高效液相色谱-质谱联用法检查止喘灵胶囊中非法添加的醋酸泼尼松和茶碱

Determination of Prednisone Acetate and Theophylline Illegally Added into Zhichuanling Capsules by HPLC-MS/MS

目的采用高效液相色谱-质谱联用技术,检查止喘灵胶囊中非法添加的醋酸泼尼松和茶碱。方法色谱柱为Shimadzu shim-pack VP-ODS柱(250 mm×4.6 mm,5μm),0.02 mol/L乙酸铵-0.1%冰醋酸水溶液∶乙腈(71∶29)为流动相,流速为1.0 mL/min;Agilent6310型离子阱质谱仪,电喷雾离子源(ESI),雾化气压力为50 psi,干燥气温度为380℃,流速为9.5 mL/min,毛细管电压为3 500 V,扫描范围为100～500 m/z,检测方式为正、负模式一级、二级同时扫描。结果在高效液相色谱、质谱中,样品出现与醋酸泼尼松、茶碱成分一致的色谱峰、质谱峰。结论所用方法简单可行,结果准确可靠,可用于止喘灵胶囊中非法添加醋酸泼尼松、茶碱的定性鉴别。

Objective To establish a HPLC-MS/MS method for detecting prednisone acetate and theophylline illegally added in Zhichuanling Capsules.Methods The detection was performed on the Shimadzu shim-pack VP-ODS column（250 mm×4.6 mm,5 μg） with the mobile phase of 0.02 mol/L ammonium acetate-0.1% glacial acetic acid solution：acetonitrile（71 ∶29） at a flow rate of 1.0 mL/min.The Agilent 6310 ion trap mass spectrometer was adopted with electrospray ion sourse（ESI）.The nebulizer pressure was 50 psi and the dry air temperature was 380 ℃ with a rate of 9.5 mL/min,the capillary voltage was 3 500 V.The scan range was 100-500 m/z.The detection mode：simultaneous first and second level scanning with positive and negative modes.Results In HPLC and MS,the chromatographic and mass peaks coinciding with prednisone acetate and theophylline reference substances were found in the sample.Conclusion This method is simple and feasible with the accurate and reliable results,so which can be used to qualita-tively identify prednisone acetate and theophylline illegally added into Zhichuanling Capsules.