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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 gas chromatographic method for the determination of phthalates in foods by internal standard method. Methods Phthalates in food were extracted with n-hexane or acetonitrile. The extracts were purified by silica gel / PSA solid-phase extraction (SPE) column, concentrated, and fixed in n-hexane. Gas chromatography-mass spectrometry Quantitative determination of standard method, and the method of precision, accuracy and detection limits to verify. Results 16 kinds of phthalate compounds had good linearity in the corresponding concentration range, the correlation coefficient was 0.995-1.000, the lowest detection concentration was 0.05 mg / L ~ 0.15 mg / L, 16 kinds of phthalate compounds The spiked recoveries ranged from 81% to 118% with relative standard deviations of 5.6% to 13.9% (n = 6). Conclusion The method is simple, rapid, sensitive and stable, and the technical indexes meet the need of phthalate in food.