解吸附电晕束电离质谱辅助高效液相色谱法检测减肥类保健食品中的违禁药物

Detection of illegal synthetic drugs in weight reducing dietary supplements by hybrid of DCBI-MS and HPLC-UV

目的利用解吸附电晕束电离质谱(DCBI-MS)对减肥类保健食品中违禁药物进行快速筛选,进而用高效液相色谱法(HPLC-UV)对疑似检出样品准确定量。方法通过DCBI-MS直接分析,对比标准物质的一级、二级质谱谱图,对检测样品中非法添加的芬氟拉明、酚酞、西布曲明、单去甲基西布曲明、双去甲基西布曲明进行定性鉴别。HPLC-UV对5种目标化合物准确定量。结果 HPLC-UV方法中各目标物的线性范围为0.25～300 mg/L。12个检测样品中3个样品共3种违禁物被DCBI-MS方法检出。高效液相色谱法准确复检结果显示DCBI-MS的半定量结果可信。结论 DCBI-MS无需样品预处理,单个样品的分析时间不到1 min,辅助高效液相色谱法实现了减肥类违禁药物的快速、高通量、高精度检测。

Objective To use desorption corona beam ionization-mass spectrometry for rapidly screening illegal synthetic drugs in weight reducing dietary ＇supplements, and precisely quantifying the suspected sample by HPLC-UV. Methods The qualitative identification of illegal additives, i. e. , fenfluramine, phenolphthalein, sibutramine, N-didesmethylsibutramine, N-mono-desmethylsibutramine in samples was performed by comparing MS and MS2 spectra of samples with standard substances by DCBI-MS. Accurate quantitation of these five targets was obtained by HPLC-UV. Results The concentration of targets was linear in the range of 0. 25-300 mg/L. Three illegal synthetic drugs in three of twelve samples were detected by DCBI-MS. The re-detecting results of HPLC-UV showed that the semi-quantitative results of DCBI-MS were credible. Conclusion Using DCBI-MS and cooperatively with HPLC-UV in detecting illegal synthetic drugs in weight reducing dietary supplements is fast, high-throughput and high-precision. Sample pretreatment is unnecessary when the determination of multiple components with DCBI-MS method. The analysis time for one aliquot is less than 1 min.