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目的探讨应用高效液相色谱-二极管阵列检测器(HPLC-DAD)技术建立中药及保健品中非法添加氢化可的松琥珀酸钠、泼尼松龙、氢化可的松、泼尼松、甲泼尼龙、倍他米松、地塞米松、曲安奈德、醋酸泼尼松龙、醋酸氢化可的松、醋酸氟氢可的松、醋酸泼尼松、醋酸可的松、醋酸地塞米松、丁酸氢化可的松、醋酸曲安奈德、醋酸氟轻松和哈西奈德等18种糖皮质激素类添加剂成分的检查方法。方法采用Alltima C18色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-10 mmol/L醋酸铵二元梯度洗脱,流速为0.5 m L/min,检测波长242nm。对于HPLC-DAD检出的疑似阳性样品用液相色谱-质谱法(LC-MS/MS)进行进一步确认。结果氢化可的松和泼尼松的色谱峰重叠,其他16种糖皮质激素在5~320 mg/L内线性关系良好,线性相关系数(r)均大于0.9998;灵敏度高,最低检测限均在0.49~0.51 ng之间,定量限均在1.23~1.27 ng之间;回收率良好,低、中、高3个浓度的回收率均在97.52%~104.2%之间;精密度良好,相对标准偏差(RSD)均小于0.47%;稳定性良好,12 h内峰面积和保留时间的相对标准偏差(RSD)均小于0.68%。14种不同剂型的样品通过HPLC-DAD检查和LC-MS/MS确认,结果显示:某片剂中检测出醋酸地塞米松,某喷雾剂中检出倍他米松。结论 HPLC-DAD技术应用快速、灵敏、易推广,可作为筛查药品及保健品中非法添加18种糖皮质激素的检查方法。
Objective To investigate the application of high performance liquid chromatography-diode array detector (HPLC-DAD) in the establishment of traditional Chinese medicine and health care products illegally added hydrocortisone sodium succinate, prednisolone, hydrocortisone, prednisone, Nylon, betamethasone, dexamethasone, triamcinolone acetonide, prednisolone acetate, hydrocortisone acetate, fludrocortisone acetate, prednisone acetate, cortisone acetate, dexamethasone acetate, butyrate Hydrocortisone, triamcinolone acetonide, fluocinolone acetonide and halcinonide and other 18 kinds of glucocorticoid additive components of the inspection method. Methods Alltima C18 column (4.6 mm × 250 mm, 5 μm) was used. The mobile phase consisted of a binary gradient of acetonitrile-10 mmol / L ammonium acetate with a flow rate of 0.5 mL / min and a detection wavelength of 242 nm. Suspected positive samples detected by HPLC-DAD were further confirmed by liquid chromatography-mass spectrometry (LC-MS / MS). Results The chromatograms of hydrocortisone and prednisone overlapped. The other 16 glucocorticoids showed a good linearity in the range of 5-320 mg / L with a linear correlation coefficient (r) greater than 0.9998. The highest sensitivity and lowest detection limit 0.49 ~ 0.51 ng, the limits of quantification were in the range of 1.23 ~ 1.27 ng. The recoveries were good, and the recoveries of the three concentrations were between 97.52% and 104.2%. The precision was good and the relative standard deviation (RSD) were less than 0.47%. The stability was good. The relative standard deviations (RSDs) of peak area and retention time within 12 h were all less than 0.68%. Fourteen samples of different dosage forms were confirmed by HPLC-DAD and LC-MS / MS. The results showed that dexamethasone acetate was detected in one tablet and betamethasone was detected in one spray. Conclusion HPLC-DAD is a rapid, sensitive and easy-to-use method that can be used as a screening method to illegally add 18 glucocorticoids to drugs and health products.