液质联用检查15种降压类药物及数据检索库的建立

 目的为打击中药制剂及保健食品中非法添加化学药物现象,建立准确、灵敏的HPLC-MS/MS方法甄别中药制剂及保健食品中可能添加的15种化学降压药物。方法采用Waters Sunfire C₁₈色谱柱,梯度洗脱:流动相A为20 mmol·L^-1醋酸铵溶液,流动相B为甲醇-乙腈(2∶1),检测波长为230 nm,流速为1 mL·min^-1(分流比为4∶1)。选择正负离子全扫描方式检测临床常用的15种降压药,利用质谱解析软件研究了上述化合物的质谱裂解规律。通过比较样品峰与对照品峰的一级质谱、二级质谱质荷比,确定样品中是否掺杂了化学药物。结果在上述色谱及质谱条件下,15种降压药物HPLC图谱分离度良好,质谱分辨率符合鉴别要求。HPLC-MS/MS方法测定上述化学物质的最小检出量为1～80 ng。结论该方法灵敏度、准确性、重现性均可满足定性检查的要求,简便,快捷。

Identification of Antihypertensive by HPLC-MS/MS and Its Database Development

OBJECTIVE To develop a high performance liquid chromatography-electrospray ion trap mass spectrometry method for identifying fifteen kinds of antihypertensive illegally adulterated in traditional Chinese medicine(TCM) preparations.METHODS The fragmentation pattern of these drugs was summarized.After being separated by HPLC,the organic solvent extraction from TCM preparations was analyzed by the mass spectrometer,operated in positive ion or negative mode and in three scan modes including full scan MS,selected ion monitoring and full scan MS2.The obtained pseudo molecular ions and fragment ions were used to identify these drugs.RESULTS A good resolution of fifteen kinds of antihypertensive were obtained by HPLC and MS. The determination limit were in the range of 1～80 ng.CONCLUSION The method is simple,rapid and sensitivity.