超高效液相色谱-质谱联用快速同时检测止痒类中药制剂中添加11种化学药物成分

Simultaneous Determination of 11 Chemicals Added in Itching Agents Traditional Chinese ?edicines by UPLC-MS/MS

目的建立超高效液相色谱-质谱联用方法快速检测中药制剂中添加的11种化学药物成分(马来酸氯苯那敏、氯雷他定、硝酸咪康唑、盐酸特比萘芬、酮康唑、艾司唑仑、盐酸氯丙嗪、丙酸氯倍他索、醋酸地塞米松、醋酸泼尼松和吲哚美辛)。方法采用Waters ACQUITY UPLC BEH C18 column(2.1 mm×100 mm,1.7μm);梯度洗脱:流动相A为乙腈,流动相B为5 mmol·L^(-1)乙酸铵(0.1%甲酸)水溶液。通过比较样品峰与对照品峰的保留时间、一级质谱和二级质谱碎片离子,确定样品中是否掺杂化学止痒药物。结果建立的快速超高效液相串联质谱方法检测上述化学药物成分不受药物辅料干扰,各色谱峰分离良好,11种待测成分最低检出限为0.01~0.46 ng·m L^(-1)。结论该方法简便、灵敏度高,可快速有效地判断中药制剂中是否非法掺入上述化学药品。

OBJECTIVE To develop a method for simultaneous determination of 11 chemicals（chlorphenamine maleate, loratadine, miconazole nitrate, hydrochloric acid terbinafine, ketoconazole, estazolam, chlorpromazine hydrochloride, clobetasol propionate, dexamethasone acetate, prednisone acetate and indomethacin） added illegally in itching agents traditional Chinese medicines（TCMs） by UPLS-MS/MS. METHODS Separation was performed on Waters ACQUITY UPLC BEH C18 column（2.1 mm×100 mm, 1.7 μm）, and by gradient elution with acetonitrile and 5 mmol·L-（-1） ammonium acetate aqueous solution（contain 0.1% formic acid） as the mobile phase. The chemicals detected in samples were identified by comparison of sample peaks with the retention time, mass spectra and the product ions with those of reference substances. RESULTS The developed UPLC-MS/MS method was did not interfered by the adjuvants. The peaks detected could be separated from each other. The range of detection limits（LODs） for 11 chemicals were 0.01-0.46 ng·m L-（-1）. CONCLUSION The developed UPLC-MS/MS method is convenient, accurate and sensitive, which can be used for rapid screening of above-mentioned chemicals added illegally in TCMs.