移液枪头式固相微萃取-气相色谱-三重四极杆质谱分析尿液中4种苯丙胺类毒品  

Determination of four amphetamines in human urine by pipette tip solid phase microextraction coupled with gas chromatography-triple quadrupole mass spectrometry

作　　者：施家威 周静峰[1] 赵永纲[2] SHI Jiawei;ZHOU Jingfeng;ZHAO Yonggang(Zhejiang Pharmaceutical College,Ningbo,315000,China;Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang Province,Ningbo Municipal Center for Disease Control and Prevention,Ningbo,315010,China)

机构地区：[1]浙江医药高等专科学校,宁波315000 [2]浙江省微量有毒化学物健康风险评估技术研究重点实验室,宁波市疾病预防控制中心,宁波315000

出　　处：《中国药物依赖性杂志》2020年第2期111-116,141,共7页Chinese Journal of Drug Dependence

基　　金：浙江省食品药品监管系统科技计划项目(2019011);宁波市领军和拔尖人才工程。

摘　　要：目的:建立尿液中4种苯丙胺类毒品的移液枪头式固相微萃取-气相色谱-三重四极杆质谱测定方法。方法:尿液中4种苯丙胺类化合物使用C18固相吸取嘴富集,甲醇洗脱,衍生化后,用三重串联四级杆-气相色谱/质谱联用法测定。结果:方法在50-2000 ng/ml内线性良好,相关系数均大于0.99,加标回收率范围为78.9%~112.8%,RSD小于10%,方法的定量限范围为8.4~27.5 ng/ml(10倍信噪比)。结论:该方法灵敏度高、操作简便、省时,适合尿液中4种苯丙胺类毒品的测定。Objective:To develop a method for simultaneous analysis of amphetamines(AMP), methamphetamine(MA), 3,4-methylenedioxyamphetamine(MDA)and 3,4-methylenedioxymethamphetamine(MDMA) in human urine by pipette tip solid phase microextraction coulped with gas chromatography-triple quadrupole mass spectrometry(GC-QqQ-MS/MS). Methods:The target chemicals in samples were extracted and cleaned up by C18 solid phase microextraction, and then eluted with Methanol. The elutant was dried-up under N2 and the residue derivatized with trifluoroacetic anhydride. The derivatives were analyzed by GC-QqQ-MS/MS using internal standard method. Results:The linearity was obtained over the range of 50 ng/ml to 2 000 ng/ml, and the correlation coefficients were all over 0.99, the recoveries were ranged from 78.9% to 112.8 %, the RSDs were less than 10%. The limits of quantification(LOQs) were between 8.4μg/kg to 27.5 μg/kg(Signal/Noise is 10). Conclusion:The method is highly sensitive, easy to operate, time-saving and economic, which can be used for trace analysis of amphetamines in human urine.

关 键 词：尿液 苯丙胺 三重四极杆气相色谱/质谱联用 固相微萃取 

分 类 号：R917[医药卫生—药物分析学]