液质联用法检测中药制剂中添加的肾上腺皮质激素

HPLC-MS Determination of Adrenal Cortical Hormone in Traditional Chinese Medicine

目的建立检测中药制剂中掺入的肾上腺皮质激素的液质联用法,并对11批市售药品及医院制剂进行检测。方法采用C8色谱柱,以乙腈-水(35∶65)为流动相,流速0.5mL.min-1,柱温45℃。电喷雾离子化源,正离子检测,扫描方式:一级全扫描及二级全扫描方式。根据所检测到化合物的色谱保留时间及二级质谱信息,并与对照品比较,对中药制剂中掺入的化学药进行定性鉴别。结果11批样品中,3批被检测出掺有醋酸泼尼松,1批掺有醋酸地塞米松。结论该法操作简便、选择性强、灵敏度高、结果准确可靠,可以有效检测出中药制剂中添加的肾上腺皮质激素。

Objective To develop an HPLC-MS adulterated in the traditional Chinese medicine and test preparations. Methods The analysis was performed on method for the detection of adrenal cortical hormone 11 batches of commercially available drugs and hospital a C8 column with the mobile phase of acetonitrile-water （35 ： 65） at a flow rate of 0.5 mL · min^-1 and column temperature at 45 ℃. The mass spectrometer was equipped with ESI ion source and operated in a positive ion mode. Two scan modes including full scan MS and full scan MS2 were used. The compounds were identified according to the chromatographic behavior and the mass data by comparison with those of reference substances. Results Among the 11 batches of samples, 3 batches were found with adulterated prednisone acetate and 1 batch was detected with adulterated dexamethasone acetate. Conclusion The method is simple, selective, sensitive, reliable and accurate, which can be used to detect adrenal cortical hormone adulterated into the traditional Chinese medicine.