摘要
利用顶空固相微萃取（HS／SPME）结合气／质联用（GC／MS—SIM）技术同时快速检测尿液中苯丙胺、甲基苯丙胺、MDA和MDMA．80℃下采用100μm聚二甲基硅氧烷萃取头萃取10min，3-苯基-1-丙胺作内标，探讨了影响SPME萃取效果的萃取时间、盐浓度、酸碱条件等因素，优化了实验条件．结果：苯丙胺、甲基苯丙胺、MDA和MDMA在50～2000ng／mL质量浓度范围内线性良好，相关系数（r^2）分别为0．9985，0．9971．0．9928和0．9994．检测限（信噪比=3）0．09ng／mL，0．02ng／mL，1．71ng／mL和0．15ng／mL，定量限（信噪比=10）0．31ng／mL，0．05ng／mL，5．68ng／mL．0．49ng／mL．1mL空白尿液加标250ng和1000ng，回收率在82％～108％之间，相对标准偏差（RSD）〈13％（n=5）．建立的方法适用于尿液中苯丙胺、甲基苯丙胺、MDA和MDMA的同时快速检测．
Rapid simultaneous determination of amphetamine, methamphetamine MDA and MDMA in urine using head-space solid phase microextraction （HS/SPME） and gas chromatography and mass spectrometry in select ion monitor mode （GC/MS-SIM）. The factors of extraction time, salt concentration, pH value were tested by performing 1007 m polydimethylsiloxane （PDMS） fiber at 80℃for 10min using 3-phenyl-l-propylamine as internal standard to optimize the experimental condition. Amphetamine, methamphetamine, MDA and MDMA showed excellent linearity in the range of 50 - 2 000 ng/mL with correlation coefficients （r^2） 0.9985, 0.9971, 0.9928 and 0.9994, respectively. The respective detection limits（S/N=3） were （S/N=3）0. 09 ng/mL,0.02 ng/mL,1.71 ng/mL and 0.15 ng/mL. The respective quantitative limits were 0. 31 ng/mL, 0.05 ng/mL, 5.68 ng/mL and 0.49 ng/mL. The recovery ratios were in the range of 82%-108% with RSD〈 13% （n = 5） by spiking 250 ng and 1 000 ng standard samples to 1 mL blank urine,respectively. Conclusion： The method introduced was suitable for rapid simultaneous detecting amphetamine, methamphetamine, MDA and MDMA in. urine.
出处
《广西大学学报（自然科学版）》
CAS
CSCD
2007年第3期266-269,共4页
Journal of Guangxi University（Natural Science Edition）
基金
公安部科研项目(2004523401)
