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HPLC-MS/MS法检测生物样品中的手性苯丙胺类药物和司来吉兰 | |
其他题名 | Determination of chiral amphetamines and selegiline in biological samples by HPLC-MS/MS method |
汤文川; 王爱华; 任昕昕; 于哲; 常靖; 王瑞花; 王元凤 | |
来源期刊 | 中国法医学杂志
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ISSN | 1001-5728 |
出版年 | 2021 |
卷号 | 36期号:4页码:364-368 |
中文摘要 | 目的建立全血、尿液中手性甲基苯丙胺、手性苯丙胺和司来吉兰同时分析检测的方法。方法全血、尿液经Oasis PRiME MCX固相萃取柱前处理,采用Phenomenex Lux AMP(150*3.0mm,3mum)手性液相色谱柱,以甲醇-5mmol/L碳酸氢铵水溶液(pH=11)为流动相,梯度洗脱,流速为0.35mL/min,以正离子多反应监测(MRM)模式检测,扫描时间21min。结果甲基苯丙胺两种对映异构体、苯丙胺两种对映异构体和司来吉兰在1-500ng/mL的范围内线性关系良好(各物质r2 >0.99);甲基苯丙胺两种对映异构体的检出限为0.05ng/mL,定量限为0.1ng/mL,苯丙胺两种对映异构体和司来吉兰的检出限为0.1ng/mL,定量限为0.5ng/mL;在低(5ng/mL)、中(50ng/mL)、高(200ng/mL)三个添加浓度下,各目标物的绝对回收率和基质效应均在可接受的范围内,日内精密度和日间精密度均小于12.61%。应用该方法对口服司来吉兰的比格犬的血液和尿液进行检测,结果表明仅存在司来吉兰原体、代谢物R-甲基苯丙胺和R-苯丙胺。结论本研究建立了全血、尿液中手性甲基苯丙胺、手性苯丙胺和司来吉兰的HPLCMS/MS定性、定量分析检测方法,该方法操作方便,灵敏度高,可为司法实践中法医毒物鉴定提供一定参考。 |
英文摘要 | Objective To establish a method for simultaneous determination of chiral methamphetamine,chiral amphetamine and selegiline in whole blood and urine.Methods The whole blood and urine samples were treated by Oasis PRiME MCX solid phase extraction column.Phenomenex Lux AMP (150*3.0mm,3mum),a chiral column,was used to analyze.The mobile phase was methanol-5 mmol/L ammonium bicarbonate (pH=11) with gradient elution at a flow rate of 0.35mL/min.The detection was performed in positive ion multiple reaction monitoring (MRM) mode with a scanning time of 21min.Results The linear range of the two enantiomers of methamphetamine,the two enantiomers of amphetamine and selegiline in the blood and urine sample is 1-500ng/mL,and the linear relationship is good (the correlation coefficient of each substance was greater than 0.99).The detection limit of the two enantiomers of methamphetamine was 0.05ng/mL,the limit of quantification was 0.1ng/mL,and the limit of quantification was 0.5 ng/mL.The results showed that the absolute recoveries and matrix effects of each target were within the acceptable range at low (5ng/mL),medium (50ng/mL) and high (200ng/mL),and the intra-day precision and inter-day precision were less than 12.61%.The blood and urine samples of beagle dogs taking selegiline orally were detected by this method.The results showed that there were only selegiline,metabolites R-methamphetamine and R-amphetamine.Conclusion In this study,an HPLC-MS/MS method was established for the qualitative and quantitative analysis of chiral methamphetamine,chiral amphetamine and selegiline in whole blood and urine.The method is sensitive and easy to conduct,which can provide reference for forensic toxicological identification in judicial practice. |
中文关键词 | 法医毒物分析 ; 高效液相色谱-串联质谱法 ; 手性拆分 ; 甲基苯丙胺 ; 苯丙胺 ; 司来吉兰 |
英文关键词 | Forensic toxicological analysis HPLC-MS/MS Chiral separation Methamphetamine Amphetamine Selegiline |
类型 | Article |
语种 | 中文 |
收录类别 | CSCD |
WOS类目 | Government & Law |
CSCD记录号 | CSCD:7034972 |
资源类型 | 期刊论文 |
条目标识符 | http://119.78.100.177/qdio/handle/2XILL650/378073 |
作者单位 | 汤文川, 中国政法大学证据科学研究院, 北京 100088, 中国.; 王元凤, 中国政法大学证据科学研究院, 北京 100088, 中国.; 王爱华, 公安部物证鉴定中心, 北京 100038, 中国.; 任昕昕, 公安部物证鉴定中心, 北京 100038, 中国.; 常靖, 公安部物证鉴定中心, 北京 100038, 中国.; 王瑞花, 公安部物证鉴定中心, 北京 100038, 中国.; 于哲, 中国人民公安大学刑事科学技术学院, 北京 100038, 中国. |
推荐引用方式 GB/T 7714 | 汤文川,王爱华,任昕昕,等. HPLC-MS/MS法检测生物样品中的手性苯丙胺类药物和司来吉兰[J],2021,36(4):364-368. |
APA | 汤文川.,王爱华.,任昕昕.,于哲.,常靖.,...&王元凤.(2021).HPLC-MS/MS法检测生物样品中的手性苯丙胺类药物和司来吉兰.中国法医学杂志,36(4),364-368. |
MLA | 汤文川,et al."HPLC-MS/MS法检测生物样品中的手性苯丙胺类药物和司来吉兰".中国法医学杂志 36.4(2021):364-368. |
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