GC/MS 衍生化法检测血中4-溴-2,5-二甲氧基苯乙胺

摘要

Objective To establish a GC/MS derivatization method for determining the 4-bromo-2, 5-dimethoxy-phenethylamine in blood. Methods Blood sample was extracted and purified by Bond Elut Centify® solid phase extraction column after diluted to four times by deionized water. The residuum was derivatized by trifluoroacetic anhydride. 4-bromo-2, 5-dimethoxyphenethylamine and 4-phenylbutylamine (internal standard) were analyzed by gas chromatography-mass spectrum. The ions m/z 242 and m/z 91 were applied in quantitative analysis for 4-bromo-2, 5-dimethoxyphenethylamine and 4-phenylbutylamine, respectively. Results The limit of detection was 6 ng/mL in blood sample and the calibration curve was linear in the range of 0.02~10μg/mL (=0.9993) for 4-bromo-2, 5-dimethoxyphenethylamine. The RSDs of intra-day and inter-day were less than 10%; the average extraction recovery of 4-bromo-2, 5-dimethoxyphenethylamine was about 69%. Conclusions This method is rapid, sensitive and suitable for qualitative analysis of 4-bromo-2, 5-dimethoxyphenethylamine in blood.%目的：建立人体全血中4-溴-2,5-二甲氧基苯乙胺的衍生化 GC/MS 分析方法。方法血液样品经去离子水稀释4倍，8000r/min 高速离心20min 后，加入 NaH2PO4缓冲溶液（pH 值为6.0）2mL，混匀。将上述混合液加入用甲醇、NaH2PO4缓冲溶液（pH 值为6.0）活化的 Bond Elut Centify®固相萃取柱后，依次采用1.0M乙酸溶液、去离子水、甲醇、二氯甲烷/异丙醇/氨水（78/20/2，V/V/V）混合洗脱液进行提取、分离、净化处理，40℃空气流下挥干，三氟乙酸酐衍生化，GC/MS 检测4-溴-2,5-二甲氧基苯乙胺和4-苯基丁胺衍生物。采用标准品衍生化产物的标准质谱图定性分析，选择 m/z 242（4-溴-2,5-二甲氧基苯乙胺）、m/z 91（4-苯基丁胺）作为定量离子进行定量分析。结果血液中4-溴-2,5-二甲氧基苯乙胺的最低检出限为6ng/mL，在0.02~10µg/mL 浓度范围内，线性关系良好（=0.9993），日内精密度和日间精密度均小于10%，平均提取回收率约为69%。结论该方法操作简便、灵敏度高，适用于全血中4-溴-2,5-二甲氧基苯乙胺检测。