液相色谱-串联质谱高通量检测酸乳中多种塑料添加剂的迁移量

文章建立了一种液相色谱-串联质谱(Liquid chromatography tandem mass spectrometry,LC-MS/MS)高通量检测酸乳中多种塑料添加剂迁移量的方法。以乙酸乙酯为提取溶剂,超声提取两次,每次10 min,离心分离取上清液,氮吹至近干后用甲醇复溶,过有机滤膜后进LC-MS/MS检测;使用Eclipse plus C;RRHD色谱柱,5 mmol/L乙酸铵水溶液-甲醇为流动相,梯度洗脱,串联质谱以电喷雾离子源正、负离子模式下电离,多反应监测模式下定性和定量分析33种目标物;经过方法学验证,33种目标物的工作曲线线性范围内相关性良好(R;>0.99),加标回收率在94.90%~103.57%,精密度(RSD%)在1.57%~7.43%。应用该方法对10种酸乳样品进行了检测分析,有5种塑料添加剂检出,分别是3种塑化剂和2种抗氧化剂。所以新建的检测方法适合酸乳中多种塑料添加剂的高通量检测,而且灵敏度高、检测结果准确、稳定,前处理过程简单、高效,易操作。

High Throughput Determination of Migration of Several Plastic Additives in Yogurt by Liquid Chromatography-Tandem Mass Spectrometry

In this paper,a high throughput liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of plastic additives in yogurt.Ethyl acetate was used as extraction solvent and extracted twice,and the supernatant was extracted by ultrasonic for 10 min.The supernatant was extracted by centrifugation.After the nitrogen was blown to dry,the supernatant was re-dissolved with methanol and then passed through organic filtration membrane for detection.Using Eclipse plus C;RRHD column,5 mmol/L ammonium acetate aqueous solution-methanol as mobile phase,gradient elution,tandem mass spectrometry with electrospray ionization in positive and negative ion modes,multiple reaction monitoring mode (MRM) for qualitative and quantitative analysis of a variety of target compounds.The results showed that the linear range of the 33 targets was good (R;>0.99),the recovery was between 94.90%~103.57%,and the standard deviation (RSD%) was in the range of 1.57%~7.43%.The method was used to detect 10 kinds of yoghurt samples and five kinds of plastic additives were detected,including three kinds of plasticizers and two kinds of antioxidants.Therefore,the new detection method was suitable for the high throughput detection of a variety of plastic additives in yogurt,with high sensitivity,stable and accurate detection results,simple pretreatment,high efficiency and easy operation.