HPLC/UV/MS鉴别中药制剂中糖皮质激素的方法研究

HPLC/UV/MS Identification of Corticosteroids in Traditional Chinese Medicinal Preparation

目的建立鉴别中药制剂中可能添加的糖皮质激素的分析方法。方法采用高效液相色谱、质谱法。SUPELCO Discovery C18(250 mm×4.6 mm,5μm)分析柱;乙腈-水为流动相进行梯度洗脱;检测波长为243 nm;流速1.0 mL/min;电喷雾离子源,采用质谱多重反应监测(MRM)扫描方式。结果在该液相条件下,能同时有效分离6种糖皮质激素。应用该法鉴定了中药制剂中的糖皮质激素,通过液相色谱保留时间、相对分子质量、二级质谱碎片信息等方面信息,可确定样品中含有氢化可的松、醋酸泼尼松龙。结论本测定方法简便、灵敏,专属性强,可为中药制剂中糖皮质激素的检测提供快捷有效的分析方法。

Objective To develop the method for identification of corticosteroids added illegally in traditional Chinese medicinal preparation.Methods The HPLC-quadrupole mass spectrometry method was used.The analyses were performed on a SUPELCO Discovery C18（250 mm×4.6 mm,5 μm） with gradient elution using acetonitrile-water as mobile phase.The detection wavelength was 243 nm.The flow rate was 1.0 mL/min.The corticosteroids illegally added into traditional Chinese medicinal preparations were identified according to the chromatographic behavior and mass spectral data by comparison with those of reference substance.Results Six kinds of corticosteroids can be identified at above conditions.Hydrocortisone and prednisolone acetate were found in one preparation.Electrospay ionization source was applied.Conclusion This method is simple,sensitive and specific.It can provide an efficient way for the identification of corticosteroids.