高效液相色谱-电喷雾串联质谱法测定人体液中LSD及其代谢物

J Canezin , A Cailleux , A Turcant , A Le Bouil , P Harry , P Allain
{"title":"高效液相色谱-电喷雾串联质谱法测定人体液中LSD及其代谢物","authors":"J Canezin ,&nbsp;A Cailleux ,&nbsp;A Turcant ,&nbsp;A Le Bouil ,&nbsp;P Harry ,&nbsp;P Allain","doi":"10.1016/S0378-4347(01)00386-3","DOIUrl":null,"url":null,"abstract":"<div><p>A liquid chromatographic procedure with electrospray ionization tandem mass spectrometric detection has been developed and validated for LSD and iso-LSD determination. A one-step liquid–liquid extraction on 1 ml blood or urine was used. The lower limit for quantitative determination was 0.02 μg/l for LSD and iso-LSD. The analytical procedure has been applied in two positive cases (case 1: LSD=0.31 μg/l, iso-LSD=0.27 μg/l in plasma and LSD=1.30 μg/l, iso-LSD=0.82 μg/l in urine; case 2: LSD=0.24 μg/l, iso-LSD=0.6 μg/l in urine). LSD metabolism was investigated using MS–MS neutral loss monitoring for the screening of potential metabolites. The main metabolite was 2-oxo-3-hydroxy-LSD (O–H–LSD) present in urine at the concentrations of 2.5 μg/l and 6.6 μg/l, respectively, for case 1 and 2, and was not present in plasma. Nor-LSD was also found in urine at 0.15 and 0.01 μg/l levels. Nor-iso-LSD, lysergic acid ethylamide (LAE), trioxylated-LSD, lysergic acid ethyl-2-hydroxyethylamide (LEO) and 13 and 14-hydroxy-LSD and their glucuronide conjugates were detected in urine using specific MS–MS transitions.</p></div>","PeriodicalId":15463,"journal":{"name":"Journal of Chromatography B: Biomedical Sciences and Applications","volume":null,"pages":null},"PeriodicalIF":0.0000,"publicationDate":"2001-12-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0378-4347(01)00386-3","citationCount":"53","resultStr":"{\"title\":\"Determination of LSD and its metabolites in human biological fluids by high-performance liquid chromatography with electrospray tandem mass spectrometry\",\"authors\":\"J Canezin ,&nbsp;A Cailleux ,&nbsp;A Turcant ,&nbsp;A Le Bouil ,&nbsp;P Harry ,&nbsp;P Allain\",\"doi\":\"10.1016/S0378-4347(01)00386-3\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>A liquid chromatographic procedure with electrospray ionization tandem mass spectrometric detection has been developed and validated for LSD and iso-LSD determination. A one-step liquid–liquid extraction on 1 ml blood or urine was used. The lower limit for quantitative determination was 0.02 μg/l for LSD and iso-LSD. The analytical procedure has been applied in two positive cases (case 1: LSD=0.31 μg/l, iso-LSD=0.27 μg/l in plasma and LSD=1.30 μg/l, iso-LSD=0.82 μg/l in urine; case 2: LSD=0.24 μg/l, iso-LSD=0.6 μg/l in urine). LSD metabolism was investigated using MS–MS neutral loss monitoring for the screening of potential metabolites. The main metabolite was 2-oxo-3-hydroxy-LSD (O–H–LSD) present in urine at the concentrations of 2.5 μg/l and 6.6 μg/l, respectively, for case 1 and 2, and was not present in plasma. Nor-LSD was also found in urine at 0.15 and 0.01 μg/l levels. Nor-iso-LSD, lysergic acid ethylamide (LAE), trioxylated-LSD, lysergic acid ethyl-2-hydroxyethylamide (LEO) and 13 and 14-hydroxy-LSD and their glucuronide conjugates were detected in urine using specific MS–MS transitions.</p></div>\",\"PeriodicalId\":15463,\"journal\":{\"name\":\"Journal of Chromatography B: Biomedical Sciences and Applications\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2001-12-05\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://sci-hub-pdf.com/10.1016/S0378-4347(01)00386-3\",\"citationCount\":\"53\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Chromatography B: Biomedical Sciences and Applications\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0378434701003863\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Chromatography B: Biomedical Sciences and Applications","FirstCategoryId":"1085","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0378434701003863","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 53

摘要

电喷雾电离串联质谱检测的液相色谱方法已经开发并验证了LSD和异LSD的测定。采用1 ml血液或尿液一步液-液萃取法。LSD和异LSD的定量下限为0.02 μg/l。本方法已应用于2例阳性病例(病例1:血浆中LSD=0.31 μg/l, iso-LSD=0.27 μg/l;尿液中LSD=1.30 μg/l, iso-LSD=0.82 μg/l;病例2:尿中LSD=0.24 μg/l, iso-LSD=0.6 μg/l)。采用MS-MS中性损失监测方法研究LSD代谢,筛选潜在代谢物。主要代谢物为2-氧-3-羟基lsd (O-H-LSD),在病例1和病例2中分别以2.5 μg/l和6.6 μg/l的浓度存在于尿液中,而在血浆中不存在。尿液中也发现了0.15和0.01 μg/l的非lsd。采用特异的质谱联用技术检测尿中非异异lsd、麦角酸乙基酰胺(LAE)、三氧化lsd、麦角酸乙基-2-羟乙基酰胺(LEO)、13和14-羟基lsd及其葡萄糖醛酸缀合物。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
查看原文
分享 分享
微信好友 朋友圈 QQ好友 复制链接
本刊更多论文
Determination of LSD and its metabolites in human biological fluids by high-performance liquid chromatography with electrospray tandem mass spectrometry

A liquid chromatographic procedure with electrospray ionization tandem mass spectrometric detection has been developed and validated for LSD and iso-LSD determination. A one-step liquid–liquid extraction on 1 ml blood or urine was used. The lower limit for quantitative determination was 0.02 μg/l for LSD and iso-LSD. The analytical procedure has been applied in two positive cases (case 1: LSD=0.31 μg/l, iso-LSD=0.27 μg/l in plasma and LSD=1.30 μg/l, iso-LSD=0.82 μg/l in urine; case 2: LSD=0.24 μg/l, iso-LSD=0.6 μg/l in urine). LSD metabolism was investigated using MS–MS neutral loss monitoring for the screening of potential metabolites. The main metabolite was 2-oxo-3-hydroxy-LSD (O–H–LSD) present in urine at the concentrations of 2.5 μg/l and 6.6 μg/l, respectively, for case 1 and 2, and was not present in plasma. Nor-LSD was also found in urine at 0.15 and 0.01 μg/l levels. Nor-iso-LSD, lysergic acid ethylamide (LAE), trioxylated-LSD, lysergic acid ethyl-2-hydroxyethylamide (LEO) and 13 and 14-hydroxy-LSD and their glucuronide conjugates were detected in urine using specific MS–MS transitions.

求助全文
通过发布文献求助,成功后即可免费获取论文全文。 去求助
来源期刊
自引率
0.00%
发文量
0
期刊最新文献
News Section Influence of various biological matrices (plasma, blood microdialysate) on chromatographic performance in the determination of β-blockers using an alkyl-diol silica precolumn for sample clean-up Highly sensitive analysis of the antifolate pemetrexed sodium, a new cancer agent, in human plasma and urine by high-performance liquid chromatography. Preliminary application of liquid chromatography–electrospray-ionization mass spectrometry to the detection of 5-methyltetrahydrofolic acid monoglutamate in human plasma Improved high-performance liquid chromatographic method to estimate aminosugars and its application to glycosaminoglycan determination in plasma and serum
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
现在去查看 取消
×
提示
确定
0
微信
客服QQ
Book学术公众号 扫码关注我们
反馈
×
意见反馈
请填写您的意见或建议
请填写您的手机或邮箱
已复制链接
已复制链接
快去分享给好友吧!
我知道了
×
扫码分享
扫码分享
Book学术官方微信
Book学术文献互助
Book学术文献互助群
群 号:481959085
Book学术
文献互助 智能选刊 最新文献 互助须知 联系我们:info@booksci.cn
Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。
Copyright © 2023 Book学术 All rights reserved.
ghs 京公网安备 11010802042870号 京ICP备2023020795号-1