皮革中烷基酚聚氧乙烯醚含量的高效液相色谱质谱法测定

Determination of Alkylphenol Ethoxylates in Leather by High Performance Liquid Chromatography-Mass Spectrometry

该文建立一种测定皮革制品中烷基酚聚氧乙烯醚的高效液相色谱质谱(HPLC-MS)分析方法.采用甲醇溶剂对样品进行超声提取,经滤膜过滤后直接进样,正离子选择离子监测模式进行定性和定量分析.结果表明:辛基酚聚氧乙烯醚和壬基酚聚氧乙烯醚在0.05~2 mg/L浓度范围内具有良好的线性关系,相关系数(r^(2))均在0.999以上,方法检出限分别为0.42 mg/kg和0.54 mg/kg.在3个加标水平下的平均回收率分别为79.5%~90.7%和83.0%~119.5%,相对标准偏差(RSD,n=6)分别为2.4%~3.2%和0.3%~4.3%.该检测方法具有简捷、准确、稳定可靠等特点,可用于皮革制品中烷基酚聚氧乙烯醚的分析检测.

A method for the determination of alkylphenol polyoxyethylene ether in leather products by high performance liquid chromatography-mass spectrometry(HPLC-MS)was established.The samples were extracted by ultrasonic with methanol solvent,directly injected after filtration by filter membrane,and analyzed qualitatively and quantitatively by positive ion selective ion monitoring mode.The results showed that octylphenol polyoxyethylene ether and nonylphenol polyoxyethylene ether had a good linear relationship in the concentration range of 0.05~2 mg/L,the correlation coefficient(R^(2))was more than0.999,and the detection limits were 0.42 mg/kg and 0.54 mg/kg,respectively.The average recoveries at the three spiked levels were 79.5%~90.7%and 83.0%~119.5%respectively,and the relative standard deviations(RSD,n=6)were 2.4%~3.2%and 0.3%~4.3%respectively.The method is simple,accurate,stable and reliable.It can be used for the analysis of alkylphenol polyoxyethylene ether in leather products.