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目的建立醋和黄酒中13种邻苯二甲酸酯类塑化剂的超高效液相色谱-串联质谱测定方法。方法样品加入适量盐后,经乙酸乙酯-正己烷(1∶1,V/V)提取,涡旋离心后,吸取上清液浓缩吹干,用甲醇定容后进液相色谱-串联质谱系统分析,内标法定量。色谱柱采用Agilent EC-C18柱(2.1 mm×75 mm,2.7μm),流动相为甲醇-0.1%甲酸,进行梯度洗脱;质谱采用电喷雾离子源,在正离子多反应监测模式下进行检测。结果 13种邻苯二甲酸酯类塑化剂在10 ng/ml~500 ng/ml线性关系良好(r≥0.995 0);检出限和定量限分别为0.1 ng/ml~0.8 ng/ml和0.3 ng/ml~2.5 ng/ml;低、中、高3种浓度(20 ng/ml、100 ng/ml、500 ng/ml)的回收率分别为90.2%~114.2%、97.1%~114.3%、94.7%~107.0%,精密度(RSD)分别为3.1%~13.0%、4.5%~12.1%、3.8%~9.4%。结论该方法简便、灵敏、准确、稳定,适用于醋和黄酒中邻苯二甲酸类塑化剂的测定。
Objective To establish a method for the determination of 13 phthalate plasticizers in vinegar and rice wine by ultra performance liquid chromatography-tandem mass spectrometry. Methods After adding appropriate amount of salt, the sample was extracted with ethyl acetate-n-hexane (1: 1, V / V), vortexed and centrifuged. The supernatant was aspirated and concentrated to dryness, fixed with methanol and subjected to liquid chromatography-tandem mass spectrometry Analysis, internal standard method. The column was eluted with an Agilent EC-C18 column (2.1 mm × 75 mm, 2.7 μm) using a mobile phase of methanol-0.1% formic acid and eluted with a gradient elution mass spectrometer. Electrospray ionization (ESI) . Results The linearity of 13 phthalate plasticizers was between 10 ng / ml and 500 ng / ml (r≥0.995 0). The limits of detection and limit of quantification were 0.1 ng / ml ~ 0.8 ng / ml and 0.3 ng / ml ~ 2.5 ng / ml. The recoveries of low, medium and high concentrations of 20 ng / ml, 100 ng / ml and 500 ng / ml were 90.2% ~ 114.2% and 97.1% ~ 114.3% , 94.7% ~ 107.0%, RSD were 3.1% ~ 13.0%, 4.5% ~ 12.1%, 3.8% ~ 9.4% respectively. Conclusion The method is simple, sensitive, accurate and stable and is suitable for the determination of phthalate plasticizers in vinegar and rice wine.