超高效液相色谱-飞行时间质谱联用法检测牙痛灵胶囊中非法添加的4种化学成分

Detection of four kinds of compounds illegally added in Yatongling capsules by UPLC-Q-TOF-MS

目的采用超高效液相色谱-飞行时间质谱联用法(UPLC-Q-TOF-MS)检测牙痛灵胶囊中非法添加的甲硝唑、马来酸氯苯那敏、吡罗昔康及醋酸泼尼松。方法采用Agilent Zorbax SB C18色谱柱(100 mm×2.1 mm,1.8μm),流动相为10mmol·L^(-1)乙酸铵溶液-甲醇,梯度洗脱,流速0.3 m L·min^(-1),柱温35℃,正离子扫描检测。结果牙痛灵胶囊中非法掺入的甲硝唑、马来酸氯苯那敏、吡罗昔康及醋酸泼尼松的保留时间与相应对照品的相同,并经Targeted MS/MS进一步得到快速确证。结论所用方法操作简便、结果可靠,可用于快速确证牙痛灵胶囊中非法添加的甲硝唑、马来酸氯苯那敏、吡罗昔康和醋酸泼尼松。

OBJECTIVE To establish a method for the qualitative analysis of metronidazole, chlorphenamine maleate,piroxicam and prednisone acetate which were illegally added in Yatongling capsules by UPLC - Q - TOF - MS. METHODS Sample was performed on Agilent ZORBAX SB Cls column （100 mm × 2. 1 mm, 1. 8 μm） with the mobile phase of 10 mmol· L-1 ammonium acetate - methanol in a gradient elution manner, with the flow rate of 0.3 mL·min-1 and the column temperature of 35℃, and with ESI＋. RESULTS The retention time and UV spectra of metronidazole, chlorphenamine maleate, piroxicam and prednisone acetate illegally added in Yatongling capsules were the same as the reference substance. Then they were verified by targeted MS/MS. CONCLUSION The method is simple and accurate. It can be used for rapid screening and rapid identification of metronidazole, chlorphenamine maleate, piroxicam and prednisone acetate which were illegally added in Yatongling capsules.