LC-MS/MS检测降压类中药制剂中非法添加的9种化学药物

目的 建立快速、准确、灵敏的检测降压类中药制剂中非法添加盐酸肼屈嗪、阿替洛尔、氨苯蝶啶、卡托普利、盐酸哌唑嗪、盐酸普萘洛尔、氯沙坦钾、利血平和螺内酯等9种化学药物的LC-MS/MS方法.方法 采用KINETEX 2.6 C18 100A(50.0×2.10mm)色谱柱,梯度洗脱:流动相A为乙腈-甲醇(4∶1),流动相B为5mmol·L -1甲酸铵缓冲液(用甲酸调节pH至3.0),流速为0.3mL· min -1,检测波长为230、272nm,柱温为50℃；离子源为ESI源,雾化气压力为40psi,干燥气流速为12L·min -1,干燥气温度为325℃,毛细管电压为3.5kV,正离子检测模式.通过与对照品的色谱和质谱行为比较,对样品中是否添加该9种化学药物进行定性鉴别.结果 上述色谱-质谱条件下,9种化学药物的检出限为0.2～2ng,符合鉴别要求.结论 该方法的专属性较强、灵敏度较高,适用于降压类中药制剂中添加该9种化学药物的定性分析.

Detection of nine chemical components added into antihypertension traditional Chinese medicine by LC-MS/MS

OBJECTIVE To establish a rapid,accurate and sensitive method for analysis of hydralazine hydrochloride,atenolol,triamterene,caotopril,prazosin hydrochloride,propranolol hydrochloride,reserpine,losartan potassium and spironolactone added into anti-hypertension traditional Chinese medicine by LC-MS/MS.METHODS KINETEX 2.6μ C18 100A（50×2.10mm） column was used;The mobile phase were acetonitrile-methanol（4∶1）（A） and 5mmol·L-1 ammonium formate buffer（adjust to pH3.0 with formic acid）（B） with gradient elution;The flow rate was 0.3mL·min-1;The detection wavelength was 230nm and 272nm;The column temperature was 50℃;The electrospray ionization（ESI） source was applied and operated in the positive ion mode,the drying gas flow rate was 12L·min-1,the drying gas pressure was 40 psi,the drying gas temperature was 325℃ and the ionization voltage was 3.5kV.The samples were indentified by comparison with the chromatographic behavior and mass spectral data of reference substances.RESULTS Nine kinds of antihypertensive were obtained by LC-MS and the detection limits were in the range of 0.2～2 ng.CONCLUSION The method is selective and sensitive.It can be used to identify the nine drugs illegally added in antihypertension traditional Chinese medicine.