName=中国民族民间医药, refType=null, unstructuredReference=林忆龙，文亦磊，黄洪，等. 龙血竭化学成分及药理作用研究进展[J]. 中国民族民间医药，2020，29(6)：50, articleTitle=龙血竭化学成分及药理作用研究进展, refAbstract=null), Reference(id=1239250716666164059, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2020, volume=29, issue=6, pageStart=50, pageEnd=null, url=null, language=null, rfNumber=[8], rfOrder=15, authorNames=LIN YL, WEN YL, HUANG H, journalName=Chin J Ethnomed Ethnopharm, refType=null, unstructuredReference=LIN YL，WEN YL，HUANG H，et al. Chemical constituents and pharmacological research of the Resina Draconis[J]. Chin J Ethnomed Ethnopharm，2020，29(6)：50, articleTitle=Chemical constituents and pharmacological research of the Resina Draconis, refAbstract=null), Reference(id=1239250716750050138, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2003, volume=1, issue=1, pageStart=27, pageEnd=null, url=null, language=null, rfNumber=[9], rfOrder=16, authorNames=屠鹏飞, 陶晶, 胡迎庆, journalName=中国天然药物, refType=null, unstructuredReference=屠鹏飞，陶晶，胡迎庆，等. 龙血竭黄酮类成分研究[J]. 中国天然药物，2003，1(1)：27, articleTitle=龙血竭黄酮类成分研究, refAbstract=null), Reference(id=1239250716821353310, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2003, volume=1, issue=1, pageStart=27, pageEnd=null, url=null, language=null, rfNumber=[9], rfOrder=17, authorNames=TU PF, TAO J, HU YQ, journalName=Chin J Nat Med, refType=null, unstructuredReference=TU PF，TAO J，HU YQ，et al. Flavones from wood Dracaena conchinensis[J]. Chin J Nat Med，2003，1(1)：27, articleTitle=Flavones from wood Dracaena conchinensis, refAbstract=null), Reference(id=1239250716913628003, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2012, volume=18, issue=3, pageStart=45, pageEnd=null, url=null, language=null, rfNumber=[10], rfOrder=18, authorNames=李云, 萧伟, 秦建平, journalName=中国实验方剂学杂志, refType=null, unstructuredReference=李云，萧伟，秦建平，等. HPLC测定龙血竭提取物中龙血素A，B和7，4’-二羟基黄酮的含量[J]. 中国实验方剂学杂志，2012，18(3)：45, articleTitle=HPLC测定龙血竭提取物中龙血素A，B和7，4’-二羟基黄酮的含量, refAbstract=null), Reference(id=1239250718410994539, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2012, volume=18, issue=3, pageStart=45, pageEnd=null, url=null, language=null, rfNumber=[10], rfOrder=19, authorNames=LI Y, XIAO W, QIN JP, journalName=Chin J Exp Tradit Med, refType=null, unstructuredReference=LI Y，XIAO W，QIN JP，et al. Determination of loureirin A，B and 7，4’-dihydroxy flavone in extract of Resina Draconis by HPLC[J]. Chin J Exp Tradit Med，2012，18(3)：45, articleTitle=Determination of loureirin A，B and 7，4’-dihydroxy flavone in extract of Resina Draconis by HPLC, refAbstract=null), Reference(id=1239250718503269232, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2022, volume=44, issue=4, pageStart=1058, pageEnd=null, url=null, language=null, rfNumber=[11], rfOrder=20, authorNames=江立, 孙成逊, 田雪丽, journalName=中成药, refType=null, unstructuredReference=江立，孙成逊，田雪丽，等. 龙血竭片中3种成分体外溶出度的测定[J]. 中成药，2022，44(4)：1058, articleTitle=龙血竭片中3种成分体外溶出度的测定, refAbstract=null), Reference(id=1239250718599738230, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2022, volume=44, issue=4, pageStart=1058, pageEnd=null, url=null, language=null, rfNumber=[11], rfOrder=21, authorNames=JIANG L, SUN CX, TIAN XL, journalName=Chin Tradit Pat Med, refType=null, unstructuredReference=JIANG L，SUN CX，TIAN XL，et al. Determination of in vitro dissolution rates of three constituents in Longxuejie tablets[J]. Chin Tradit Pat Med，2022，44(4)：1058, articleTitle=Determination of in vitro dissolution rates of three constituents in Longxuejie tablets, refAbstract=null), Reference(id=1239250718754927487, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2014, volume=34, issue=5, pageStart=819, pageEnd=null, url=null, language=null, rfNumber=[12], rfOrder=22, authorNames=秦建平, 吴建雄, 李艳静, journalName=药物分析杂志, refType=null, unstructuredReference=秦建平，吴建雄，李艳静，等. DART/Q-TOF-MS快速鉴定龙血竭中5个酚酸类成分[J]. 药物分析杂志，2014，34(5)：819, articleTitle=DART/Q-TOF-MS快速鉴定龙血竭中5个酚酸类成分, refAbstract=null), Reference(id=1239250718834619264, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2014, volume=34, issue=5, pageStart=819, pageEnd=null, url=null, language=null, rfNumber=[12], rfOrder=23, authorNames=QIN JP, WU JX, LI YJ, journalName=Chin J Pharm Anal, refType=null, unstructuredReference=QIN JP，WU JX，LI YJ，et al. Rapid identification and characterization of five phenolic compounds in Resina Draconis by DART/Q-TOF-MS[J]. Chin J Pharm Anal，2014，34(5)：819, articleTitle=Rapid identification and characterization of five phenolic compounds in Resina Draconis by DART/Q-TOF-MS, refAbstract=null), Reference(id=1239250718926893956, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2012, volume=37, issue=7, pageStart=929, pageEnd=null, url=null, language=null, rfNumber=[13], rfOrder=24, authorNames=李云, 萧伟, 秦建平, journalName=中国中药杂志, refType=null, unstructuredReference=李云，萧伟，秦建平，等. HPLC同时测定龙血竭及其提取物中5个有效成分的含量[J]. 中国中药杂志，2012，37(7)：929, articleTitle=HPLC同时测定龙血竭及其提取物中5个有效成分的含量, refAbstract=null), Reference(id=1239250719019168648, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2012, volume=37, issue=7, pageStart=929, pageEnd=null, url=null, language=null, rfNumber=[13], rfOrder=25, authorNames=LI Y, XIAO W, QIN JP, journalName=China J Chin Mater Med, refType=null, unstructuredReference=LI Y，XIAO W，QIN JP，et al. Simultaneous determination of five active components in Resina Draconis and its extract by HPLC[J]. China J Chin Mater Med，2012，37(7)：929, articleTitle=Simultaneous determination of five active components in Resina Draconis and its extract by HPLC, refAbstract=null), Reference(id=1239250719136609162, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2013, volume=28, issue=4, pageStart=547, pageEnd=null, url=null, language=null, rfNumber=[14], rfOrder=26, authorNames=秦建平, 吴建雄, 李家春, journalName=现代药物与临床, refType=null, unstructuredReference=秦建平，吴建雄，李家春，等. 不同产地龙血竭中5种成分的HPLC法测定[J]. 现代药物与临床，2013，28(4)：547, articleTitle=不同产地龙血竭中5种成分的HPLC法测定, refAbstract=null), Reference(id=1239250719224689550, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2013, volume=28, issue=4, pageStart=547, pageEnd=null, url=null, language=null, rfNumber=[14], rfOrder=27, authorNames=QIN JP, WU JX, LI JC, journalName=Drugs Clin, refType=null, unstructuredReference=QIN JP，WU JX，LI JC，et al. Determination of five components in Draconis Resina from different habitats by HPLC[J]. Drugs Clin，2013，28(4)：547, articleTitle=Determination of five components in Draconis Resina from different habitats by HPLC, refAbstract=null), Reference(id=1239250719321158547, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2017, volume=48, issue=21, pageStart=4541, pageEnd=null, url=null, language=null, rfNumber=[15], rfOrder=28, authorNames=万青, 王文清, 方建国, journalName=中草药, refType=null, unstructuredReference=万青，王文清，方建国，等. 一测多评法测定龙血竭中5种有效成分[J]. 中草药，2017，48(21)：4541, articleTitle=一测多评法测定龙血竭中5种有效成分, refAbstract=null), Reference(id=1239250719405044631, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2017, volume=48, issue=21, pageStart=4541, pageEnd=null, url=null, language=null, rfNumber=[15], rfOrder=29, authorNames=WAN Q, WANG WQ, FANG JG, journalName=Chin Tradit Herb Drugs, refType=null, unstructuredReference=WAN Q，WANG WQ，FANG JG，et al. Determination of five active components in Draconis Resina by QAMS method[J]. Chin Tradit Herb Drugs，2017，48(21)：4541, articleTitle=Determination of five active components in Draconis Resina by QAMS method, refAbstract=null), Reference(id=1239250719493125017, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2021, volume=24, issue=3, pageStart=599, pageEnd=null, url=null, language=null, rfNumber=[16], rfOrder=30, authorNames=高柳, 张晓莉, 杨晨, journalName=中国药师, refType=null, unstructuredReference=高柳，张晓莉，杨晨，等. 超声波协同半仿生法提取龙血竭中4种成分的工艺研究[J]. 中国药师，2021，24(3)：599, articleTitle=超声波协同半仿生法提取龙血竭中4种成分的工艺研究, refAbstract=null), Reference(id=1239250719631537057, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2021, volume=24, issue=3, pageStart=599, pageEnd=null, url=null, language=null, rfNumber=[16], rfOrder=31, authorNames=GAO L, ZHANG XL, YANG C, journalName=China Pharm, refType=null, unstructuredReference=GAO L，ZHANG XL，YANG C，et al. Study on the ultrasonic-assisted semi-bionic extraction technology for 4 components from Resina Draconis[J]. China Pharm，2021，24(3)：599, articleTitle=Study on the ultrasonic-assisted semi-bionic extraction technology for 4 components from Resina Draconis, refAbstract=null), Reference(id=1239250719744783267, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2023, volume=29, issue=1, pageStart=39, pageEnd=null, url=null, language=null, rfNumber=[17], rfOrder=32, authorNames=林爽, 王杰, 高珊珊, journalName=中医药导报, refType=null, unstructuredReference=林爽，王杰，高珊珊，等. 基于薄层色谱法和超高效液相色谱法对龙血竭的质量评价研究[J]. 中医药导报，2023，29(1)：39, articleTitle=基于薄层色谱法和超高效液相色谱法对龙血竭的质量评价研究, refAbstract=null), Reference(id=1239250719870612391, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, doi=null, pmid=null, pmcid=null, year=2023, volume=29, issue=1, pageStart=39, pageEnd=null, url=null, language=null, rfNumber=[17], rfOrder=33, authorNames=LIN S, WANG J, GAO SS, journalName=Guid J Tradit Chin Med Pharm, refType=null, unstructuredReference=LIN S，WANG J，GAO SS，et al. Study on the quality evaluation of Longxuejie (Resina Draconis) based on TLC and UPLC[J]. Guid J Tradit Chin Med Pharm，2023，29(1)：39, articleTitle=Study on the quality evaluation of Longxuejie (Resina Draconis) based on TLC and UPLC, refAbstract=null)], funds=[Fund(id=1239250715118465810, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, awardId=2020Y0073, language=CN, fundingSource=*福建省科技计划项目(2020Y0073), fundOrder=null, country=null), Fund(id=1239250715202351897, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, awardId=2020Z007, language=CN, fundingSource=国家药典委员会标准提高项目(2020Z007), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1239250710022386213, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, xref=null, ext=[AuthorCompanyExt(id=1239250710026580518, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, companyId=1239250710022386213, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Fujian Institute for Food and Drug Quality Control, Fuzhou 350012, China), AuthorCompanyExt(id=1239250710034969127, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, companyId=1239250710022386213, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=福建省食品药品质量检验研究院，福州 350012)])], figs=[ArticleFig(id=1239250712308282051, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=EN, label=Fig.1, caption=TLC of specific experiment of Zhenghonghua oil, figureFileSmall=LVE7EaKEBGSpsxyWHNjYjQ==, figureFileBig=POE3cpFCvFB/2h6HLD52tQ==, tableContent=null), ArticleFig(id=1239250712396362441, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=CN, label=图1, caption=正红花油专属性实验薄层色谱图

1.缺血竭阴性样品(negative sample without Draconis Sanguis)　2.标准制剂样品(standard preparation sample)　3.阳性样品(positive sample) 4. 7，4’-二羟基黄酮对照品溶液(7，4’-dihydroxyflavone reference substance solution)　5.血竭对照药材溶液(Draconis Sanguis　reference crude drug solution)　6.龙血竭对照药材溶液(Resina Draconis reference crude drug solution)

, figureFileSmall=LVE7EaKEBGSpsxyWHNjYjQ==, figureFileBig=POE3cpFCvFB/2h6HLD52tQ==, tableContent=null), ArticleFig(id=1239250714015363798, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=EN, label=Fig.2, caption=TLC of Zhenghonghua oil, figureFileSmall=vip5LbH43/OUMhA1+L3R9w==, figureFileBig=QknFgWO0p0SmHfh68Ykxqw==, tableContent=null), ArticleFig(id=1239250714103444186, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=CN, label=图2, caption=正红花油薄层色谱

1. 7，4’-二羟基黄酮对照品(7，4’-dihydroxyflavone reference substance)　2~31.正红花油样品（编号A1~A30） [Zhenghonghua oil sample （No.A1-A30）]

, figureFileSmall=vip5LbH43/OUMhA1+L3R9w==, figureFileBig=QknFgWO0p0SmHfh68Ykxqw==, tableContent=null), ArticleFig(id=1239250714191524572, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=EN, label=Fig.3, caption=UPLC-MS/MS chromatograms of Zhenghonghua oil, figureFileSmall=IWD6SaDb2DyG5PLyPs+sbA==, figureFileBig=GJNThayGOUTZLW7HXyTJkA==, tableContent=null), ArticleFig(id=1239250714262827746, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=CN, label=图3, caption=正红花油UPLC-MS/MS色谱图

1. 7，4’-二羟基黄酮(7，4’-dihydroxyflavone)

, figureFileSmall=IWD6SaDb2DyG5PLyPs+sbA==, figureFileBig=GJNThayGOUTZLW7HXyTJkA==, tableContent=null), ArticleFig(id=1239250714338325223, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=EN, label=Fig.4, caption=TLC of Draconis Sanguis and Resina Draconis, figureFileSmall=aKuIaBc++ItS+YvzoYFWPw==, figureFileBig=qW8ObMOs+KBJ25eztTHolQ==, tableContent=null), ArticleFig(id=1239250714434794221, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=CN, label=图4, caption=血竭与龙血竭薄层色谱图

1~5.血竭药材溶液(Draconis Sanguis solution)　6.血竭对照药材溶液(Draconis Sanguis control solution)　7.龙血竭对照药材溶液(Resina Draconis control solution)　8~12.龙血竭药材溶液(Resina Draconis solution)

, figureFileSmall=aKuIaBc++ItS+YvzoYFWPw==, figureFileBig=qW8ObMOs+KBJ25eztTHolQ==, tableContent=null), ArticleFig(id=1239250714543846131, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=EN, label=Tab.1, caption=

MS parameters for 7，4’-dihydroxyflavone

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)		母离子
(parent ion)m/z		子离子
(product ion) m/z		去簇电压
(declustering potential)/V		碰撞能量
(collision energy)/eV
7，4’-二羟基黄酮(7，4’-dihydroxyflavone)253.1117.1[定量(quantification)]-76-38
91.0-138-37
), ArticleFig(id=1239250714640315129, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=CN, label=表1, caption=

7，4’-二羟基黄酮的质谱参数

, figureFileSmall=null, figureFileBig=null, tableContent=
成分
(component)		母离子
(parent ion)m/z		子离子
(product ion) m/z		去簇电压
(declustering potential)/V		碰撞能量
(collision energy)/eV
7，4’-二羟基黄酮(7，4’-dihydroxyflavone)253.1117.1[定量(quantification)]-76-38
91.0-138-37
), ArticleFig(id=1239250714724201215, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=EN, label=Tab.2, caption=

The results recovery test of 7，4’-dihydroxyflavone

, figureFileSmall=null, figureFileBig=null, tableContent=
序号
No.		取样量
(weighed)/g		含量
(original)/ng		加入量
(added)/ng		测得量
(measured)/ng		回收率
(recovery)		平均回收率
(average recovery)		RSD/%
10.248 910.1559.39518.91193.296.13.2
20.261 110.6539.39519.81397.5
30.263 710.7599.39519.75095.7
40.250 110.2049.39519.702101.1
50.257 610.5109.39519.56796.4
60.243 79.9439.39518.66292.8
), ArticleFig(id=1239250714837447429, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=CN, label=表2, caption=

7，4’-二羟基黄酮回收率试验结果(n=6)

, figureFileSmall=null, figureFileBig=null, tableContent=
序号
No.		取样量
(weighed)/g		含量
(original)/ng		加入量
(added)/ng		测得量
(measured)/ng		回收率
(recovery)		平均回收率
(average recovery)		RSD/%
10.248 910.1559.39518.91193.296.13.2
20.261 110.6539.39519.81397.5
30.263 710.7599.39519.75095.7
40.250 110.2049.39519.702101.1
50.257 610.5109.39519.56796.4
60.243 79.9439.39518.66292.8
), ArticleFig(id=1239250714938110729, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=EN, label=Tab.3, caption=

Determination of 7，4’-dihydroxyflavone in Zhenghonghua oil

, figureFileSmall=null, figureFileBig=null, tableContent=
编号(No.)批号(batch)含量(content)/(ng·g-1)
A1210531113
A2220604111
A3210608137
A421060194
A521070154
A621070444
A7211026122
A8211027122
A9211028143
A1021103153
A1121110144
A12201228153
A1319041949
A1422041841
A1522051841
A1622051756
A17210407116
A1821070250
A19R210862436
A20R211077406
A21R211297375
A22R211298367
A23R220101387
A24R220201387
A25200413ND
A26210702ND
A27210703ND
A28211203ND
A29220107ND
A30220514ND
), ArticleFig(id=1239250715030385422, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1239250706637582709, language=CN, label=表3, caption=

正红花油样品检出7，4’-二羟基黄酮情况(n=2)

, figureFileSmall=null, figureFileBig=null, tableContent=
编号(No.)批号(batch)含量(content)/(ng·g-1)
A1210531113
A2220604111
A3210608137
A421060194
A521070154
A621070444
A7211026122
A8211027122
A9211028143
A1021103153
A1121110144
A12201228153
A1319041949
A1422041841
A1522051841
A1622051756
A17210407116
A1821070250
A19R210862436
A20R211077406
A21R211297375
A22R211298367
A23R220101387
A24R220201387
A25200413ND
A26210702ND
A27210703ND
A28211203ND
A29220107ND
A30220514ND
)], attaches=null, journal=Journal(id=1205114436974182403, delFlag=0, nameCn=药物分析杂志, nameEn=Chinese Journal of Pharmaceutical Analysis, nameHistory1=null, nameHistory2=null, issn=0254-1793, eissn=, cn=11-2224/R, coden=null, periodic=月刊, language=CN, oaType=1, ccby=null, superviseOffice=null, ownerOffice=null, pubOffice=null, editorOffice=null, officeType=null, aims=null, clcCode=null, officeProv=null, officeCity=null, officeAddr=null, officeZip=null, officeEmail=, officePhone=, editDirector=null, officeDirector=null, officeDirectorPhone=null, officeStaffNum=null, officeEmpNum=null, coverPicUrl=E+iq5BU+frOtpo6YF6JpQQ==, journalPrice=null, startedYear=null, abbrevIsoEn=Chinese Journal of Pharmaceutical Analysis, journalRemark=null, publicationField=null, createdTime=1765251271721, updatedTime=1765252167692, createdBy=18614031015, updatedBy=13701087609, firstLetterCn=C, firstLetterEn=C, subjectCode=Life Sciences, subjectName=生命医学, subjectCodeEn=Life Sciences, subjectNameEn=null, picCn=E+iq5BU+frOtpo6YF6JpQQ==, picEn=n/3T/+AptjYTGmmMsE/a0Q==, jcr=null, cjcr=null, exts=[JournalExt(id=1205118195070906572, language=CN, name=药物分析杂志, nameHistory1=null, nameHistory2=null, managedBy=, sponsoredBy=, publishedBy=, editorOffice=, officeProv=null, officeCity=null, officeAddr=, officeZip=, editDirector=, officeDirector=null, officePhone=null, coverPicUrl=null, journalRemark=, submitArticleUrl=null, websiteUrl=, createdTime=1765252167718, updatedTime=1765252167718, createdBy=13701087609, updatedBy=13701087609, submissionGuidelinesUrl=, submissionAuthorUrl=https://ywfxauthor.manuscriptcloud.com/login, submissionEditorUrl=https://ywfxeditor.manuscriptcloud.com/login, submissionReviewUrl=https://ywfxauthor.manuscriptcloud.com/login, submissionCeEditorUrl=, submissionAeEditorUrl=, option={"copyright":""}), JournalExt(id=1205118195133821133, language=EN, name=Chinese Journal of Pharmaceutical Analysis, nameHistory1=null, nameHistory2=null, managedBy=, sponsoredBy=, publishedBy=, editorOffice=, officeProv=null, officeCity=null, officeAddr=, officeZip=, editDirector=, officeDirector=null, officePhone=null, coverPicUrl=null, journalRemark=, submitArticleUrl=null, websiteUrl=, createdTime=1765252167733, updatedTime=1765252167733, createdBy=13701087609, updatedBy=13701087609, submissionGuidelinesUrl=, submissionAuthorUrl=https://ywfxauthor.manuscriptcloud.com/login, submissionEditorUrl=https://ywfxeditor.manuscriptcloud.com/login, submissionReviewUrl=https://ywfxauthor.manuscriptcloud.com/login, submissionCeEditorUrl=, submissionAeEditorUrl=, option={"copyright":""})], databaseList=null, tenantJournalId=1205117023404326918, websiteList=[Website(id=1205118568045195478, webName=null, webTitle=null, webDomain=null, webCopyrigh=null, webIpcNo=null, seoTitle=null, seoKeywords=null, seoDescription=null, tenantJournalId=null, journalId=1205117023404326918, journalNameCn=null, journalNameEn=null, grayFlag=null, tenantId=1146029695717560320, platformId=null, journalGroupId=null, journalGroupNameCn=null, journalGroupNameEn=null, type=1, domain=https://castjournals.cast.org.cn/joweb/ywfxzz/CN, language=CN, createTime=1765252256642, createBy=18614031015, updateTime=1765252521924, updateBy=18614031015, name=药物分析杂志-中文, tplId=1146099689490845704, title=药物分析杂志, delFlag=0, indexPage=/home, props=[WebsiteProps(id=1205154326156128935, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=articleTextType, value=kx, createTime=1765260782040, updateTime=1765260782040, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326135157412, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=banner, value=null, createTime=1765260782035, updateTime=1765260782035, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326172906154, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=grayFlag, value=0, createTime=1765260782044, updateTime=1765260782044, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326126768803, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=logo, value=https://castjournals.cast.org.cn/joweb/ywfxzz/CN/file/pic?fileId=5+7UKv7ckvsJ8AsWJeRI6g==, createTime=1765260782033, updateTime=1765260782033, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326181294764, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=minRunFlag, value=0, createTime=1765260782046, updateTime=1765260782046, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326147740326, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=picServerUrl, value=https://castjournals.cast.org.cn/joweb/ywfxzz/CN/file/pic, createTime=1765260782038, updateTime=1765260782038, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326177100459, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=silenceFlag, value=0, createTime=1765260782045, updateTime=1765260782045, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326143546021, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=staticResourcePath, value=https://castjournals.cast.org.cn/joweb/cast_kjdb_cn_619/, createTime=1765260782037, updateTime=1765260782037, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326160323240, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=themeColor, value=null, createTime=1765260782041, updateTime=1765260782041, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154326164517545, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568045195478, code=themeStyle, value=null, createTime=1765260782042, updateTime=1765260782042, creator=18614031015, updator=18614031015)]), Website(id=1205118568124887259, webName=null, webTitle=null, webDomain=null, webCopyrigh=null, webIpcNo=null, seoTitle=null, seoKeywords=null, seoDescription=null, tenantJournalId=null, journalId=1205117023404326918, journalNameCn=null, journalNameEn=null, grayFlag=null, tenantId=1146029695717560320, platformId=null, journalGroupId=null, journalGroupNameCn=null, journalGroupNameEn=null, type=1, domain=https://castjournals.cast.org.cn/joweb/ywfxzz/EN, language=EN, createTime=1765252256661, createBy=18614031015, updateTime=1765252537379, updateBy=18614031015, name=药物分析杂志-英文, tplId=1146101810881728533, title=Chinese Journal of Pharmaceutical Analysis, delFlag=0, indexPage=/home, props=[WebsiteProps(id=1205154361170174338, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=articleTextType, value=kx, createTime=1765260790388, updateTime=1765260790388, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361145008511, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=banner, value=null, createTime=1765260790382, updateTime=1765260790382, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361195340165, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=grayFlag, value=0, createTime=1765260790394, updateTime=1765260790394, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361132425598, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=logo, value=https://castjournals.cast.org.cn/joweb/ywfxzz/EN/file/pic?fileId=5+7UKv7ckvsJ8AsWJeRI6g==, createTime=1765260790379, updateTime=1765260790379, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361207923079, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=minRunFlag, value=0, createTime=1765260790397, updateTime=1765260790397, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361157591425, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=picServerUrl, value=https://castjournals.cast.org.cn/joweb/ywfxzz/EN/file/pic, createTime=1765260790385, updateTime=1765260790385, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361199534470, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=silenceFlag, value=0, createTime=1765260790396, updateTime=1765260790396, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361149202816, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=staticResourcePath, value=https://castjournals.cast.org.cn/joweb/cast_kjdb_en_623/, createTime=1765260790383, updateTime=1765260790383, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361174368643, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=themeColor, value=null, createTime=1765260790389, updateTime=1765260790389, creator=18614031015, updator=18614031015), WebsiteProps(id=1205154361186951556, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1205118568124887259, code=themeStyle, value=null, createTime=1765260790392, updateTime=1765260790392, creator=18614031015, updator=18614031015)])], journalTitle=药物分析杂志, weixinUrl=null, journalUrl=null, iacademicId=null, status=1, seqNo=null, journalTitleEn=Chinese Journal of Pharmaceutical Analysis, journalPhotoCn=E+iq5BU+frOtpo6YF6JpQQ==, journalPhotoEn=n/3T/+AptjYTGmmMsE/a0Q==, journalFirstLetter=C, journalRecommend=null, journalNew=null, journalCollection=null, jcrJf=null, cjcrJf=null, jcrJfStr=null, cjcrJfStr=null, submissionFirstDecision=null, sciSubjectClassification=null, casSubjectClassification=null, citeScore=null, totalCitationFrequency=null, icpCode=null, psCode=null, advertisingLicenseCode=null, copyrightInformation=null, country=null, option=, provinceCode=null, provinceName=null, collectFlag=false), detailUrlCn=https://castjournals.cast.org.cn/joweb/ywfxzz/CN/10.16155/j.0254-1793.2024.04.09, detailUrlEn=https://castjournals.cast.org.cn/joweb/ywfxzz/EN/10.16155/j.0254-1793.2024.04.09, pdfUrlCn=https://castjournals.cast.org.cn/joweb/ywfxzz/CN/PDF/10.16155/j.0254-1793.2024.04.09, pdfUrlEn=https://castjournals.cast.org.cn/joweb/ywfxzz/EN/PDF/10.16155/j.0254-1793.2024.04.09, aliStartDate=null, aliEndDate=null, collectionFlag=false, citedCount=null, citedUrl=null, reference=null)
收藏切换
正红花油中血竭掺伪龙血竭检查方法的研究*
收藏切换
PDF下载
刘岩庭 , 陈在敏 ** , 王勇 **
药物分析杂志 | 安全监测 2024,44(4): 620-627
收起
收藏切换
药物分析杂志 | 安全监测 2024, 44(4): 620-627
正红花油中血竭掺伪龙血竭检查方法的研究*
全屏
刘岩庭 , 陈在敏** , 王勇**
作者信息
  • 福建省食品药品质量检验研究院，福州 350012

    • Tel：18805903391；E-mail：

通讯作者:

** 陈在敏　Tel：(0591)87671677；E-mail：
王勇　Tel：18959193539；E-mail：
Research on the detection method of Draconis Sanguis adulterated Resina Draconis in Zhenghonghua oil*
Yan-ting LIU , Zai-min CHEN** , Yong WANG**
Affiliations
  • Fujian Institute for Food and Drug Quality Control, Fuzhou 350012, China
出版时间: 2024-04-30 doi: 10.16155/j.0254-1793.2024.04.09
文章导航
收藏切换
摘要
收起
目的：

建立正红花油中血竭掺伪的检测方法。

方法：

以7，4’-二羟基黄酮为指标建立薄层色谱(TLC)法，快速筛查正红花油中掺伪的龙血竭。TLC筛查出可疑样品，用超高效液相色谱串联质谱(UPLC-MS/MS)法进行确证并定量分析，采用SuperLu C18(2)(100 mm×2.1 mm，1.8 μm)色谱柱，以乙腈-水(25∶75)为流动相，流速0.3 mL·min-1，柱温25 ℃，选择m/z 253.1→117.1(定量)和m/z 253.1→91.0(定性)作为7，4’-二羟基黄酮检测离子对。

结果：

TLC方法专属性、耐用性良好。采用UPLC-MS/MS法，7，4’-二羟基黄酮质量浓度在0.470~37.58 ng·mL-1范围内线性良好(r=0.999 7)，加样平均回收率(n=6)为96.1%，RSD为3.2%。对30批正红花油进行薄层初筛，结果有24批疑似检出7，4’-二羟基黄酮。疑似样品通过UPLC-MS/MS验证，有24批正红花油超出拟定的限度，验证结果与TLC方法一致。

结论：

本方法快速，结果准确，灵敏度高，可用于正红花油中掺伪龙血竭筛查与分析。

正红花油  /  7，4’-二羟基黄酮  /  掺伪  /  血竭  /  龙血竭  /  薄层色谱法  /  超高效液相-质谱联用
Objective:

To establish a screening method for the detection of adulteration of Draconis Sanguis in Zhenghonghua oil.

Methods:

To establish a thin layer chromatography (TLC) method with 7, 4’-dihydroxyflavone as an index for fast screen of the adulteration in Zhenghonghua oil. The suspected samples were screened by TLC and the quantification was performed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The chromatographic column was SuperLu C18 (2)(100 mm×2.1 mm, 1.8 μm), the mobile phase was acetonitrile-water (25∶75) at a flow rate of 0.3 mL·min-1 and the column temperature was 25 ℃. The detection ion pairs for 7, 4’-dihydroxyflavone were m/z 253.1→117.1 (quantitative) and m/z 253.1→91.0 (qualitative).

Results:

TLC method was specific and durable. The linear range of 7, 4’-dihydroxyflavone was 0.470-37.58 ng·mL-1 (r=0.999 7) by UPLC-MS/MS. The average recovery rate(n=6) was 96.1% and RSD was 3.2%. Thirty batches of Zhenghonghua oil were screened by TLC, and 24 batches were suspected to have 7, 4’-dihydroxyflavone. The suspected samples were verified by UPLC-MS/MS, 24 batches of Zhenghonghua oil exceeded the proposed limit, and the verification results were consistent with TLC method.

Conclusion:

This method is rapid, accurate and can be used for the screening and analysis of adulterated Zhenghonghua oil.

Zhenghonghua oil  /  7，4’-dihydroxyflavone  /  adulteration  /  Draconis Sanguis  /  Resina Draconis  /  TLC  /  UPLC-MS/MS
刘岩庭, 陈在敏, 王勇. 正红花油中血竭掺伪龙血竭检查方法的研究*. 药物分析杂志, 2024 , 44 (4) : 620 -627 . DOI: 10.16155/j.0254-1793.2024.04.09
Yan-ting LIU, Zai-min CHEN, Yong WANG. Research on the detection method of Draconis Sanguis adulterated Resina Draconis in Zhenghonghua oil*[J]. Chinese Journal of Pharmaceutical Analysis, 2024 , 44 (4) : 620 -627 . DOI: 10.16155/j.0254-1793.2024.04.09
正文
收起
正红花油是由血竭、水杨酸甲酯等多味药物组成的常用搽剂，能够起到消炎消肿、止血止痛的作用，常用于风湿、腰背酸痛、跌打扭伤、水火烫伤等。血竭在正红花油处方中是一味关键药味，其主要功效有活血化瘀、止血止痛、生肌[1]，常用于外科软组织损伤、出血以及伤口经久不愈合的治疗，还可以用于淤血引起的心腹疼痛等。血竭主产地为东南亚等国，因其价格昂贵，市场上存在血竭中掺龙血竭、树脂、松香以及非法添加人工色素等现象[2-4]。血竭最常见的掺伪品是龙血竭，张明童等[5]对血竭药材掺伪龙血竭进行定性鉴别、定量计算，结果血竭中掺龙血竭检出率高达55.6%。薛恒跃等[6]对含血竭的4种中成药中掺龙血竭进行研究，结果4种含血竭中成药掺龙血竭检出率有31.58%。该研究只涉及极少数品种、部分剂型，尚未涉及基质复杂的含血竭制剂如正红花油等，目前尚无正红花油中血竭掺伪的研究，基于此，有必要建立筛查正红花油中血竭掺伪龙血竭的方法。
血竭与龙血竭来源不同，二者的化学成分差异较大，血竭特征性成分有血竭素等，龙血竭特征性成分有7，4’-二羟基黄酮、龙血素A、龙血素B等[7-12]。文献对血竭及含血竭的部分中成药中是否掺伪通过薄层色谱法，均用龙血竭对照药材进行判定，但是含血竭的中成药成分复杂，干扰多，采用龙血竭对照药材建立薄层色谱方法筛查，容易出现判定困难，需选用特征性成分为指标进行掺伪研究。龙血素A、龙血素B在紫外光灯(254、365 nm)下无明显荧光，通用显色剂硫酸乙醇、磷钼酸乙醇等加热后可显色，但需较高浓度方能显色清晰，灵敏度低，无法以此2个成分为检测指标建立薄层色谱法对正红花油中血竭掺伪龙血竭进行初筛。低浓度7，4’-二羟基黄酮在紫外光灯(365 nm)下有很强的蓝色荧光，基于此，本文选用龙血竭特征性成分7，4’-二羟基黄酮作为正红花油掺伪检测指标，建立薄层色谱法进行筛查，该方法快速，灵敏度高，操作简单，能够快速筛查出可疑样品。对薄层色谱筛查出的可疑样品进行验证，最终采用超高效液相色谱-三重四极杆质谱联用法对样品进行确证并定量。
1　仪器与试药
收起
1.1　仪器
卡玛自动点样仪，薄层色谱数码成像系统(CAMAG公司)；UPLC-Q Exactive Orbitrap超高效液相色谱-高分辨质谱联用仪(赛默飞公司)，AB Sciex Triple QuadTM 5500系列高效液相色谱-三重四极杆质谱联用仪，配有Analyst、Sciex OS工作站(爱博才思公司)；XR105十万分之一天平(梅特勒公司)，BS224万分之一天平(赛多利斯公司)；KQ-500VDE超声波清洗器(昆山市超声仪器有限公司)；Milli-Q IQ7000超纯水机(密理博公司)。
1.2　试药
血竭对照药材(批号120906-201611)、龙血竭对照药材(批号121252-201303)、7，4’-二羟基黄酮对照品(批号111787-201002，含量以98.6%计)均购于中国食品药品检定研究院。乙腈为色谱纯，水为超纯水机制备，其他试剂均为分析纯。
1.3　样品
正红花油样品共30批(编号为A1~A30)，其中18批样品来自于生产企业，其余12批样品来自于省级监督抽检及市场收集。收集到10批血竭(Draconis Sanguis)和10批龙血竭(Resina Draconis)，经福建省食品药品质量检验研究院金鸣主任药师鉴定为正品。
缺血竭阴性样品：除不加血竭外，按规定的处方量及工艺制得。标准制剂样品：按照规定的处方量及工艺自制的正红花油。阳性样品：以龙血竭替代血竭投料，按照规定的处方量和工艺自制的阳性样品。
2　方法与结果
收起
2.1　薄层色谱法
2.1.1　对照药材溶液制备
取血竭及龙血竭的对照药材各约20 mg，分别置具塞锥形瓶中，加甲醇10 mL，超声(250 W，45 kHz)处理20 min，滤过，即得。
2.1.2　对照品溶液的制备
取7，4’-二羟基黄酮对照品适量，加甲醇制成质量浓度为1 mL约含0.2 μg的溶液，即得。
2.1.3　检测方法
照2020年版《中华人民共和国药典》薄层色谱法(通则0502)试验，吸取正红花油样品20 μL与对照品溶液10 μL，分别点于同一硅胶G薄层色谱板上，先以石油醚(60~90 ℃)-乙酸乙酯(17∶3)为展开剂，展至约6~8 cm，取出，晾干，再以二氯甲烷-甲醇(15∶1)为展开剂，展至约6~8 cm，取出，晾干，置紫外光灯(365 nm)下检视。
2.1.4　专属性试验
吸取血竭及龙血竭的对照药材溶液、对照品溶液各10 μL及缺血竭阴性样品、阳性样品、标准制剂样品各20 μL，分别点于同一硅胶G薄层色谱板上，按“2.1.3”项方法操作；结果色谱图(图1)中血竭对照药材溶液、标准制剂样品及缺血竭阴性样品在对照品溶液相应的位置上未出现相同颜色的荧光斑点，阳性样品在对照品溶液相应的位置上出现同颜色的荧光斑点，表明7，4’-二羟基黄酮为龙血竭特征性成分，正红花油中其他药味对检测结果无干扰，方法专属性强。
2.1.5　耐用性试验
吸取阳性样品20 μL及对照品溶液10 μL，按“2.1.3”项下方法，采用青岛海洋化工厂硅胶G预制板、默克公司硅胶G预制板、安徽良臣硅源材料有限公司硅胶G预制板进行检测，结果7，4’-二羟基黄酮斑点均清晰可见，分离度良好，耐用性试验满足要求。
2.1.6　检测限测定
量取7，4’-二羟基黄酮对照品溶液(0.756 μg·mL-1)0.02、0.04、0.06、0.08、0.10、0.15 mL分别置2 mL量瓶中，加缺血竭阴性样品至刻度，摇匀，得到6种不同浓度溶液(7，4’-二羟基黄酮的质量浓度分别为7.56、15.12、22.68、30.24、37.80、56.70 ng·mL-1)，吸取上述溶液各20 μL，分别点于同一硅胶G薄层色谱板上，按“2.1.3”项方法操作，结果对照品质量浓度为22.68 ng·mL-1时在紫外灯(365 nm)下检视的斑点清晰可见，则TLC最低检测限浓度为22.68 ng·mL-1。
2.1.7　结果
30批正红花油按“2.1.3”项下方法试验，结果有24批正红花油样品的色谱中，在与7，4’-二羟基黄酮对照品相应的位置上显相同颜色的荧光斑点，见图2。
供试品溶液色谱若在与对照品色谱相应的位置上，显相同颜色的荧光斑点，则采用超高效液相色谱-三重四极杆质谱联用法进行验证。
2.2　UPLC-MS/MS法
2.2.1　色谱-质谱条件
2.2.1.1　色谱条件
采用Super Lu C18(2) (100 mm×2.1 mm，1.8 μm)色谱柱，以乙腈-水(25∶75)为流动相，流速0.3 mL·min-1，柱温25 ℃，进样量5 μL。
2.2.1.2　质谱条件
离子源为ESI，检测模式为负离子模式，多反应监测；雾化温度为550 ℃，碰撞气压力为62.1 kPa，喷雾气压力为379.2 kPa，辅助气压力为379.2 kPa，气帘气压力为206.8 kPa，喷雾电压为-4 500 V。7，4’-二羟基黄酮的质谱参数见表1。
2.2.2　对照品溶液的制备
取7，4’-二羟基黄酮对照品9.53 mg，精密称定，加甲醇制成7，4’-二羟基黄酮质量浓度为1.879 μg·mL-1的对照储备溶液；再用甲醇将储备液稀释至每1 mL含0.8 ng的溶液，即得。
2.2.3　供试品溶液的制备
取样品约0.5 g置烧杯中，精密称定，加环己烷10 mL充分溶解，转移至分液漏斗中，用70%甲醇10 mL充分振摇提取2次，合并70%甲醇液，再用环己烷5 mL洗涤，弃去环己烷液，收集70%甲醇液，蒸干，残渣加甲醇溶解，转移至25 mL量瓶中，加甲醇稀释至刻度，摇匀，过0.22 μm滤膜，即得。
2.2.4　基质效应考察
正红花油基质复杂，净化后可能还存在基质效应，有必要考察基质效应。以标准制剂样品按“2.2.3”项下方法制备得到基质溶液，精密量取储备液适量，用基质溶液与甲醇分别配制成0.940、4.70、18.79 ng·mL-1的对照品溶液，按“2.2.1”项下条件进样测定，记录峰面积，计算基质效应，结果以上3种浓度的对照品基质效应分别为100.1%、100.3%、100.7%，说明净化后消除了基质效应。
2.2.5　线性关系考察及定量限、检测限测定
取对照品储备液适量，用甲醇稀释成每1 mL含7，4’-二羟基黄酮为0.470、0.940、1.879、4.70、9.40、18.79、37.58 ng的系列对照品溶液，按“2.2.1”项下条件进样测定，记录峰面积。以浓度(X，ng·mL-1)为横坐标，峰面积(Y)为纵坐标，绘制标准曲线并进行线性回归，回归方程为
线性范围为0.470~37.58 ng·mL-1。
将对照品溶液稀释至质量浓度为0.094 ng·mL-1时，S/N≥10，则此质量浓度为定量限浓度，方法定量限为4.7 ng·g-1；质量浓度为0.031 ng·mL-1时，S/N≥3，则此质量浓度为检测限浓度，方法检测限1.55 ng·g-1。
2.2.6　专属性试验
取缺血竭阴性样品、阳性样品、标准制剂样品，分别按“2.2.3”项下方法制备相应的供试溶液。
取上述3种供试溶液及对照品溶液(9.40 ng·mL-1)按“2.2.1”项下条件，进样测定。结果在色谱图中，缺血竭阴性样品及标准制剂样品的供试溶液在与对照品溶液相应的保留时间处未出现相应的离子峰；阳性样品的供试溶液在与对照品溶液相应的保留时间处出现色谱峰，详见图3，表明正红花油中其他药味对检测结果无干扰，方法专属性强。
2.2.7　精密度试验
取同一对照品溶液(7，4’-二羟基黄酮质量浓度为1.879 ng·mL-1)，按“2.2.1”项下条件连续进样6次，测得7，4’-二羟基黄酮峰面积的RSD为0.71%，表明仪器精密度良好。
2.2.8　重复性试验
分别取正红花油样品(批号220418)6份，各约0.5 g，精密称定，按“2.2.3”方法制备供试品溶液，按“2.2.1”项下条件进样测定，结果7，4’-二羟基黄酮的平均含量(n=6)为40.8 ng·g-1，RSD为3.7%，表明重复性良好。
2.2.9　稳定性试验
取同一份供试品溶液(样品批号220418)，在溶液制备后0、3、6、9、12、24 h进行测定，结果7，4’-二羟基黄酮峰面积的RSD为2.4%，表明供试品溶液稳定性良好。
2.2.10　回收率试验
取正红花油样品(批号220418)6份，各约0.25 g，精密称定，分别精密加入质量浓度为18.79 ng·mL-1的对照品溶液0.5 mL，按“2.2.3”项下方法制备供试溶液，按“2.2.1”项下条件进样测定，结果平均回收率为96.1%(RSD=3.2%)，结果见表2。
2.2.11　限度拟定
血竭、龙血竭二者产地不同，来源不同，价格差异悬殊，存在着掺杂掺假的风险，照2020年版《中华人民共和国药典》四部药材和饮片检定通则规定药屑及杂质不得超过3%，作为血竭中掺入龙血竭的限度。按照龙血竭掺伪3%的比例，按正红花油制法制备10批正红花油掺伪样品，按“2.2.3”项方法制备供试溶液，按“2.2.1”项下条件进行测定，结果掺伪样品中7，4’-二羟基黄酮平均含量为41 ng·g-1。故暂定7，4’-二羟基黄酮限度为不得过40 ng·g-1，折算对应7，4’-二羟基黄酮对照品浓度为0.8 ng·mL-1作为限度。判定依据：以m/z 253.1→117.1和m/z 253.1→91.0提取的样品离子流色谱中，应不得同时出现与7，4’-二羟基黄酮对照品保留时间一致的色谱峰；若同时出现，则样品色谱中m/z 253.1→117.1的色谱峰面积不得大于对照品色谱峰面积。
2.2.12　样品测定
30批正红花油样品分别按“2.2.3”项方法供试品溶液，按“2.2.1”项下条件进样测定，结果有24批检出7，4’-二羟基黄酮，具体结果见表3。
本研究收集到A、B、C 3个厂家生产的正红花油共30批，其中A厂家有18批，其余2家均为6批，按本研究拟定结果有A、B 2个厂家生产的共24批正红花油全部检出龙血竭成分，存在掺伪问题。
3　讨论
收起
3.1　龙血竭特征性成分发现与鉴定
取血竭、龙血竭药材粉末各约0.1 g，置具塞锥形瓶中，加甲醇50 mL，超声处理(功率250 W，频率45 kHz)15 min，滤过，取续滤液作为供试品溶液，另取血竭、龙血竭对照药材各约0.1 g，同法制成对照药材溶液。照2020年版《中华人民共和国药典》薄层色谱法(通则0502)试验，吸取上述供试品溶液与2种对照药材溶液各5 μL，分别点于同一硅胶G薄层色谱板上，以二氯甲烷-甲醇(15∶1)为展开剂，展开，取出，晾干，置紫外光灯(365 nm)下检视。发现龙血竭、龙血竭对照药材溶液色谱中，在比移值约0.3位置均出现蓝色荧光斑点，血竭、血竭对照药材溶液均无此斑点，专属性良好，该斑点为龙血竭特征性成分，结果见图4。通过对龙血竭对照药材溶液进行分离、纯化，使用UPLC-Q Exactive Orbitrap超高效液相色谱-高分辨质谱联用仪进行负离子扫描，出现准分子离子峰m/z 253.051 0，与文献报道[13]的7，4’-二羟基黄酮准分子离子峰一致，再与7，4’-二羟基黄酮对照品进行比较，二者保留时间，一级质谱和二级质谱母离子及碎片离子均一致，确定该特征性成分为7，4’-二羟基黄酮。
3.2　检测指标成分的选择
7，4’-二羟基黄酮在紫外光(365 nm)下有很强的蓝色荧光，可用于薄层色谱初筛。血竭中掺伪龙血竭的研究多采用龙血素A、龙血素B作为检测指标，因灵敏度问题，无法以此2个成分建立薄层色谱法对正红花油进行初筛。龙血竭药材中7，4’-二羟基黄酮的含量与龙血素A、龙血素B的含量相当或略低[14-17]，但在薄层色谱有很高的灵敏度，方法快捷，操作简单，另从对照品成本的角度考虑，选用7，4’-二羟基黄酮可以节约成本，更加经济，具有优异性，适用于生产企业、基层单位推广使用。
3.3　薄层色谱展开剂的选择
正红花油含有大量的水杨酸甲酯等油性基质，一次展开容易造成斑点条带不平，错位等现象，影响结果的判定。故采用二次展开的方式，先用低极性的展开剂把油性基质展开，此时目标斑点在原点，再用极性较大的展开剂把目标斑点展开。通过考察，石油醚(60~90 ℃)-乙酸乙酯(85∶15)能把水杨酸甲酯等大量干扰物展至前沿，此时目标斑点依旧在原点，二次展开剂考察了三氯甲烷-甲醇(20∶1)、二氯甲烷-甲醇(20∶1)、二氯甲烷-甲醇(15∶1)、乙酸乙酯-无水乙醇(20∶1)等，最终确定二氯甲烷-甲醇(15∶1)为二次展开剂，特征斑点清晰，分离度良好。
3.4　样品的净化方式考察
正红花油基质主要为挥发油类成分，直接稀释进样，不仅容易损坏色谱柱，还损坏仪器。正红花油低极性成分多，不溶于水，故未考察反相吸附剂固相萃取。考察正相吸附剂中性氧化铝、硅胶、PSA、NH2进行固相萃取，回收率达不到要求。
尝试QuECHRS法对样品进行净化，因正相材料对目标化合物吸附严重，故未予以考虑。考察的净化材料有石墨化碳黑(GCB)、多壁碳纳米管、活性炭、C18，结果前3种材料均能较好地除去色素，但是对7，4’-二羟基黄酮吸附严重，C18净化效果不佳。
最终选用萃取法对正红花油样品进行净化。样品加一定量环己烷溶解后再加甲醇萃取，当萃取第2次时样品不分层。故改用含水甲醇溶液萃取，并比较了不同浓度的甲醇萃取效果，结果70%甲醇萃取效果最佳，萃取2次已经萃取完全。
3.5　限度拟定
现行正红花油质量标准中未对处方中血竭进行质量控制，生产企业可能少投血竭或者投掺伪的血竭，存在着产品质量风险。收集到A厂家近年来投料用的3批血竭药材，研究发现均存在掺龙血竭的现象。本次研究收集的龙血竭只有10批，且B、C厂家的正红花油批数较少，故只是初步拟定7，4’-二羟基黄酮限度，在今后研究中收集更多批次龙血竭及正红花油样品，积累更多的数据再验证。
本试验所建立的方法操作简单，灵敏度高，专属性强，能够准确判定正红花油中是否存在血竭掺龙血竭的问题，可为正红花油质量控制提供技术支撑。
基金
收起
  • *福建省科技计划项目(2020Y0073)
  • 国家药典委员会标准提高项目(2020Z007)
文献
收起
参考文献 引证文献
排序方式：
[1]
中华人民共和国药典2020年版. 一部[S]. 2020：149
ChP 2020. Vol Ⅰ[S]. 2020：149
[2]
赵江红. 高效液相色谱法鉴定29批血竭中非法添加的3种化学成分[J]. 中医研究，2011，24(8)：17
ZHAO JH. Identification of three chemical components illegally added in 29 batches of Draconis Sanguis by high performance liquid chromatography[J]. Tradit Chin Med Res，2011，24(8)：17
[3]
冼小敏，林蔚文，陈伟康，等. HPLC-DAD法测定血竭饮片中添加苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ及808猩红[J]. 药物分析杂志，2020，40(5)：865
XIAN XM，LIN WW，CHEN WK，et al. Determination of Sudan scarlet added in Draconis Sanguis by HPLC-DAD[J]. Chin J Pharm Anal，2020，40(5)：865
[4]
廖嘉宝，张鹏，谭沛，等. 利用红外光谱法快速测定血竭中掺假松香的含量[J]. 浙江中医杂志，2019，54(9)：695
LIAO JB，ZHANG P，TAN P，et al. The content of adulterated rosin in Draconis Sanguis was rapidly determined by infrared spectroscopy[J]. Zhejiang J Tradit Chin Med，2019，54(9)：695
[5]
张明童，刘志荣，李冬华，等. 薄层色谱法和高效液相色谱法鉴别掺伪龙血竭的血竭[J]. 理化检验-化学分册，2020，56(12)：1267
ZHANG MT，LIU ZR，LI DH，et al. Identification of Draconis Sanguis adulterated with Resina Draconis by thin layer chromatography and HPLC[J]. Phys Test Chem Anal Part B：Chem Anal，2020，56(12)：1267
[6]
薛恒跃，邹亮，秦峥. 含血竭中成药中掺杂龙血竭的鉴别研究[J]. 世界最新医学信息文摘，2019，19(66)：36
XUE HY，ZOU L，QIN Z. Identification study of Resina Draconis mixed into traditional Chinese medicine containing Draconis Sanguis[J]. World Latest Med Inf，2019，19(66)：36
[7]
张丽，王绪平，黄孝闻，等. 血竭及龙血竭化学成分、药理作用研究进展[J]. 中国现代应用药学，2019，36(20)：2605
ZHANG L，WANG XP，HUANG XW，et al. Advance of the chemical components and pharmacological effects of Draconis Sanguis and Resina Draconis[J]. Chin J Mod Appl Pharm，2019，36(20)：2605
[8]
林忆龙，文亦磊，黄洪，等. 龙血竭化学成分及药理作用研究进展[J]. 中国民族民间医药，2020，29(6)：50
LIN YL，WEN YL，HUANG H，et al. Chemical constituents and pharmacological research of the Resina Draconis[J]. Chin J Ethnomed Ethnopharm，2020，29(6)：50
[9]
屠鹏飞，陶晶，胡迎庆，等. 龙血竭黄酮类成分研究[J]. 中国天然药物，2003，1(1)：27
TU PF，TAO J，HU YQ，et al. Flavones from wood Dracaena conchinensis[J]. Chin J Nat Med，2003，1(1)：27
[10]
李云，萧伟，秦建平，等. HPLC测定龙血竭提取物中龙血素A，B和7，4’-二羟基黄酮的含量[J]. 中国实验方剂学杂志，2012，18(3)：45
LI Y，XIAO W，QIN JP，et al. Determination of loureirin A，B and 7，4’-dihydroxy flavone in extract of Resina Draconis by HPLC[J]. Chin J Exp Tradit Med，2012，18(3)：45
[11]
江立，孙成逊，田雪丽，等. 龙血竭片中3种成分体外溶出度的测定[J]. 中成药，2022，44(4)：1058
JIANG L，SUN CX，TIAN XL，et al. Determination of in vitro dissolution rates of three constituents in Longxuejie tablets[J]. Chin Tradit Pat Med，2022，44(4)：1058
[12]
秦建平，吴建雄，李艳静，等. DART/Q-TOF-MS快速鉴定龙血竭中5个酚酸类成分[J]. 药物分析杂志，2014，34(5)：819
QIN JP，WU JX，LI YJ，et al. Rapid identification and characterization of five phenolic compounds in Resina Draconis by DART/Q-TOF-MS[J]. Chin J Pharm Anal，2014，34(5)：819
[13]
李云，萧伟，秦建平，等. HPLC同时测定龙血竭及其提取物中5个有效成分的含量[J]. 中国中药杂志，2012，37(7)：929
LI Y，XIAO W，QIN JP，et al. Simultaneous determination of five active components in Resina Draconis and its extract by HPLC[J]. China J Chin Mater Med，2012，37(7)：929
[14]
秦建平，吴建雄，李家春，等. 不同产地龙血竭中5种成分的HPLC法测定[J]. 现代药物与临床，2013，28(4)：547
QIN JP，WU JX，LI JC，et al. Determination of five components in Draconis Resina from different habitats by HPLC[J]. Drugs Clin，2013，28(4)：547
[15]
万青，王文清，方建国，等. 一测多评法测定龙血竭中5种有效成分[J]. 中草药，2017，48(21)：4541
WAN Q，WANG WQ，FANG JG，et al. Determination of five active components in Draconis Resina by QAMS method[J]. Chin Tradit Herb Drugs，2017，48(21)：4541
[16]
高柳，张晓莉，杨晨，等. 超声波协同半仿生法提取龙血竭中4种成分的工艺研究[J]. 中国药师，2021，24(3)：599
GAO L，ZHANG XL，YANG C，et al. Study on the ultrasonic-assisted semi-bionic extraction technology for 4 components from Resina Draconis[J]. China Pharm，2021，24(3)：599
[17]
林爽，王杰，高珊珊，等. 基于薄层色谱法和超高效液相色谱法对龙血竭的质量评价研究[J]. 中医药导报，2023，29(1)：39
LIN S，WANG J，GAO SS，et al. Study on the quality evaluation of Longxuejie (Resina Draconis) based on TLC and UPLC[J]. Guid J Tradit Chin Med Pharm，2023，29(1)：39
2024年第44卷第4期
PDF下载
82
35
引用本文
BibTeX
文章信息
doi: 10.16155/j.0254-1793.2024.04.09
  • 接收时间：2023-06-19
  • 首发时间：2026-03-13
  • 出版时间：2024-04-30
补充材料
相关文章
文章信息
作者
出版历史
  • 收稿日期：2023-06-19
基金
*福建省科技计划项目(2020Y0073)
国家药典委员会标准提高项目(2020Z007)
作者信息
    福建省食品药品质量检验研究院，福州 350012

通讯作者:

** 陈在敏　Tel：(0591)87671677；E-mail：
王勇　Tel：18959193539；E-mail：
参考文献
分享链接
https://castjournals.cast.org.cn/joweb/ywfxzz/CN/10.16155/j.0254-1793.2024.04.09
分享至
全文二维码

扫描看全文

引用本文
BibTeX
本文的引用情况
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
关闭全屏
相关链接
论文
最新文章
热读文章
热点专题
内参
蓝皮书
产业发展报告
传播力报告
期刊分级目录
资讯
学术新闻
行业新闻
学术会议
行业会议
关于
关于我们
联系我们
北京市海淀区学院南路86号
100081
010-62199257
qkjq@cast.org.cn

中国科学技术协会版权所有 京ICP 备10216604号-4 海淀分局备案 1101084647
科技导报社主办 中国科协信息中心技术支持