气相色谱-质谱联用内标法测定食品中邻苯二甲酸酯

Determination of phthalic acid esters in food by gas chromatography-mass spectrometry with internal standard method

目的建立内标法测定食品中邻苯二甲酸酯的气相色谱质谱方法。方法食品中邻苯二甲酸酯被正己烷或乙腈萃取,萃取液经硅胶/PSA固相萃取柱净化、浓缩、正己烷定容,进行气相色谱-质谱分析,以选择离子监测方式分析,以内标法定量测定,并对方法的精密度、准确度和检测限进行验证。结果 16种邻苯二甲酸酯化合物在对应的浓度范围内线性较好,相关系数为0.995~1.000,最低检测浓度为0.05 mg/L^0.15 mg/L,16种邻苯二甲酸酯化合物加标回收率为81%~118%,相对标准偏差为5.6%~13.9%(n=6)。结论该方法简便、快速、灵敏、稳定,各项技术指标满足食品中邻苯二甲酸酯的检测需要。

Objective To establish a method for determination of phthalic acid esters in food by gas chromatography-mass spectrometrywith internal standard method. Methods The phthalic acid esters in food were extracted with n-hexane or acetonitrile,and extracts were enriched and purified with silica / PSA column,then diluted with n-hexane,finally tested by GC-MS under selection ion monitoring mode and quantified with intemal standard method. In addition,the precision,accuracy and detection limit of the assay were evaluated. Results The 16 PAEs showed good linearity in a certatin concentration range,with correlation coefficients（ R） of 0. 995 - 1. 000 and the lowest detection concentration was 0. 05 mg / L - 0. 15 mg / L. The standard recoveries of the 16 PAEs in food were 81% - 118%,and the relative standard deviations were 5. 6% - 13. 9%（ n = 6）. Conclusion The method is simple,rapid,sensitive and stable,and each index of the method is available for the test requirements of PAEs in food.