顶空固相微萃取-气相色谱-质谱联用法测定尿液中美沙酮及其主要代谢物
GC-MS with HS-SPME Determination of Methadone and Its Main Metabolite in Urine
摘 要
提出了用顶空固相微萃取-气相色谱-质谱联用法测定尿液中美沙酮及其主要代谢物2-亚乙基-1,5-二甲基-3,3-二苯基吡咯烷(EDDP)的含量.对影响萃取效率的萃取温度、萃取时间、pH以及离子强度等因素进行了试验,并予以优化.在优化的条件下,采用二苯基丙基己酸β-二己基氨基乙酯(SKF525A)为内标,选定m/z 277,m/z 72和m/z 86分别作为EDDP、美沙酮和SKF525A的定量离子,在选择离子监测模式下,美沙酮及EDDP的线性范围均为0.01~1.0 mg·L-1,相对标准偏差(n=5)都小于9.0%,平均回收率分别为104.2%和97.6%.
气相色谱-质谱联用法
美沙酮
EDDP
HS-SPME
GC-MS
Methadone
EDDP
Abstract
GC-MS with HS-SPME was applied to the determination of contents of methadone and its main metabolite EDDP in urine.Influtential factors to extraction efficiency,including extracting time,extracting temperature,pH value,and ionic strength were studied and optimized.SKF525A was used as internal standard,and the ions with m/z 277,72 and 86 was selected as quantitative ions for the determination of EDDP,methadone and SKF525A,respectively.Linearity ranges for both methadone and EDDP were between 0.01-1.0 mg·L-1,with RSD′s (n=5) less than 9.0%.The values of recovery of methadone and EDDP found by standard addition method were 104.2% and 97.6% respectively.
中图分类号 O657.7
所属栏目 工作简报
基金项目 公安部应用创新计划项目资助项目(2007YYCXGXST081)
收稿日期 2008/4/12
修改稿日期
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备注黄克建(1969-),男,广西崇左人,高级工程师学士,从事刑事理化检验鉴定工作.
引用该论文: HUANG Ke-jian,PAN Zhi-wen,LIN Cui-wu,LI Hong-sen,LIU Xiao-feng,LI Lu,LUO Zheng-jian,CHEN Er-lian. GC-MS with HS-SPME Determination of Methadone and Its Main Metabolite in Urine[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(8): 962～964
黄克建,潘智文,林翠梧,李宏森,刘晓锋,李璐,罗正坚,陈而廉. 顶空固相微萃取-气相色谱-质谱联用法测定尿液中美沙酮及其主要代谢物[J]. 理化检验－化学分册, 2009, 45(8): 962～964
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参考文献
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【2】蒋铁平,刘永红.低剂量美沙酮中毒一例[J].中国药物依赖性杂志,2006,15(1):76-78．
【3】SPORKERT F,PRAGST F.Determination of methadone and its metabolites EDDP and EMDP in human hair by headspace solid-phase microextraction and gas chromatography-mass spectrometry[J].Journal of Chromatography B,2000,746:255-264．
【4】ETTER M L,GEORGE S,GRAYBIEL K,et al.Determination of free and protein-bound methadone and its major metabolite EDDP: Enantiomeric separation and quantitation by LC/MS/MS[J].Clinical Biochemistry,2005,38:1095-1102．
【5】MOORE C,GUZALDO F,HUSSAIN M J,et al.Determination of methadone in urine using ion trap GC/MS in positive ion chemical ionization mode[J].Forensic science international,2001,119:155-160．
【6】LUCAS A C S,BERMEJO A M,TABERNERO M J,et al.Use of solid-phase microextraction (SPME) for the determination of methadone and EDDP in human hair by GC-MS[J].Forensic science international,2000,107:225-232．
【7】李文君,王继芬,李瑛,等.毛发中美沙酮及其代谢物的分析[J].现代仪器,2005(4):33-34．
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