固相萃取-超高效液相色谱串联质谱法测定饮用水中15种邻苯二甲酸酯

Determination of 15 Phthalate Esters in Drinking Water by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了饮用水中15种邻苯二甲酸酯的固相萃取超高效液相色谱串联质谱测定方法。样品经C18固相萃取柱富集,以苯基柱分离,以甲醇和水为流动相进行梯度洗脱,正离子模式下质谱多反应监测（MRM）模式检测,外标法定量。结果表明,邻苯二甲酸二丁酯在0.63~1000μg/L,其余14种邻苯二甲酸酯在0.002~500μg/L范围内线性关系良好,相关系数均大于0.9970。本方法对15种邻苯二甲酸酯的定量限为2.2~632 ng/L,回收率在81.3%~109%之间,RSD〈14%。

A method of solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry （SPE-UPLC/MS/MS） was developed for the determination of 15 phthalate esters. Drinking water samples were concentrated by C18 SPE cartridge. The fifteen phthalate esters were separated on a phenyl column with gradient elution using methanol and water as mobile phases. Multiple reaction monitoring （MRM） acquisition under positive ion mode was performed. The external matrix standard solutions were used for the quantitative determination. The linear range of Di-n-butyl phthalate was 0.63- 1000μg/L. The other 14 phthalate esters showed good linearity in the range of 0.002-500 μg/L with the correlation coefficients more than 0.9970. The limits of quantification （LOQ） were 2.2-632 ng/L. The spiked recoveries ranged from 81.3% to 109%. The relative standard deviations were less than 14%.