论文部分内容阅读
目的建立消字号产品中地塞米松和氯倍他索丙酸酯的液相色谱-串联质谱(LC-MS/MS)同时测定方法。方法以饱和氯化钠溶液以及乙腈2次液液萃取样品后做蛋白沉淀处理,然后经过固相萃取小柱净化后,采用Waters C18色谱柱(50 mm×2.1 mm,1.7μm)为分离柱,流动相为0.1%甲酸-5 mmol/L乙酸铵水(A)-乙腈(B),梯度洗脱,流速为0.25 ml/min,柱温为25℃。电喷雾离子源正离子多反应监测(MRM)模式进行定性分析和定量分析。结果地塞米松和氯倍他索丙酸酯在2.5 ng/ml~810 ng/ml内呈良好的线性关系,相关系数分别为0.998 2和0.997 6;检出限为0.02μg/g;定量限为0.05μg/g;平均回收率为98.0%~103.6%,相对标准偏差(RSD)为1.1%~6.5%。10批来自不同厂家市售样品中有8批检出氯倍他索丙酸酯。结论本方法操作简便、灵敏度高,可用于消字号产品中非法添加糖皮质激素的检测。
Objective To establish a method for simultaneous determination of dexamethasone and clobetasol propionate in Xiao Xiao products by liquid chromatography-tandem mass spectrometry (LC-MS / MS). Methods The samples were extracted with saturated sodium chloride solution and acetonitrile twice. After the samples were purified by solid phase extraction (SPE), the column was separated on a Waters C18 column (50 mm × 2.1 mm, 1.7 μm) The mobile phase consisted of 0.1% formic acid and 5 mmol / L ammonium acetate in water (A) - acetonitrile (B). The mobile phase was eluted with a gradient of 0.25 ml / min and the column temperature was 25 ℃. Electrospray ionization positive ion multiple reaction monitoring (MRM) mode for qualitative analysis and quantitative analysis. Results Dexamethasone and clobetasol propionate showed a good linearity in the range of 2.5 ng / ml ~ 810 ng / ml with correlation coefficients of 0.998 2 and 0.997 6, respectively. The limit of detection was 0.02 μg / g. The limit of quantification The average recovery was 98.0% ~ 103.6%, and the relative standard deviation (RSD) was 1.1% ~ 6.5%. 10 batches of samples from different manufacturers available in commercial samples were tested with clobetasol propionate. Conclusion The method is simple, sensitive and can be used for the detection of illegally added glucocorticoids.