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目的建立气相色谱-三重四级杆质谱法(GC-QqQ MS)测定肥胖儿童血清中6种邻苯二甲酸酯类(PAEs)。方法血清样品经乙醇沉定蛋白、正己烷提取后,利用GC-QqQ MS进行测定。结果 6种PAEs(邻苯二甲酸二甲酯,邻苯二甲酸二乙酯,邻苯二甲酸二丁酯,邻苯二甲酸丁基苄基酯,邻苯二甲酸(2-乙基己基)酯,邻苯二甲酸二正辛酯)在1~200μg/L浓度范围内线性良好,相关系数(r值)均大于0.999。终浓度分别为5、25和50μg/L的基质加标实验显示6种PAEs平均回收率在79.1%~93.0%之间,相对标准偏差(RSD%,n=3)在1.4%~6.9%之间。方法定量限低于现有的相关报道,其中DBP和DEHP的最低定量限分别为0.5μg/L和0.8μg/L,其余PAEs最低定量限为0.2μg/L。肥胖儿童血清测定结果显示,血清中不同程度检出PAEs,其中DEHP的检出率和含量范围分别为100%和10μg/L~400μg/L(n=30)。结论该法前处理选择性好、灵敏度高、简单、快速,适用于肥胖儿童血清中PAEs的测定。
Objective To establish a gas chromatography-triple quadrupole mass spectrometry (GC-QQQ MS) for the determination of six phthalates (PAEs) in obese children. Methods Serum samples were extracted with ethanol and n-hexane, then determined by GC-QqQ MS. Results Six PAEs (dimethyl phthalate, diethyl phthalate, dibutyl phthalate, butyl benzyl phthalate, (2-ethylhexyl) phthalate) Ester and phthalic acid di-n-octyl ester) showed a good linearity in the concentration range of 1 ~ 200μg / L with the correlation coefficient (r value) greater than 0.999. Matrix spiked experiments at final concentrations of 5, 25 and 50 μg / L showed that the average recoveries of six PAEs ranged from 79.1% to 93.0% with relative standard deviations (RSD%, n = 3) ranging from 1.4% to 6.9% between. The limit of quantification of the method was lower than the existing reports. The lowest limit of quantification (DBP) and DEHP (0.5μg / L and 0.8μg / L) was the lowest, and the lowest limit of quantification was 0.2μg / L. Serum samples from obese children showed that PAEs were detected in different sera. The detection rate and range of DEHP were 100% and 10μg / L ~ 400μg / L respectively (n = 30). Conclusion The pretreatment of this method has good selectivity, high sensitivity, simple and rapid, and is suitable for the determination of PAEs in obese children.