超高效液相色谱-串联质谱法测定化妆品中27种磺胺类药物

Determination of 27 sulfonamides in cosmetics by ultra-high performance liquid chromatography-tandem mass spectrometry

建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定化妆品中27种非法添加磺胺类药物的分析方法。样品经甲醇提取,用Thermo Hypersil GOLD(100×2.1 mm,1.9μm)色谱柱分离,以0.1%(V/V)乙酸水溶液-0.1%(V/V)乙酸乙腈溶液为流动相梯度洗脱,在电喷雾正、负离子模式下以多反应监测(MRM)方式对化妆品中的27种磺胺类药物进行定性定量测定。27种待测组分在各自的质量浓度范围内线性关系良好,相关系数均大于0.99,在3个不同添加水平下,平均回收率为79.3%~112.2%,RSD为1.4%~13.1%(n=6),方法的检出限(S/N≥3)和定量限(S/N≥10)分别为2.3~97.6μg/kg和7.7~322.0μg/kg。该方法简单快速,灵敏可靠,适用于化妆品中27种磺胺类药物的同时定性定量筛查分析。

The study aims to establish an analytical method for determination of 27 illegally added sulfonamides in cosmetics by ultra-high performance liquid chromatography-tandem mass spectrometry.The samples were extracted by methanol,and separated on Thermo Hypersil GOLD column(100×2.1 mm,1.9μm),0.1%(V/V)acetic acid aqueous solution and 0.1%(V/V)acetic acid acetonitrile solution were used as mobile phases with gradient elution.The quantitative analysis of 27 sulfonamides were operated in the electrospray ionization positive/negative mode using multiple reaction monitoring(MRM).The correlation coefficients of linear calibration curves are greater than 0.99 in the corresponding mass concentration ranges of the 27 sulfonamides.The average recoveries of the 27 sulfonamides at three spiked levels range from 79.3%to 112.2%with the relative standard deviations of 1.4%-13.1%(n=6).The LODS(S/N≥3)and LOQS(S/N≥10)are 2.3-97.6μg/kg and 7.7-322.0μg/kg,respectively.The results show that this method is simple,rapid,sensitive and reliable.It is suitable for qualitative and quantitative screening analysis of the 27 sulfonamides in cosmetics simultaneously.