提出了超高效液相色谱-串联质谱法测定化妆品中水杨酸含量的方法。化妆品试样用甲醇溶解,振荡提取20 min,离心分离取上清液过ACQUITYTM BET C18色谱柱(2.1 mm×100 mm,1.7 μm)并用乙腈和甲酸-水(0.3+99.7)溶液(体积比6比4)的混合溶液作为流动相进行分离,串联质谱法进行测定。采用正离子模式多反应监测,同位素内标法定量。水杨酸的线性范围为1.0~5.0×103μg·L-1,方法的检出限(3S/N)为0.15 μg·L-1,测定下限(10S/N)为0.50 μg·L-1。方法用于分析8种化妆品试样,回收率在97.3%~107.0%之间,相对标准偏差(n=5)在2.0%~3.8%之间。

A rapid method of UPLC-MS/MS for the determination of salicylic acid in cosmetics was proposed. The sample was dissolved with methanol and extracted vortically for 20 min. After centrifugation, supernatant was taken for separation by using the column ACQUITYTM BET C18 (2.1 mm×100 mm, 1.7 μm) and using the mixed solution of acetonifrile and formic acid water solution (0.3+99.7), mixed in the ratio of 6 to 4, as mobile phase. The content of salicylic acid was determined by MS/MS. The positive electrospray ionization as well as multiple reactions monitoring mode was used in the detection. The isotope internal standard method was used for quantification of salicylic acid. Linearity range of salicylic acid was kept from 1.0 to 5.0×103μg·L-1, with limit of detection (3S/N) of 0.15 μg·L-1 and limit of determination (10S/N) of 0.50 μg·L-1. The proposed method was applied to the analysis of 8 cosmetic samples, giving values of recovery in the range from 97.3%-107.0% and RSD (n=5) in the range from 2.0%-3.8%.