UPLC-MS/MS检测镇静安神类中成药中违禁添加地西泮、氯硝西泮和艾司唑仑

目的建立镇静安神类中成药中添加地西泮、氯硝西泮和艾司唑仑的专属检测方法。方法采用超高效液相色谱-串联四级杆质谱,C₁₈色谱柱（2.1 mm×50 mm,1.7μm）,10 mmol/L乙酸铵溶液-乙腈（90:10）梯度洗脱,流速0.4 ml/min,检测波长254nm;离子源为ESI源,正离子检测,对中成药中添加地西泮、氯硝西泮和艾司唑仑定性、定量检测。结果地西泮、氯硝西泮和艾司唑仑线性范围分别为109.8-878.4、102.1-816.8、106.9～855.2 ng/ml,地西泮、氯硝西泮和艾司唑仑的检出限为分别0.016、2.5×10^-3、2.8×10^-3ng,定量限分别为0.19、8.2×10^-3、9.2×10^-3ng,3种药物平均回收率在95.7%～103.7%之间。结论本方法选择性强、灵敏度高、处理方法简单,测定快速,可用于镇静安神类中成药中添加地西泮、氯硝西泮和艾司唑仑的测定。

Determination of forbidden addition drugs of Diazepam,Clonazepam and Estazolam in tranquilizing mind traditional Chinese medicine by UPLC-MS/MS

Objective To establish a specific method for determination of forbidden addition drugs of Diazepam, Clonazepan and Es- tazolam in tranquilizing mind Traditional Chinese Medicine. Methods Diazepam, Clonazepam and Estazolam were determined and analyzed by UPLC-MS/MS. ACQUITY BEH Cls analysis column（2.1 mm× 50 mm, 1.7μm） was used with the mobile phase of 10 mmol/L ammonium acetate and acetonitrile（90 ：10） with gradient elution. The flow rate was 0.4 ml/min,and the detection wavelength was 254 nm. EIS ion source was used with positive ion monitoring. Results The standard curves of Diazepam, Clonazepam and Estazolam showed good linearity over the concentration rang of 109.8 - 878.4, 102.1 - 816.8,106.9 - 855.2 ng/ml ,The detection limits were 0.06,2.5×10 -3,2.8× 10 -3 ng, the quantitation limits were 0.19,8.2× 10-3,9.2 × 10 3 ng,the average recoveries of three chemicals was 95.7% - 103.7%. Conclution The method was specific, sensitive, easily and quickly,which could be used to detect Diazepam, Clonazepan and Estazolam in tranquilizing mind traditional Chinese medicine.