Article(id=1292130499967869920, tenantId=1146029695717560320, journalId=1246415772164075586, issueId=1292130366320562708, articleNumber=null, orderNo=null, doi=10.13699/j.cnki.1001-6821.2026.07.013, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1772208000000, receivedDateStr=2026-02-28, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1785997517816, onlineDateStr=2026-08-06, pubDate=1776355200000, pubDateStr=2026-04-17, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1785997517816, onlineIssueDateStr=2026-08-06, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1785997517816, creator=13701087609, updateTime=1785997517816, updator=13701087609, issue=Issue{id=1292130366320562708, tenantId=1146029695717560320, journalId=1246415772164075586, year='2026', volume='42', issue='7', pageStart='901', pageEnd='1050', issueExtLink='null', onlineDate='null', pubDate='1776355200000', pubDateStr='2026-04-17', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1785997485952, creator='13701087609', updateTime=1786014433453, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1292201449350516861, tenantId=1146029695717560320, journalId=1246415772164075586, issueId=1292130366320562708, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1292201449350516862, tenantId=1146029695717560320, journalId=1246415772164075586, issueId=1292130366320562708, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=982, endPage=989, ext={EN=ArticleExt(id=1292130500173390817, articleId=1292130499967869920, tenantId=1146029695717560320, journalId=1246415772164075586, language=EN, title=Determination of 14 sedative hypnotics and their metabolites in serum and urine by ultra-high performance liquid chromatography-tandem mass spectrometry with isotope dilution, columnId=1246531413395263850, journalTitle=Chinese Journal of Clinical Pharmacology, columnName=Research Method, runingTitle=null, highlight=null, articleAbstract=
Objective To establish an ultra-high performance liquid chromatography-tandem mass spectrometry method for the determination of 14 sedative hypnotics and their metabolites in serum and urine.
Methods Serum or urine samples were treated with acetonitrile to precipitate proteins. Separated on an Agilent EclipsePlus C18 RRHD column, the liquid was eluted with 0.1% formic acid in water and methanol, at a flow rate of 0.30 mL·min-1 and column temperature of 35 ℃. Quantified by the internal standard method, and multiple reaction monitoring (MRM) was performed by electrospray ionization (ESI+). The method was evaluated for specificity, standard curves and limits of quantification, precision and recovery, matrix effects, and stability. This method was applied to test the proficiency testing samples from the 2023 National Medical Emergency Toxicant Detection Laboratory Comparison Program, including qualitative and quantitative test samples for emergency poisoning assessment of sedative-hypnotic drugs in serum.
Results The method demonstrated good specificity, with no cross-interference between the various sedative hypnotics and their metabolites. The linear range of 14 sedative hypnotics and metabolites were 1.00-45.00 μg·L-1, with a correlation coefficient greater than 0.998 2, the detection limit in serum and urine was 0.30 μg·L-1, and the quantification limit was 1.00 μg·L-1. In serum, recovery rates at three spiked levels (10.00, 50.00 and 200.00 μg·L-1) ranged from 85.60% to 105.20%, with relative standard deviations (RSD) between 0.73% and 4.45%. In urine, recovery rates ranged from 88.93% to 108.12%, with relative standard deviations between 0.50% and 6.92%. Fluphenazine hydrochloride and clozapine were identified by this method. The two determined quantitative concentrations of fluphenazine hydrochloride were 339.00 μg·L-1 and 349.00 μg·L-1 , with an average value of 344.00 μg·L-1 and a deviation of 2.90%. The two determined quantitative concentrations of clozapine were 1 668.00 μg·L-1 and 1 707.00 μg·L-1 , with an average value of 1 688.00 μg·L-1 and a deviation of 2.30%. The final feedback result was satisfactory.
Conclusion This method is rapid and accurate, making it suitable for emergency poisoning detection of sedative hypnotics. Its application to the blind sample detection of emergency poisoning cases is satisfactory.
, authors=Chun-yang MENG, Yu-tian WU, Yi-bing ZHOU, Ye LIN, Xue ZHONG, authorsList=Chun-yang MENG, Yu-tian WU, Yi-bing ZHOU, Ye LIN, Xue ZHONG, authorCompany=null, correspAuthors=Xue ZHONG, 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, fund=null), CN=ArticleExt(id=1292130500534100962, articleId=1292130499967869920, tenantId=1146029695717560320, journalId=1246415772164075586, language=CN, title=同位素稀释-UPLC-MS检测血清和尿液中的14种镇静催眠药及代谢物, columnId=1246531413600784769, journalTitle=中国临床药理学杂志, columnName=研究方法, runingTitle=null, highlight=null, articleAbstract=
目的 建立超高效液相色谱串联质谱（UPLC-MS）检测血清和尿液中14种镇静催眠药及代谢物的方法。
方法 用乙腈沉淀蛋白法处理血清或尿液样品，用Agilent EclipsePlus C18 RRHD色谱柱进行色谱分离，流动相为0.1%甲酸水和甲醇，流速为0.30 mL·min-1，柱温为35 ℃，以同位素内标法定量，用电喷雾电离（ESI+）（正离子采集模式）进行多反应监测（MRM）。考察该方法的专属性、标准曲线与定量下限、精密度与回收率、基质效应、稳定性。检测2023年全国中毒医疗应急毒物检测实验室比对样品，血清中镇静催眠药应急中毒考核的定性定量检测样品。
结果 方法的专属性结果良好，各镇静催眠药之间相互无干扰，14种镇静催眠药及代谢物的线性范围在1.00～45.00 μg·L-1，相关系数r均>0.998 2，血清和尿液中检出限（LOD）为0.30 μg·L-1，定量限（LOQ）为1.00 μg·L-1。3个加标水平下（10.00、50.00和200.00 μg·L-1）血清中14种镇静催眠药及代谢物的回收率在85.60%～105.20%之间，相对标准偏差（RSD）为0.73%～4.45%；尿液中14种镇静催眠药及代谢物的回收率在88.93%～108.12%之间，RSD为0.50%～6.92%。检出盐酸氟奋乃静和氯氮平，盐酸氟奋乃静结果检出实测定量分别为339.00 μg·L-1和349.00 μg·L-1，平均值为344.00 μg·L-1，偏差为2.90%；氯氮平结果检出实测定量分别为1 668.00 μg·L-1和1 707.00 μg·L-1，平均值为1 688.00 μg·L-1，偏差为2.30%。
结论 本方法快速准确，适用于镇静催眠药的应急中毒检测，应用此方法对应急中毒盲样检测，考核结果满意。
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孟春杨（1987-），女，副主任技师，主要从事食品药品检验方面的工作和研究
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