摘要
建立了乳液、霜、水以及油类化妆品中25种邻苯二甲酸酯类化合物的气相色谱-质谱和液相色谱-质谱测定方法。不同基质样品经不同方法净化处理后,采用气相色谱-质谱或液相色谱-质谱进行测定。气相色谱-质谱法采用DB-5MS毛细管色谱柱(30 m,250 mm×0.25μm),程序升温,选择离子模式同时测定21种邻苯二甲酸酯类化合物。液相色谱-质谱采用MN EC-C18色谱柱(4.6×100 mm,2.7μm),以甲醇和0.1%甲酸为流动相,梯度洗脱,流速0.7 mL/min,采用电喷雾电离(ESI+),多反应监测(MRM)模式同时测定24种邻苯二甲酸酯类化合物。25种邻苯二甲酸酯类化合物的线性关系良好,相关系数均大于0.999,回收率实验结果为89.3%~105.6%,RSD为0.4%~4.0%,检出限均小于0.3 mg/kg。方法适用于化妆品中邻苯二甲酸酯类化合物的全面筛查。
A method for the determination of 25 phthalates esters in cosmetics was developed by GC/MS and LC/MS/MS,respectively.Different pretreatment methods were available for samples with different matrice.21 phthalates esters were separated on a DB-5MS capillary column(30 m,250 mm × 0.25 μm) by GC/MS,with temperature programming and selected ion mode.24 phthalates esters were separated on a EC-C18 column(4.6 ×100 mm,2.7 μm) by LC/MS/MS with positive electric spraying mode(ESI +) and determined with multireaction monitoring(MRM) mode.Gradient elution was employed by using methanol and 0.1% formic acid as the mobile phase.The flow rate was 0.7 mL/min.All of the phthalates esters showed good linearities with correlation coefficients greater than 0.999.The average recoveries were 9.3% ~ 105.6% with RSDs of 0.4% ~4.0%.The detection limits were less than 0.3 mg/kg.The methods can be applied to the phthalates esters screening of different cosmetics.
出处
《分析试验室》
CAS
CSCD
北大核心
2014年第7期864-868,共5页
Chinese Journal of Analysis Laboratory