UPLC-MS/MS法测定海洛因中10种掺杂物  

Determination of 10 adulterants in Heroin by UPLC-MS /MS

作　　者：刘翠梅[1,2] 刘培培[2] 白燕平[2] 

机构地区：[1]中国人民公安大学,北京100038 [2]公安部禁毒情报技术中心,北京100193

出　　处：《中国法医学杂志》2013年第5期363-366,共4页Chinese Journal of Forensic Medicine

基　　金：国家科技支撑计划(2011BAK04B06)

摘　　要：目的采用超高效液相色谱-串联四极杆质谱仪(UPLC-MS/MS),在电喷雾离子源正离子(ESI+)和多反应监测(MRM)模式下建立了定性、定量测定海洛因中10种掺杂物的方法。方法使用甲醇超声溶样,ACQUITY UPLCTMBEH C18(1.7μm,100 mm×2.1 mm)色谱柱,流动相为pH=9.66的10 mmol/L的碳酸氢铵和乙腈,在梯度条件下分析。结果该方法定量限为0.005-0.5μg/g。添加水平在25-250 ng/mL范围内,加标回收率为95.8%-114.2%,相对标准偏差为1.1%-6.5%。结论本方法简便、快速、准确、灵敏,满足对海洛因样品中掺杂物进行快速定性、定量分析的需要。Objective A novel method has been developed for the determination of 10 adulterants in heroin samples by ultra performance liquid chromatography combined with tandem mass spectrometry （UPLC- MS/MS）. The sample was extracted by ultrasonic, using methanol as solvent. Methods A Acquity UPLCTM BEH C18 column（ 1.7 μm, 100 mm × 2. 1 mm）with binary gradients containing 10 mmoL/L ammonium bicarbonate（pH =9.66） / acetonitrile mixtures was investigated for the analysis. For MS/MS detection, an atmospheric pressure positive electrospray source was employed with multiple reaction monitoring （MRM）. Results LOQ of different adulterants ranged over 0. 005 - 0. 5μg/g. Recoveries at 25 - 250 ng/mL ranged from 95.8% -114.2% and RSD% was1. 1% -6.5%. Conclusion The established method can be applied for determining the adulterants in heroin samples with high sensitivity and high selectivity.

关 键 词：法医毒物分析 海洛因 超高效液相色谱-串联四极杆质谱仪 掺杂物 

分 类 号：D919[医药卫生—法医学]