摘要
采用三因素三水平响应面分析法对尿液中甲基苯丙胺(MPM)的固相萃取(SPE)条件作优化试验,所得最佳SPE条件为:①尿样的酸度:pH 9.35(PBS);②上样速率:0.9 mL·min^(-1);③洗脱剂(乙酸乙酯)的用量:3.2 mL。所得淋出液氮吹蒸干,溶于100μL内标物(SKF_(525-A))乙醇溶液中,供气相色谱分析。用AB-5毛细管色谱柱分离,进样量为1μL。采用氮磷检测器进行测定。甲基苯丙胺的质量浓度与其峰面积在0.10~10.0 mg·L^(-1)范围内呈线性关系,检出限(3S/N)为0.062 mg·L^(-1)。日内和日间相对标准偏差(n=6)均小于5%。
Response surface analysis with 3 factors and at 3 levels was applied to the optimization of conditions of solid phase extraction （SPE） of methamphetamine （MPM） in human urine, and the optimum conditions found were as follows： ① acidity of the urine sample： pH 9. 35 （PBS）; ② flow-rate of sample introduction： 0. 9 mL · min^-1 ; ③ appropriate volume of ethyl acetate as eluant： 3.2 mL. The eluate obtained was evaporated to dryness by N2-blowing, and the residue was taken up with 100/2L of ethanol solution of the internal standard of SKF525 A, and the solution was used for GC analysis. Chromatographic separation was carried out on AB-5 capillary column with volume of sample introduction of μL. Nitrogen-phosphorus detector was used in the determination. Linear relationship between values of peak area and mass concentration of methamphetamine was kept in the range of 0. 10=10.0 mg·L^-1 with detection limit （3S/N） of 0, 062 mg ·L^-1. Values of within-day and inter-day RSD＇s （n=6） obtained were same to be less than 5%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2013年第10期1205-1208,1212,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
公安部重点研究计划项目(2010ZDYJJLST015)
关键词
气相色谱法
甲基苯丙胺
尿液
固相萃取
响应面法
GC
Methamphetamine
Urine
Solid phase extraction
Response surface method
