镇痛平喘类中成药中违禁添加的6种糖皮质激素的液相色谱-质谱检测

Simultaneous Determination of Six Glucocorticoid Drugs in Chinese Traditional Medicine by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了N-丙基乙二胺(PSA)基质固相萃取-高效液相色谱串联质谱同时测定镇痛平喘类中成药中添加的泼尼松、地塞米松、倍他米松、曲安奈德、倍氯米松、氯倍他索6种糖皮质激素的方法。样品用乙腈提取,PSA基质分散净化,采用Zobax SB C18分析柱(4.6mm×150mm,5μm),以保留时间和质谱二级特征离子作为定性依据。在建立的色谱条件下,6种糖皮质激素能得到很好的分离,线性范围均为1.5～300mg/kg,加标回收率为85%～102%。该法可同时对6种糖皮质激素进行定量分析,可用于镇痛平喘类中成药中掺杂该6种成分的快速鉴定。

A high performance liquid chromatography- tandem mass spectrometry（ HPLC -MS/MS） method was established for the determination of six glucocortieoid drugs, prednisone, dexametha- sone, betamethasone, triamcinolone, beclomethasone, and clobetasol in Chinese traditional medi- cine. The sample was extracted with acetonitrile, and cleaned up by dispersive solid-phase extraction with PSA sorbent. The separation of six glucocorticoids was achieved on Zobax SB C18 column（4. 6 mm × 150 mm, 5μm）. Identification of glucocorticoid was based on retention time and characteris- tic fragment ions. Under the optimal conditions, the assay was linear over the range of 1.5 -300 mg/kg. The spiked recoveries were in the range of 85% -102% . The method has obvious advanta- ges of simplicity, sensitivity and good repeatibility, and was suitable for simultaneous determination of six glucocorticoids in the Chinese traditional medicine.