固相萃取-液相色谱-串联质谱法检测血液中海洛因及其代谢产物

发布时间：2019-01-05 12:08

【摘要】：建立了固相萃取-液相色谱-串联质谱(SPE-LC-MS/MS)法分析吸毒者血样中的O6-单乙酰吗啡、吗啡、3-β-D-葡萄糖醛酸吗啡。以3-β-D-葡萄糖醛酸吗啡-d3为内标,选取Oasis HLB为固相萃取柱,AtlantisTMdC18(150mm×3.9mm×5μm)色谱柱为分析柱,采用甲醇-0.1%甲酸水溶液为流动相进行梯度洗脱;采用电喷雾正离子电离源,多反应监测(MRM)扫描方式,通过两对母离子/子离子和保留时间定性定量检测目标化合物。结果表明:血样中O6-单乙酰吗啡、吗啡、3-β-D-葡萄糖醛酸吗啡的检测限为3~5μg/L,线性关系良好,相关系数均在0.997 5以上;添加50、500、1 000μg/L加标水平后,O6-单乙酰吗啡、吗啡、3-β-D-葡萄糖醛酸吗啡的平均回收率为80.6%~98.9%,准确度为-7.3%~9.1%。该方法具有较高的灵敏度和选择性,可用于实际案件中海洛因及其代谢产物的检测。
[Abstract]:A solid phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) method was established for the determination of O6-monoacetomorphine and 3- 尾 -D-glucuronide morphine in the blood samples of drug addicts. With 3- 尾 -D-glucuronate-morphine d3 as internal standard, Oasis HLB as solid phase extraction column, AtlantisTMdC18 (150mm 脳 3.9mm 脳 5 渭 m) column as analytical column, methanol-0.1% formic acid solution as mobile phase for gradient elution. The target compounds were detected qualitatively and quantitatively by two pairs of parent ions / subions and retention time by electrospray positive ion ionization source and multi-reaction monitoring (MRM) scanning method. The results showed that the detection limit of O6-monoacetomorphine and 3- 尾 -D-glucuronide morphine in blood samples was 3 渭 g / L, the linear relationship was good, and the correlation coefficient was above 0.997; The average recovery of O6-monoacetylmorphine and 3- 尾 -D-glucuronide morphine was 80.6 and 98.9 respectively, and the accuracy was -7.3% -9.1% after adding 50 渭 g / L of 50 渭 g / L of 500 渭 g / L of O6-monoacetylmorphine and 3- 尾 -D-glucuronide. The method has high sensitivity and selectivity and can be used for the detection of heroin and its metabolites in practical cases.
【作者单位】：重庆市公安局交通管理局;重庆市公安局物证鉴定中心;
【分类号】：O657.63;D918.9

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