超高效液相色谱-串联质谱法测定化妆品中三氯生和三氯卡班

Determination of Triclosan and Triclocarban in Cosmetics by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry

目的建立超高效液相色谱-串联质谱法分析化妆品中三氯生和三氯卡班的方法。方法样品用有机溶剂涡旋超声提取后,用甲醇定容。采用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×50 mm,1.7μm)分离,以甲醇-水为流动相,梯度洗脱。采用多反应监测(MRM)模式进行质谱确认,根据保留时间和特征离子的相对丰度比进行定性,外标法定量。结果三氯生和三氯卡班分别在5~500 ng/ml和0.5~50 ng/ml响应值与浓度呈良好线性关系,方法定量限分别为0.5μg/g和0.01μg/g。在阴性样品中加入低、中、高3个水平点,三氯生和三氯卡班平均回收率分别为96.8%~100.3%和92.8%~110.2%;相对标准偏差(RSD)分别为2.3%~8.8%和1.7%~4.5%。结论此法适用各剂型的化妆品,灵敏度高,重现性好,用于化妆品中三氯生和三氯卡班的检测具有良好的适应性。

Objective To develop a method based on ultra-performance liquid chromatography-tandem mass spectrometry(UPLC/MS-MS)for determination of triclosan and triclocarban in cosmetics.Methods After being vortexed and ultrasonically extracted with organic solvent,the sample was made to volume with methanol.The separation was carried out on a Waters ACQUITY UPLC BEH C18 column(2.1 mm×50 mm,1.7μm)using methanol and water as mobile phase,and gradient elution was adopted.Multi-reaction monitoring(MRM)mode was used for mass spectrometry confirmation.Qualitative analysis was carried out according to retention time and relative abundance ratio of characteristic ions,and quantitative analysis was carried out by external standard method.Results The response values of triclosan and triclocarban showed good linear relationships within the ranges of 5-500 ng/ml and 0.5-50 ng/ml,respectively,and the limits of quantitation were 0.5μg/g and 0.01μg/g,respectively.the average recoveries of the low,medium and high levels of triclosan and triclocarban added in the negative sample were 96.8%-100.3%and 92.8%-110.2%,respectively,and RSDs were 2.3%-8.8%and 1.7%-4.5%,respectively.Conclusion This method is suitable for various types of cosmetics,with high sensitivity and good reproducibility.It has good adaptability for the detection of triclosan and triclocarban in cosmetics.