饮料中邻苯二甲酸酯的分散式液液微萃取-高效液相色谱测定法

Simultaneous determination of phthalic acid esters in beverage by dispersive liquid-liquid microextraction/high-performance liquid chromatography

目的建立饮料中3种邻苯二甲酸酯（PAEs）的分散式液液微萃取-高效液相色谱测定法。方法以甲醇为分散剂,以四氯乙烯为萃取剂,饮料样品中PAEs经分散式液液微萃取（DLLME）富集,采用HITACHI-C18色谱柱,乙腈和水梯度洗脱分离后在203 nm检测。结果邻苯二甲酸丁卞酯（BBP）的线性范围为0.500~400.0 ng/ml（r=0.999 8）,邻苯二甲酸二丁酯（DBP）和邻苯二甲酸二异辛酯（DEHP）的线性范围均为0.250~200.0 ng/ml（r=0.999 3）,检出限均为0.05 ng/ml,回收率为85.3%~103.3%,相对标准偏差为2.4%~5.6%。结论该方法灵敏度、准确度高,适用于饮料样品中PAEs的检测。

Objective To develop a simple and highly sensitive analytical method for the determination of three phthalic acid esters （PAEs） in beverage samples. Methods PAEs in beverage samples were extracted by DLLME and separated by acetonitrile and water gradient elution system. A Hitachi-C18 column was used and the detection wavelength was 203 nm. Results Linearity was observed over the range of 0.500-400.0 ng/ml （r=0.999 8） for BBP and 0.250-200.0 ng/ml（r≥0.999 3） for DBP and DEHP; Limit of detection was 0.05 ng/ml for three PAEs. The recovery rates were 85.3%-103.3%, the relative standard deviations （RSDs） were 2.4%-5.6%. Conclusion The method is simple, rapid, accurate and applicable to the simultaneous determination of PAEs in beverage.