固相萃取-气相色谱-质谱联用法测定水产品中邻苯二甲酸酯的残留量

Determination of phthalate esters residue in aquatic products by solid phase extraction with gas chromatography-mass spectrometry

建立了测定水产品中常见的6种邻苯二甲酸酯类化合物（ PAEs）的气相色谱-质谱（GC-MS）分析方法。样品经环己烷：乙酸乙酯（V/V,1∶1）混合溶液超声提取,用乙腈饱和的正己烷除脂,再用正己烷饱和的乙腈反提,过PAE30006-C固相萃取小柱净化,用1%乙酸乙酯的正己烷淋洗,再用正己烷：乙酸乙酯（V/V,1∶1）混合溶液洗脱,洗脱液浓缩后,正己烷定容,供GC-MS测定。结果显示：6种邻苯二甲酸酯类化合物（ PAEs）在10-5000 ng/mL的线性范围内,相关系数在0．9992-0．9998,线性良好,检出限（ LOD ）在0．62-2．96μg/kg,定量限（ LOQ）在2．0-9．0μg/kg。选择罗非鱼样品为测试对象,按照10μg/kg、50μg/kg和100μg/kg 的添加量做加标回收试验,平均回收率在70．5%-105．4%之间,相对标准偏差在3．78%-7．57%之间；选用南美白对虾、草鱼、锯缘青蟹、大黄鱼和牡蛎样品对此方法进行验证,在添加浓度为50 ug/kg的水平上进行加标回收实验,6种PAEs的平均加标回收率在71．5%-102．5%之间,相对标准偏差在3．25%-7．86%之间。该方法提取效率高,净化效果好,可操作性强,符合水产品中药物残留检测的要求。

A method was developed for the determination of 6 common phthalate esters （ PAEs ） in aquatic products by gas chromatography-mass spectrometry （ GC-MS） . The PAEs were extracted by cyclohexane-ethyl acetate （1∶1） mixed solution, degreased by acetonitrile saturated n-hexane, then extracted by N-hexane saturation of acetonitrile, and purified by PAE30006-C SPE glass column, washed by 1% ethyl ace-tate and eluted by hexane-ethyl acetate （1∶1）, the eluent was concentrated and dissolved in hexane, and analyzed by GC-MS. The results showed that the linear range of 6 PAEs were 10-5 000 ng/mL, and the correlation coefficients were 0. 9992-0. 9998, limits of detection （LOD） were 0. 62-2. 96 μg/kg, limits of quantificat ions （LOQ ） were 2. 0 -9. 0 μg/kg, The average recovery of the added test in tilapia from 10, 50, 100 μg/kg was 70. 5% -105. 4%, and the relative standard deviations （ RSD） was 3. 78% -7. 57%. The average recovery of the added test with 50 ug/kg in pacific white shrimp, grass carp, mud crab, yellow croaker and oyster was 71. 5% -102. 5%, and the RSD was 3. 25% -7. 86%. The method was suitable for the determination of PAEs in aquatic products with high extraction efficiency and purification effect.