QuEChERS-同位素稀释-液相色谱-高分辨飞行时间质谱法高通量筛查化妆品中86种糖皮质激素

建立了QuEChERS-同位素稀释-液相色谱-四极杆串联飞行时间质谱同时快速筛查化妆品中86种糖皮质激素(Glucocorticoids, GCs)的高通量方法.样品经乙腈提取,改进的QuEChERS法净化,待测物选用具有多重色谱保留机理的新型色谱柱Poroshell 120 PFP (100 mm×2.1 mm,2.7 μm),以0.2% (V/V)乙酸和乙腈为流动相进行梯度洗脱分离,在电喷雾离子源的正离子模式下建立了一级精确质量数及二级碎片离子质谱图数据库,无需标准品即可完成化妆品中86种GCs的全面筛查与确证.所有待测物在2~200 μg/L浓度范围内线性良好,相关系数均大于0.99, 3个添加水平的平均回收率为66.2%~112.8%,相对标准偏差(RSD)为4.6%~13.9%,检出限(LOD,S/N≥3) 为0.006~0.015 mg/kg,定量限(LOQ,S/N≥10)为0.02~0.05 mg/kg.本方法简便高效、定性可靠、定量准确,适用于化妆品中非法添加GCs的高通量筛查.

High Throughput Screening of 86 Kinds of Glucocorticoids in Cosmetics Using QuEChERS and Isotope Dilution-Liquid Chromatography Copuled to High Resolution Time-of-Flight Mass Spectrometry

A high throughput screening method based on QuEChERS purification and stable isotope dilution-liquid chromatography coupled to high resolution time-of-flight mass spectrometry was developed for the simultaneous rapid determination of 86 kinds of glucocorticoids (GCs) in cosmetics.The analytes were extracted by acetonitrile, and then the extracts were purified using an improved QuEChERS method.The chromatographic separation was performed on a novel multiple chromatographic retention mechanisms column of Poroshell 120 PFP (100 mm × 2.1 mm, 2.7 μm) with gradient elution using 0.2% (V/V) acetic acid and acetonitrile as mobile phase.The accurate mass database of parent ions and mass spectra library of fragment ions of 86 GCs were established under positive ionization mode with electrospray ionization source.Based on the method described above, the qualitative identifications of the 86 GCs were accomplished without the contrast of standard substances.The results demonstrated that the linear range of this method was from 2 μg/L to 200 μg/L with good correlation coefficients of R2>0.99.The average recoveries of the 86 GCs ranged from 66.2% to 112.8%, and the relative standard deviation (RSDs) was 4.6%-13.9% at three different spiked levels.The limit of detection (LOD) and quantification (LOQ) were 0.006-0.015 mg/kg and 0.02-0.05 mg/kg, respectively.The method is simple, efficient, reliable and accurate, and is suitable for high throughput screening of 86 GCs added illegally in cosmetics.