分散固相萃取净化/液相色谱-串联质谱法测定化妆品中7种氨基苯甲醚

建立了同时测定化妆品中7种氨基苯甲醚类化合物(邻氨基苯甲醚、间氨基苯甲醚、对氨基苯甲醚、2,4-二氨基苯甲醚、2,5-二氨基苯甲醚、3,4-二氨基苯甲醚、3,3'-二甲氧基联苯胺)的分散固相萃取净化液相色谱-串联质谱(LC-MS/MS)分析方法。样品用甲醇-水(1∶1,含0.1%甲酸)溶液提取,经PSA分散固相萃取净化后,样液经Welch Ultimats XB-C_(18)(4.6 mm×150 mm,5μm)色谱柱分离,多反应监测(MRM)模式检测,以保留时间和特征离子对定性,外标法定量。结果表明,7种氨基苯甲醚类化合物在0.10~200.0μg/L浓度范围内线性关系良好,相关系数均大于0.998;方法检出限(S/N=3)为0.4~10.9μg/kg。样品日内回收率为64.7%~98.1%,相对标准偏差(RSD,n=6)为1.2%~10.6%;日间精密度(n=5)为2.3%~9.8%。对30个不同水剂类化妆品检测发现,其中1个样品检出3,3'-二甲氧基联苯胺,含量为5.3μg/kg。该方法准确可靠,适用于化妆品中7种氨基苯甲醚的同时测定。

Determination of Seven Aminoanisoles in Cosmetics by Dispersive Solid Phase Extraction Purification Coupled with Liquid Chromatography-Tandem Mass Spectrometry

A dispersive solid phase extraction (d-SPE) purification coupled with liquid chromatography tandem mass spectrometric (LC-MS/MS) method was developed for the simultaneous determination of seven aminoanisoles including 2-anisidine (2-ANI),3-anisidine (3-ANI),4-anisidine (4-ANI),2,4-diaminoanisole(2,4-DANI),2,5-diaminoanisole(2,5-DANI),3,4-diaminoanisole(3,4-DANI) and 3,3'-dimethoxybenzidine(3,3'-DMBD) in cosmetics.The samples were extracted with methanol aqueous solution containing 0.1％ formic acid,and purified by a simple d-SPE employing PSA as adsorbents.The target analytes were separated on a Welch Ultimate XB-C18 chromatographic column(4.6 mm× 150 mm,5 μm) and subsequently detected through an electrospray ionization (ESI) source in the positive mode under multi-reaction monitoring (MRM) conditions.An external standard method was adopted for the quantification.Under the optimized conditions,the callibration curves of seven analytes were linear in the concentration range of 0.10-200.0 μg/L,with correlation coefficients (r2) greater than 0.998.The limits of detections (LODs) were in the range of 0.4-10.9 μg/kg.The average recoveries were calculated to be between 64.7％ and 98.1％,with relative standard deviations(RSDs) of 1.2％-10.6％ for intra-day precision (n =6) and 2.3％-9.8％ for inter-day precision(n =5).The method was successfully applied in the determination of aminoanisole contents in thirty complex cosmetics samples,and 3,3'-dimethoxybenzidine (3,3'-DMBD) was detected in one sample with a content of 5.3 μg/kg.The method is accurate and reliable,and could be used for the simultaneous determination of 7 aminoanisoles in cosmetics.