加压流体萃取技术快速测定毛发中毒品及代谢物

Rapid determination of drugs and metabolites in hair by pressurized fluid extraction

目的建立加压流体萃取-液相色谱串联质谱(LC-MS/MS)法快速测定毛发中12种毒品及代谢物方法。方法以甲醇作为萃取溶剂,先后对影响加压流体萃取的温度、时间及循环次数条件进行考察,确定最佳实验方法,其萃取温度90℃、静态萃取时间6 min、萃取循环2次,收集萃取溶剂,经真空平行浓缩仪浓缩定容后,用LCMS/MS进行定性和定量分析。结果苯甲酰爱康宁在1.0~500 ng/mL范围内线性关系良好,其余11种毒品及代谢物在5.0~500 ng/mL范围内线性关系良好,相关系数r均大于0.99。方法检出限为1.0~5.0 ng/mL,加标回收率为70.8%~120.9%,相对标准偏差(RSD)1.1%~9.7%。通过分析20例毒品滥用者阳性毛发,其结果与供述吸食的毒品种类一致。结论该方法前处理操作简单,定性定量效果好,线性范围广,精密度、灵敏度高,能够满足毛发中12种毒品及代谢物的快速检测。

Objective To estabish a method for rapid determination of 12 drugs and metabolites in hair by pressurized fluid extraction-liquid chromatography tandem mass spectrometry(LC-MS/MS).Methods We use methanol as extraction solvent,then investigate the temperature,time and cycle times which affect the pressurized fluid extraction conditions,and determine the optimal experimental method:the extraction temperature was 90℃,the static extraction time was 6 min,extraction cycle was 2 times,then collect extraction solvent.After concentration with vacuum parallel concentrator,carry out qualitative and quantitative analysis by LC-MS/MS.Results Benzoylecgonine showed good linearity in the range of 1.0~500 ng/mL,and the other 11 drugs and metabolites showed good linearity in the range of 5.0~500 ng/mL,and their correlation coefficients r were all greater than 0.99.The limits of detection were 1.0~5.0 ng/mL,the recoveries were 70.8%~120.9%,and the relative standard deviations(RSD)were 1.1%~9.7%.By analyzing the positive hair of 20 drug abusers,the results were consistent with the reported drug use.Conclusions This method has the advantages of simple pretreatment,good qualitative and quantitative effect,wide linear range,high precision and sensitivity,which can meet the requirements of the rapid detection of 12 drugs and metabolites in hair.