高效液相色谱-质谱联用法测定洗涤用品中的壬基苯酚聚氧乙烯醚和辛基苯酚聚氧乙烯醚

Determination of Octylphenol Ethpxylates and Nonylphenol Ethoxylates in Laundry Detergents by High Performance Liquid Chromatography-Mass Spectrometey

建立了固相萃取净化技术结合高效液相色谱-质谱法同时测定洗衣粉和洗衣液等洗涤用品中的壬基苯酚聚氧乙烯醚和辛基苯酚聚氧乙烯醚的分析方法。样品经甲醇提取后，经HLB固相萃取小柱净化后，采用Inertsil ODS-SPC18（5μm，4．6＊150mmi．d．）色谱柱，以甲醇和0．05mmol／L乙酸铵溶液为流动相，电喷雾质谱在Q1检测模式下分析目标化合物，采用外标法定量。结果表明：壬基苯酚聚氧乙烯醚和辛基苯酚聚氧乙烯醚的平均加标回收率为88．8％～98．6％，相对标准偏差在3．1％～6．4％；方法检出限为2mg／L。将本方法用于市售的洗衣粉和洗衣液的检测发现，洗衣粉样品中壬基苯酚聚氧乙烯醚的检出率为16％，洗衣液中暂时未有检出。

A method for determining Octylphenol Ethpxylates and Nonylphenol Ethoxylates in the laundry detergents by High Performance Liquid Chromatography-Mass Spectrometey （HPLC-MS） is developed. The extraction and cleanup of the samples were performed on HLB solid-phase extraction cartridges. The targets were analyzed by HPLC-MS on Inertsil ODS-SP C18 column （5 μ m, 4.6＊150 mm i.d.） with electrosprey ionization in Q1 mode. The results showed that the average recoverires og targets cpmpounds were 88.8% -98.6% and the corresponding relative standard devia- tions were 3.1% - 6.4% ; The method limits of detection for compounds were 2 mg/L. Among the 25 powder and 15 liqi- ud detergents, the rate of positive sample of powder detergents was 16%.