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目的建立同位素稀释-气相色谱质谱法同时测定酸奶和乳饮料中17种邻苯二甲酸酯的方法。方法加入16种氘代内标的样品经乙腈涡旋提取,过SILICA/PSA玻璃固相萃取柱净化,收集液氮气吹干后用正己烷复溶,气相色谱质谱选择离子监测模式(SIM)测定,内标法定量。结果 DINP在0.25~10.0μg/m L、其他16种邻苯二甲酸酯在0.01~1.0μg/m L的范围内线性相关系数≥0.999;方法检出限为0.005~0.30mg/kg。酸奶基质加标回收率为72.9%~114.5%,相对标准偏差(RSD)为0.5%~10.5%;乳饮料基质加标回收率为84.7%~119.3%,相对标准偏差(RSD)为0.2%~13.8%。结论本法快速、准确、灵敏,可用于酸奶和乳饮料中17种邻苯二甲酸酯的测定。
Objective To establish a method for the simultaneous determination of 17 phthalates in yogurt and milk beverages by isotope dilution-gas chromatography-mass spectrometry. Methods Sixteen samples of deuterated internal standard were extracted by acetonitrile vortex and purified by SILICA / PSA glass solid phase extraction column. The collected solution was dried with nitrogen, reconstituted with n-hexane and determined by gas chromatography-mass spectrometry with selected ion monitoring mode (SIM) Internal standard method. Results The linear correlation coefficient of DINP ranged from 0.25 to 10.0 μg / mL and the other 16 phthalates ranged from 0.01 to 1.0 μg / mL. The detection limit was 0.005-0.30 mg / kg. The recoveries of yogurt matrix were 72.9% -114.5% with relative standard deviations (RSDs) of 0.5% -10.5%. The spiked recoveries of milk beverage bases were 84.7% -119.3% with relative standard deviations (RSDs) of 0.2% 13.8%. Conclusion This method is fast, accurate and sensitive and can be used for the determination of 17 kinds of phthalates in yogurt and milk drinks.