分散固相萃取-液相色谱-串联质谱法同时快速测定化妆品中81种糖皮质激素

建立了分散固相萃取-液相色谱-串联质谱同时快速测定化妆品中81种非法添加糖皮质激素(GCs)的分析方法。样品用水分散后加乙腈超声提取,经十八烷基键合硅胶(C18)和N-丙基乙二胺(PSA)净化,待测物选用具有多重色谱保留模式的Poroshell 120 PFP色谱柱(100 mm×2.1 mm,2.7μm)分离,以0.2%(v/v)乙酸水溶液-乙腈为流动相梯度洗脱,在电喷雾正离子模式下以动态多反应监测方式测定,内标法定量。81种待测物在各自的浓度范围内线性关系良好,相关系数均大于0.99,在3个不同的添加水平下,平均回收率为68.8%~105.3%,RSD为2.9%~13.1%(n=6),方法的检出限(S/N≥3)和定量限(S/N≥10)分别为0.002~0.006μg/g和0.005~0.020μg/g。筛查了137个化妆品样品,发现16个阳性样品,含量为16.9~158μg/g。结果表明,该法简便快速,灵敏可靠,适用于化妆品中81种GCs的同时快速定性定量筛查分析。

Simultaneous rapid determination of 81 glucocorticoids in cosmetics by dispersive solid phase extraction and liquid chromatography-tandem mass spectrometry

A novel method was developed for the simultaneous rapid determination of 81 illegally added glucocorticoids (GCs) in cosmetics using dispersive-solid phase extraction (d-SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The analytes were extracted by acetonitrile after dispersing with water, and then purified using the C₁₈ and primary secondary amine (PSA). The chromatographic separations were performed on a Poroshell 120 PFP column (100 mm×2.1 mm, 2.7 μ m) under multiple chromatographic retention modes. Acetonitrile and 0.2% (v/v) acetic acid aqueous solution were used as mobile phases with gradient elution, and all the 10 groups of isomers were baseline separated. The qualitative identification and quantitative analysis of the 81 GCs were operated in the electrospray ionization positive mode using dynamic multiple reaction monitoring (DMRM). The 81 GCs finally were quantified by internal standard method. The correlation coefficients of linear calibration curves were greater than 0.99 in the corresponding mass concentration ranges. The average recoveries of the 81 GCs at three spiked levels ranged from 68.8% to 105.3% with relative standard deviations (RSDs) of 2.9%-13.1% (n=6). The LODs (S/N ≥ 3) and LOQs (S/N ≥ 10) were 0.002-0.006 μ g/g and 0.005-0.020 μ g/g, respectively. A number of 137 cosmetic samples submitted by customers were screened. Sixteen positive samples were found, and the contents of GCs were from 16.9 μ g/g to 158 μ g/g. The results showed that the new method is simple, rapid, sensitive and reliable, and it is suitable for qualitative and quantitative screening analysis of the 81 GCs in cosmetics simultaneously.