| 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 |
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| 基金项目:国家质检总局科技计划项目(2015QK165) |
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| 中文摘要: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-C18(4.6mm×150mm，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。 |
| 中文关键词:液相色谱-质谱联用法(LC-MS/MS) 分散固相萃取(d-SPE) 化妆品 氨基苯甲醚类化合物 |
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| Determination of Seven Aminoanisoles in Cosmetics by Dispersive Solid Phase Extraction Purification Coupled with Liquid Chromatography-Tandem Mass Spectrometry |
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| Abstract: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(4.6mm×150mm,5μm) 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 0.10-200.0μg/L, with correlation coefficients(r2) greater than 0.998.The limits of detections(LODs) were in the range of 0.4-10.9μg/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 5.3μg/kg. The method is accurate and reliable, and could be used for the simultaneous determination of 7 aminoanisoles in cosmetics. |
| Key Words:liquid chromatography tandem mass spectrometry(LC-MS/MS) dispersive solid phase extraction(d-SPE) cosmetics aminoanisole |
| 引用本文：黄嘉乐，李秀英，寻知庆，王强，黄金凤，郭新东.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[J].分析测试学报,2017,36(7):858-864. |
| 摘要点击次数: 2014 |
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