QuEChERS-超高效合相色谱-串联质谱法测定化妆品中45种糖皮质激素

Determination of 45 glucocorticoids in cosmetics by QuEChERS-ultra performance convergence chromatography-tandem mass spectrometry

建立了QuEChERS处理,超高效合相色谱-串联质谱(UPC2-MS/MS)测定化妆品中45种糖皮质激素(GCs)含量的方法。样品经NaCl饱和溶液分散、乙腈涡旋提取、QuEChERS法净化后,以Torus 2-PIC色谱柱(100 mm×3.0 mm,1.7μm)为分析柱,以超临界CO2为主要流动相,0.1%(V/V)甲酸甲醇溶液为共溶剂梯度洗脱,以97%甲醇溶液(V/V,含0.1%甲酸)为补偿液,电喷雾电离源的三重四极杆质谱在正离子、多反应监测模式下测定,外标法定量。结果表明:45种GCs在0.20~100μg/L浓度范围内线性关系良好(R^(2)≥0.9935),检出限为0.05~0.10μg/kg,定量限为0.15~0.30μg/kg;在3个加标水平下的平均回收率为74.4%~110.7%,相对标准偏差为2.9%~11%。该法为化妆品中多种GCs的测定提供了技术支持。

A method based on QuEChERS and ultra performance convergence chromatography-tandem mass spectrometry(UPC2-MS/MS)was established for the determination of 45 kinds of glucocorticoids(GCs)in cosmetics.The samples were dispersed in saturated NaCl solution,and extracted by acetonitrile.The extractions were purified by QuEChERS adsorbents,and separated on a Torus 2-PIC column(100 mm×3.0 mm,1.7μm)under gradient elution.Supercritical carbon dioxide was used as the main mobile phase,and 0.1%(V/V)formic acid methanol was used as the co-solvent.The separated compounds were analyzed by tandem MS with electrospray ionization source in positive and multiple reaction monitoring modes.Methanol(containing 3%water and 0.1%formic acid)was used as the auxiliary pump mobile phase.External standard method was used for quantitative analysis.The method showed good linear relationships in the range of 0.20-100μg/L(R^(2)≥0.9935).The limits of detection(LODs)and limits of quantification(LOQs)were 0.05-0.10μg/kg and0.15-0.30μg/kg,respectively.The average recoveries at the three spiked levels were in the range of 74.4%-110.7%.The relative standard deviations were in the range of 2.9%-11%.The method provided an effective way to determine the contents of GCs in cosmetics.