SPE-GC/MS、GC/NPD法检测血液中苯丙胺类毒品  

Determination of amphetamine-Type Stimulants in blood by solid-phase extraction using gas chromatography/mass spectrometry and gas chromatography/nitrogen-phosphor detector Technique

作　　者：邸玉敏[1] 朱军[2] 常靖[2] 崔巍[2] 于忠山[2] 

机构地区：[1]中国人民公安大学,北京100038 [2]公安部物证鉴定中心,北京100038

出　　处：《刑事技术》2010年第3期11-14,共4页Forensic Science and Technology

基　　金："十一五"国家科技支撑计划项目(2006BAK09B06)

摘　　要：目的利用GC/MS、GC/NPD与固相萃取(SPE)技术相结合,建立血液中苯丙胺类毒品的定性定量分析方法。方法采用Bond-Elut Certify固相柱、甲醇淋洗、二氯甲烷/异丙醇/氨水(78/20/2)洗脱固相萃取分离提取,比较了不同pH体系、稀释状态、洗脱溶剂对提取回收率的影响,建立血液中苯丙胺类毒品的GC/MS、GC/NPD定性定量分析方法。结果以GC/NPD分析AM、MA、MDA和MDMA浓度在15ng/mL^2000ng/mL、10ng/mL^1600ng/mL、20ng/mL^3000ng/mL、20ng/mL^3000ng/mL范围内线性关系良好,AM、MA、MDA和MDMA的检测限分别为10ng/mL、8ng/mL、15ng/mL、15ng/mL,方法平均回收率大于85%,标准偏差小于5%,GC/MS-Scan检测限分别为40ng/mL、32.0ng/mL、60.0ng/mL、60.0ng/mL。结论此方法可满足苯丙胺类毒品滥用者的血液定性定量分析。Objective To develop a qualitative and quantitative analysis method for the determination of amphetamine-type stimulants in blood samples using solid-phase extraction combined with GC/MS and CR2/NPD. Methods The samples were extracted by solid-phase extraction with Bond Elut Certify cartridge. Analytes were washed with methanol, and eluted by dichlo romethane/isopropyl alcohol/ammonium hydroxide （78/20/2, v/v/v） mixed solvent. The optimum conditions for extraction, such as pH,dilution and elution conditions were studied in detail. Abuse drugs extracted from blood by solid phase extraction were detected and quantified with （SC/MS and GC/NPD. Results The experimental results indicated that linear calibration curves were obtained in blood concentration ranges of 15ng/mL-- 2000ng/mL for AM, 10ng/mL- 1600ng/mL for MA, 20ng/mL- 3000ng/ mL for MDA and MDMA and good limits of detection 10ng/mL for AM, 8.0ng/mL for MA, 15.0ng/mL for MDA and MDMA by GC/NPD. The method recovery were more than 85 %, and RSD〈5 %. The method was validated and showed good limits of de tection （32. 0ng/mL for MA, 60.0ng/mL for MDA and MDMA） by GC/MS. Conclusion The method developed may be applied for qualitative and quantitative analysis of amphetamine-type stimulants in blood.

关 键 词：法医毒物分析 苯丙胺类毒品 固相萃取 GC/NPD GC/MS 

分 类 号：D919.1[医药卫生—法医学]