HPLC-MS联用同时检测支气管类中成药中违禁添加的11种糖皮质激素

Simultaneous determination of eleven glucocorticoids in Chinese trandition medicines for bronchus by HPLC-MS

目的建立一个高准确性、高灵敏度的液相色谱一质谱联用方法，检测支气管哮喘类中成药中违禁添加的11种糖皮质激素（倍他米松，丙酸倍氯米松，氯氟舒松，醋酸泼尼松龙，氢化可的松，醋酸氟轻松，醋酸泼尼松，醋酸曲安奈德，醋酸可的松，氢化泼尼松，醋酸地塞米松）。方法色谱条件为Waters×Terra MS C18色谱柱（2．1mm×150mm，5μm），柱温35℃，流动相以0．1％甲酸10mmol／L乙酸铵溶液-乙腈进行梯度洗脱，体积流量为0．25mL／min。质谱条件为以电喷雾离子源正离子模式进行质谱数据采集。结果在建立的色谱条件下，11种糖皮质激素有良好的分离，且对其定性定量检出，线性范围良好，加样回收率为90％～110％。结论该法操作简便、快捷、高灵敏度、高准确性等特点，可同时对中成药中非法添加多种糖皮质激素进行定性定量分离检测。

AIM To establish a method for detecting eleven glucocorticoids （Betamethaone, Beclonmetasone, Dlpropionate, Halcinonidum, Prednisolone acetate, Hydrocortisonum, Fluocinonide, Prednisone acetate, Triamci- nolone acetonide, Cortisone acetate, Prednisolonum, Dexamethasone acetate） that were illegally added in antiasthmatic herbal preparations. METHODS Waters XTerra MS Cls （2. 1 mm× 150 mm, 5 μm） column was used with column temperature of 35 ℃, the mobile phase was consisted of 0. 1% formic acid - 10 mmol/L ammonium acetate solution and acetonitrile in gradient elution manner, the flow rate was 0. 25 mL/min. Electronspray ioniza- tion in the positive ions mode was adopted in mass spectrometry. RESULTS In the chromatographic conditions established, the eleven glucocorticoids were separated finely and could be detected qualitatively and quantitatively, the range of linearity was good with the labeled recovery from 90% to 110%. CONCLUSION This method not only is convenient, rapid, sensitive and accurate, but also can be used to separate and detect a variety of glucocorticoids qualitatively and quantitatively in Chinese trandition medicines at the same time.