面膜中41种糖皮质激素检测方法的建立及应用

Rapid detection of 41 glucocorticoids illegally added to the mask

建立了用超高效液相色谱-串联质谱法快速筛查和准确定量面膜中可能非法添加的41种糖皮质激素的分析方法。样品经甲醇提取后,用Thermo Hypersil GOLD色谱柱分离目标物,以0.1%乙酸水溶液-0.1%乙酸乙腈溶液为流动相进行梯度洗脱分离,电喷雾电离(ESI),多反应监测(MRM)模式测定41种糖皮质激素,以保留时间和离子对(母离子和2个碎片子离子)信息比较进行定性,以母离子和响应值高的碎片离子外标法定量。在该方法条件下,41种糖皮质激素分离度良好,方法检出限(LOD)为0.49~1.65μg/kg,定量限(LOQ)为1.63~5.50μg/kg,回收率为82.6~118.2%,精密度为2.3~6.8%。该方法简便、准确、快速、灵敏度高,可作为面膜中非法添加糖皮质激素成分筛查和定量检测方法。

An analytical method for rapid screening and accurate quantification of 41 kinds of glucocorticoids that may be il⁃legally added to the mask was established by ultra performance liquid chromatography tandem mass spectrometry(ultra per⁃formance liquid chromatography tandem mass spectrometry).Samples were extracted with methanol and separated by Ther⁃mo Hypersil GOLD column.Gradient elution was performed on 0.1%acetic acid aqueous solution,-0.1%acetic acid and acetonitrile as mobile phase.Electrospray ionization(ESI)and multiple reaction monitoring(MRM)mode were used to de⁃termine 41 glucocorticoids.The retention time and ion pair(parent ions and 2 fragment ions)were compared qualitatively and separated from each other.The fragment ion external standard method with high response value was used for quantita⁃tive analysis.Under the condition of this method,the resolution of 41 kinds of glucocorticoids was good,the LOD was 0.49-1.65μg/kg,the LOQ was 1.63-5.50μg/kg,the recovery was 82.6-118.2%,and the precision was 2.3-6.8%.The method is simple,accurate,rapid and sensitive,and can be used for screening and quantitative detection of glucocorticoid illegally added in facial mask.