液相色谱-串联质谱法同时检测抗风湿类中成药中添加的10种糖皮质激素

目的: 建立测定抗风湿类中成药中曲安西龙、氟米松、倍氯米松、氟米龙、氢化可的松丁酸酯、氟氢松醋酸酯、倍他米松戊酸酯、氯倍他索丙酸酯、倍他米松双丙酸酯、氯倍他松丁酸酯10种糖皮质激素的液相色谱-串联质谱法. 方法: 以Agilent SB C₁₈(2.1 mm×100 mm,1.8 μm)色谱柱分 离,柱温30 ℃,流动相为水-乙腈二元梯度洗脱,流速0.3 mL · min^-1,电喷雾离子源正离子模式质谱采集. 结果: 10种糖皮质激素有很好的分离,在测定范围内线性良好,检出限为14.7~16.3 ng,定量限为48.9~54.2 ng,平均回收率为70.4%~98.5%;20批市售样品有1批检出氯倍他索丙酸酯,5批模拟样品中分别依次检出10种糖皮质激素. 结论: 本文建立的方法经方法学验证和模拟样品检测证明可用于抗风湿类中成药中非法添加糖皮质激素的检测.

Objective: To establish a LC-MS method for detecting ten kinds of glucocorticoids(triamcinolone,flumethasone,beclomethasone,fluoromethalone,hydrocortisone 17-butyrate,fluocinonide,betamethasone 17-valerate,clobetasol 17-propionate,betamethasone dipropionate,clobetasone 17-butyrate)in anti-rheumatic Chinese medicines. Methods: The Agilent SB C₁₈ (2.1 mm×100 mm,1.8 μm)column was used with a column temperature of 30 ℃,the mobile phase consisted of water-acetonitrile in a gradient elution manner.The flow rate was 0.3 mL · min^-1.The electrospray ionization in positive ion mode was equipped in mass spectrometry. Results: Ten kinds of glucocorticoids were completely separated.Good linearity was shown in the measurement range of the compounds.The detection limit was 14.7-16.3 ng,the quantification limit was 48.9-54.2 ng and the average recovery was 70.4% to 98.5%.Twenty commercial samples were tested and clobetasone 17-butyrate was detected positive in one sample and ten kinds of glucocorticoids were detected positive in five samples. Conclusion: The method can be used for detecting glucocorticoids illegally added in anti-rheumatic Chinese medicines.

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