气相色谱-三重四极杆串联质谱法同时测定乳粉中22种邻苯二甲酸酯

王金翠; 王晰锐

doi:10.13386/j.issn1002-0306.2021060214

气相色谱-三重四极杆串联质谱法同时测定乳粉中22种邻苯二甲酸酯

Simultaneous Determination of 22 Phthalate Esters in Milk Powder by GC-MS/MS

摘要

摘要: 建立了气相色谱-三重四极杆串联质谱法测定乳粉中22种邻苯二甲酸酯含量的方法。乳粉样品以水溶解，通过乙腈提取，以氯化钠盐析后，采用气相色谱-三重四极杆串联质谱的多反应监测模式（MRM）进行定量分析。结果表明，采用基质匹配标准曲线，在5~500 ng/mL范围内，22种邻苯二甲酸酯线性关系良好，相关系数(r)均大于0.99，方法检出限在1.0~5.0 μg/kg范围，定量限在3.0~15.0 μg/kg范围。在奶粉基质中3个加标水平下邻苯二甲酸酯的平均回收率在82.4%~111.4%之间，平行测定6次相对标准偏差（RSD）为2.4%~9.5%。该方法高效便捷、灵敏度高、稳定性好，适用于乳粉中22种邻苯二甲酸酯检测。

Abstract: A suitable GC-MS/MS method was established for the determination of 22 phthalate esters (PAEs) in milk powder. The milk powder samples were dissolved in water, extracted by acetonitrile, salted out by NaCl, then quantitated by GC-MS/MS in multiple reaction monitoring mode (MRM). As a result, 22 PAEs possessed an excellent linear relation by using matrix-matched standard curve under 5~500 ng/mL, the correlation coefficients were all greater than 0.99, LODwas 1.0~5.0 μg/kg, LOQ was 3.0~15.0 μg/kg. The recoveries were 82.4%~111.4% at three spiked level with relative standard deviation (n=6) of 2.4%~9.5%. This analytical method is simple, quick, sensitive and stable, which can be used for a monitoring and screening analysis of 22 PAEs in milk powder.