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

发布时间：2019-02-26 19:23

【摘要】：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。
[Abstract]:A rapid method for the simultaneous determination of 81 illegal corticosteroids (GCs) in cosmetics by dispersion solid-phase extraction liquid chromatography-tandem mass spectrometry was established. The samples were separated by water dispersion and ultrasonic extraction with acetonitrile. The samples were purified by octadecyl bonded silica gel (C18) and N-propyl ethylenediamine (PSA). The samples were separated on a Poroshell 120 PFP column (100 mm 脳 2.1 mm, 2.7 渭 m) with multiple chromatographic retention mode. Using 0.2% (vv) acetic acid aqueous solution-acetonitrile as mobile phase gradient elution, dynamic multi-reaction monitoring method was used in electrospray positive ion mode, and the internal standard method was used for quantitative analysis. 81 kinds of compounds were linear in their respective concentration range. The correlation coefficients were all more than 0.990.The average recovery was 68.8% and 105.3%, RSD was 2.9% and 13.1% (n = 6) at three different levels of addition, and the average recovery was 68.8% and 105.3% (RSD = 2.9% and 13.1%, n = 6), respectively. The detection limits and quantitative limits of the method were 0.002 ~ 0.006ug / g and 0.0050.020ug / g, respectively. The detection limit and quantitative limit were 0.0020.006ug / g and 0.0050.020ug / g, respectively. 137 cosmetics samples were screened and 16 positive samples were found, the content was 16.9 ~ 158 渭 g / g. The results showed that the method was simple, rapid, sensitive and reliable. It was suitable for the simultaneous qualitative and quantitative analysis of 81 kinds of GCs in cosmetics.
【作者单位】：中国广州分析测试中心广东省化学危害应急检测技术重点实验室;
【基金】：广东省省级科技计划项目(2014A040401038,2014B070705001)~~
【分类号】：O657.63;TQ658

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