超高效液相色谱-串联质谱法测定酒中23种邻苯二甲酸酯残留

Determination of 23 Kinds of Phthalate Ester Residues in Liquor by UPLC-MS

建立了液相色谱质谱联用法同时测定酒中污染物23种邻苯二甲酸酯类增塑剂残留量的检测方法。样品经过沸水加热除去乙醇后，正己烷提取，经Waters ACQUITY UPLC？ BEH C18色谱柱分离，以甲醇和0.1%甲酸溶液为流动相梯度洗脱，电喷雾正离子模式离子化，选择反应监测方式监测，串联质谱测定，外标法定量。结果显示，各目标物在0.1～10.0 mg/L浓度范围内的线性关系良好，相关系数大于0.993。该方法对酒中23种邻苯二甲酸酯化合物的定量限为0.1 mg/kg，23种邻苯酸二甲酸酯的回收率为87%～102%。结果表明，该方法简便快速、灵敏可靠、经济有效，适用于酒中污染物邻苯二甲酸酯检测的需要。

The residual quantity of 23 kinds of p hthalate esters in liquor was measured simultaneously by UPLC-MS. Firstly, liquor sample was heated by boiling water to remove ethanol, then extracted with n-hexane, and then isolated by centrifugation, the separation was perfomed on a Waters ACQUITY UPLC？ BEH C18 column with aradient elution using methanol and 0.1%formic acid, and the electrospray ionization （ESI） source in positive ion mode was used for multiple reaction monitoring （RSM）, then tandem MS was used for the measurement, and the external standard method was used for the quantification.The measurement results suggested that, the linear relationship of each phthalate ester was good within the range between 0.1~10.0 mg/kg and the correlation coefficient was above 0.993. The detection limits of such method were 0.1~0.5 mg/kg. The recoveries of 23 kinds of phthalate esters were ranged from 87.5%~101.2%with the relative standard deviations of 1.7%~5.8%. Such method was easy,fast,sensitive,and suitable for the determination of 23 kinds of phalate esters in liquor samples.