超高效液相色谱-串联四极杆质谱测定酒中15种邻苯二甲酸酯

Determination of 15 phthalates in alcohol by ultra performance liquid chromatography-tandem mass spectrometry

利用超高效液相色谱-串联四极杆质谱技术建立了酒中15种邻苯二甲酸酯的快速检测方法。酒样经氯化钠盐析及液液萃取后氮吹至干,用流动相定容后测定。目标物经Agilent SB C18柱分离,以乙腈和15 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,采用选择离子扫描模式(MRM)进行检测。15种邻苯二甲酸酯CCα为0.8~3.4μg/L,CCβ为1.2~5.1μg/L,各目标物3个水平的日内重现性在82.6%~109.2%间,相对标准偏差为2.2%~14%,日间重现性在82.0%~109.6%间,相对标准偏差为2.6%~12%,方法可用于各类酒中邻苯二甲酸酯的日常监测。

A method was established for simultaneous determination of 15 phthalic acid esters （PAEs） in alcohol by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. Liquid-liquid extraction （LLE） approaches have been used for isolation of PAEs from alcohol samples, which were salted out by sodium chloride at the same time. After that, the extract solution was dried within nitrogen. In the chromatographic analysis, 15 target compounds were separated on an Agilent SB C18 column with gradient elution using mobile phase of acetonitrile and water containing 15 mmol/L ammonium acetate. Multiple reaction monitoring （MRM） acquisition under positive ion mode was performed. As a result, the detection limits （CCa） of the target compounds were from 0. 8p^g/L to 3.41xg/L in alcohol and the quantitation limits （CC/3） were from 1.2tμg/L to 5.1 μg/L. The intra-day precision of the 15 analytes spiked at three concentration levels ranged from 82. 6% to 109. 2% with the relative standard deviations （RSD） of 2.2% - 14% , while the inter-day precisions ranged from 82.0% to 109.6% with the RSD of 2. 6% - 12%. The method can be applied to the analysis of PAEs in alcohol.