液相色谱-质谱法测定指纹汗液中咖啡因及其代谢物
LC-MS Determination of Caffeine and Its Major Metabolite in Fingerprint Sweat
摘 要
采用液相色谱-质谱法测定指纹汗液中咖啡因及其代谢物副黄嘌呤的含量.指纹汗液用润湿的滤纸提取后,加入甲醇,在35 ℃下超声3 min.用Thermo Gold ODS C18色谱柱分离,用甲醇与冰乙酸(0.2+99.8)溶液以体积比65比35组成的混合液洗脱,采用正离子模式监测.咖啡因及副黄嘌呤在一定的浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)分别为0.3,1.7 ng·片-1.加标回收率在65.5%~71.3%之间,测定值的相对标准偏差在3.3%~14%之间.指纹汗液中咖啡因的检出时间从服用咖啡因后1 h开始,一直持续到14 h,副黄嘌呤检出时间从服用3 h后持续到14 h.
指纹
汗液
咖啡因
LC-MS
Fingerprint
Sweat
Caffeine
Abstract
LC-MS was applied to the determination of caffeine and its major metabolite paraxanthine in fingerprint sweat. Fingerprint sweat was extracted ultrasonically with methanol from wet filter paper for 3 min at 35 ℃. Thermo Gold ODS C18 column was used as stationary phase,and a mixture of methanol and acetic acid (0.2+99.8) solution (65+35) was used as mobile phase. Positive electrospray ionization was used in the detection. Linear relationships between values of peak area and concentration of caffeine and paraxanthine were kept in definite ranges,with detection limits (3S/N) of 0.3,1.7 ng·片-1,respectively. Values of recovery found by standard addition method were in the range of 65.5%-71.3%,and values of RSD′s in the range of 3.3%-14%. Caffeine in fingerprint sweat could be detected from 1 h to 14 h after taking caffeine,and paraxanthine could be detected from 3 h to 14 h.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201506015
所属栏目 工作简报
基金项目
收稿日期 2014/12/26
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备注张婷(1975-),女,辽宁沈阳人,讲师,博士研究生,主要从事刑事毒物及毒品的研究.
引用该论文: ZHANG Ting,CHEN Xue-guo,YANG Rui-qin,XU Ying-jian. LC-MS Determination of Caffeine and Its Major Metabolite in Fingerprint Sweat[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(6): 795～799
张婷,陈学国,杨瑞琴,许英健. 液相色谱-质谱法测定指纹汗液中咖啡因及其代谢物[J]. 理化检验－化学分册, 2015, 51(6): 795～799
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【2】ALMOG J,GLASNER H. Detection of firearms imprints on hands of suspects: study of the PDT-based field test［J］ J Forensic Sci,1997,42(6):993-996．
【3】BARNES A J,SMITH M L,KACINKO S L,et al. Excretion of methamphetamine and amphetamine in human sweat following controlled oral methamphetamine administration[J]. Clinical Chemistry,2008,54(1):172-180．
【4】SCHWILKE E W,ALLAN J B,SHERRI L K,et al. Opioid disposition in human sweat after controlled oral codeine administration[J]. Clinical Chemistry,2006,52(8):1539-1545．
【5】鹿慧,吴迪,严静,等.LC-MSn法研究曲马多在大鼠尿中的代谢产物[J].药学学报,2011,46(8):968-975．
【6】MCHALE K J,ESPOSITO C,ESPOURTEILLE F.在线富集HTLC/MS/MS分析环境水资源中多种抗生素[J].环境化学,2010,29(6):1195-1197．
【7】王萌烨,向平,严慧,等.液相色谱-串联质谱法测定尿液中的内源性类固醇激素[J].色谱,2008,26(1):10-14．
【8】王学虎,袁敏,张前上,等.液相色谱-质谱法自动筛选常见30种生物碱[J].理化检验-化学分册,2011,47(4):427-430．
【9】李晓雯,沈保华,江峥,等.HPLC-LTQ Orbitrap MS对血液、尿液中精神药品的筛选及确证[J].法医学杂志,2012,28(1):44-48．
【10】贾晶莹,张玉荣,万钧,等.LC-MS/MS法测定尿样中19种滥用药物[J].中国药物依赖性杂志,2008,17(1):36-38．
【11】孟品佳,张翘楚,许莹.毛发毒品分析[M].北京:中国人民公安大学出版社,2001:2-3．
【12】KENJI K,MIYAGUCHI T H. Time-course measurements of tramadol and its metabolites extracted from fingertips after coffee intake: a preliminary study for the detection of drugs from fingerprints[J]. Anal Bioanal Chem,2013,405:3945-3952．
【13】沈敏.法医毒物学手册[M].北京:科学出版社,2012:308-310．
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