LC-MS/MS快速筛分样本中的甲基苯丙胺、甲氧那明

Determination of methamphetamine and methoxyphenamine in samples by ultra performance liquid chromatography-mass spectrometry

目的建立准确可靠的甲氧那明、甲基苯丙胺初筛阳性样本的确证分析方法,排除由于服用甲氧那明而产生的假阳性结果。方法采用Kinetex■C18 (100×2.1mm,2.6μm)色谱柱,乙腈和0.1%的甲酸梯度洗脱,流速0.4 mL/min。质谱条件:选用电喷雾离子源,在正离子电离模式下,采用多反应监测(MRM)的质谱扫描方式,甲氧那明、甲基苯丙胺的母/子离子对分别为:m/z 180.2→120.8和m/z 150.1→91.1。结果甲氧那明线性范围0.2~500ng/mL,线性相关系数0.9913,最低检测浓度(LOQ, S/N=3)为0.2ng/ml,空白添加回收率85.6%~98.3%。甲基苯丙胺线性范围0.05~500ng/mL,线性相关系数0.9968,最低检测浓度(LOQ, S/N=3)为0.05ng/ml,空白添加回收率91.4%~103.1%。结论本研究建立的LC-MS/MS分析方法准确、快速、有效,可用于因甲氧那明干扰初筛为阳性的样本进一步的确证是否含有甲基苯丙胺成分。

Objective To establish an exact confirmatory analysis method of differentiating samples which contain methoxyphenamine, methamphetamine. to remove the false positive results by taking methoxyphenamine. Methods Kinetex■ C18 column(100×2.1 mm, 2.6μm) was used,the mobile phase consisted of acetonitrile and 0.1% formic acid, and the flow rate was 0.4 m L/min. Mass spectrometry was performed in multiple reaction monitoring(MRM) mode, with m/z of 180.2 → 120.8 for methoxyphenamine and m/z of 150.1 → 91.1 for methamphetamine. Result The linear range of methoxyphenamine was 0.2 to 500 ng/mL and the correlation coefficient was 0.9913. The limit of quantification(LOQ,S/N= 3) was 0.2 ng/mL and the recovery of appended contrast in blank sample ranged from 85.6% to 98.3%. The linear range of methamphetamine was 0.05 to 500 ng/mL and the correlation coefficient was 0.9968. The limit of quantification(LOQ S/N= 3) was 0.05 ng/mL and the recovery of appended contrast in blank sample ranged from 91.4% to 103.1%. Conclusion This analysis method by LC-MS/MS in this study is accurate fast and effective, can be used to further confirmed to contain methamphetamine components in the positive initial screening due to methoxyphenamine interference.