超高效液相色谱-串联质谱法同时测定化妆品中23种抗生素

Determination of 23 illegally added antibiotics by UPLC-ESI-Q-TOF/MS in cosmetics

建立了超高效液相色谱-串联质谱法同时测定化妆品中23种抗生素的检测方法。样品采用乙腈超声提取,经色谱柱分离,以0.1%甲酸溶液和0.1%甲酸-乙腈梯度洗脱,采用电喷雾离子源正离子模式(ESI+),利用Q-TOF获得的母离子建立含量测定方法,保留时间和二级质谱碎片用于进一步定性确证。结果表明,23种抗生素在线性范围内线性关系良好,相关系数均大于0.995;检出限为0.05~1.36μg/g,平均回收率为74.1%~125.5%,RSD为2.3%~13.2%。应用该方法对22批次样品进行筛查,首次检出了甲氧苄啶。该方法操作简便,具有良好的选择性、灵敏度及准确度,能够用于化妆品中抗生素类成分的测定。

The aim of the study is to develop an ultra high performance liquid chromatography-tandem mass spectrometry method for the identification and determination of 23 antibiotics in cosmetics.The samples were extracted by ultrasonic machine with acetonitrile,and the separation was executed on a column using a mobile phase consisting of 0.1%formic acid(A),and 0.1%formic acid-acetonitrile(B).The mass spectrometer was operated in positive ion mode,the determination was conducted in MS scan mode by the external standard method,and confirmatory analysis for target compounds was performed with the retention time and MS2 scan.The result show that the linear relationship of the 23 antibiotics in the linear range is good,and the correlation coefficient is greater than 0.995.The detection limit are between 0.05-1.36μg/g,and the average recovery rate is in the range of 74.1%-125.5%,with RSD within 2.3%-13.2%.One batch of positive sample is detected in 22 batches of the samples.Trimethoprim is detected in cosmetics for the first time.The established method is simple,selective,sensitive and accurate,and can be used for determination of antibiotics in cosmetics.