液质联用检测消肿止痛中成药的氨基比林及双氯芬酸钠

目的：建立同时测定中药制剂中非法添加氨基比林及双氯芬酸钠的HPLC—MS／MS的方法。方法：采用c．8柱分离（100mm×4．6mm，3斗m），以乙腈-水为流动相梯度洗脱，流速：0．5ml·min^-1，检测波长：280nm。离子源为ESI源，正负离子交替模式进行定性检测，HPLC测定含量。结果：5批受试制剂中有2批检测到违禁添加的双氯芬酸钠，1批检测到违禁添加的氨基比林。结论：该方法选择性强、灵敏度好，可作为分析消肿止痛类中药制剂中违禁添加氨基比林及双氯酚酸钠的有效检测方法。

Determination of Aminopyrine and Diclofenac Sodium Illegally Added into Detumescent and Analgesic Chinese Medica Preparation by HPLC-MS/MS

Objective ： To establish an HPLC-MS/MS method for simultaneous determination of aminopyrine and diclofenac sodium illegal added into the detumeseent and analgesic chinese medica preparation. Method： A C18 column （100 mm ×4. 6 mm,3 μm） was used, with a gradient mobile phase was acetonitrile-water and flow rate was 0. 5 ml·min^-1. The detective wavelength was 280 nm. The ion source was ESI and the mode was positive and negative ion alternation. The content was determined by HPLC. Result： In the five batches of samples, diclofenac sodium was found in two batches and aminopyrine was found in one batch. Conclusion： The method is exclusive and sensitive, it can be used to detect aminopyrine and diclofenac sodium illegally added into the detumescent and analgesic chinese mediea preparation.