Determination of 12 Phthalate Esters in Milk Beverage Using Ultra Performance Liquid Chromatography－Tandem Mass Spectrometry with Salting-out Assisted Liquid－Liquid Extraction

WANG Dong-xu; WANG Xin-cai; HU Qi-jie; WANG Feng-li; LI Fen

doi:10.19969/j.fxcsxb.22052505

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Determination of 12 Phthalate Esters in Milk Beverage Using Ultra Performance Liquid Chromatography－Tandem Mass Spectrometry with Salting-out Assisted Liquid－Liquid Extraction

Scientific Papers | 更新时间：2023-01-04

- Determination of 12 Phthalate Esters in Milk Beverage Using Ultra Performance Liquid Chromatography－Tandem Mass Spectrometry with Salting-out Assisted Liquid－Liquid Extraction
- Journal of Instrumental Analysis Vol. 41, Issue 10, Pages: 1516-1522(2022)
- 作者机构：
  
  湖州市食品药品检验研究院，浙江湖州 313000
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22052505
  CLC：
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王东旭,王新财,胡奇杰等.盐析辅助液液萃取/超高效液相色谱－串联质谱法测定含乳饮料中12种邻苯二甲酸酯[J].分析测试学报,2022,41(10):1516-1522.

WANG Dong-xu,WANG Xin-cai,HU Qi-jie,et al.Determination of 12 Phthalate Esters in Milk Beverage Using Ultra Performance Liquid Chromatography－Tandem Mass Spectrometry with Salting-out Assisted Liquid－Liquid Extraction[J].Journal of Instrumental Analysis,2022,41(10):1516-1522.
王东旭,王新财,胡奇杰等.盐析辅助液液萃取/超高效液相色谱－串联质谱法测定含乳饮料中12种邻苯二甲酸酯[J].分析测试学报,2022,41(10):1516-1522. DOI： 10.19969/j.fxcsxb.22052505.

WANG Dong-xu,WANG Xin-cai,HU Qi-jie,et al.Determination of 12 Phthalate Esters in Milk Beverage Using Ultra Performance Liquid Chromatography－Tandem Mass Spectrometry with Salting-out Assisted Liquid－Liquid Extraction[J].Journal of Instrumental Analysis,2022,41(10):1516-1522. DOI： 10.19969/j.fxcsxb.22052505.

摘要

建立了基于盐析辅助液液萃取（SALLE）/超高效液相色谱－串联质谱（UPLC－MS/MS）技术检测含乳饮料中12种邻苯二甲酸酯的分析方法。样品采用乙腈提取，硫酸铵作为盐析剂，以苯基色谱柱分离，串联质谱正离子模式扫描，多反应监测模式检测。实验考察了萃取溶剂、盐析剂对萃取效率的影响。最优条件下，12种邻苯二甲酸酯在对应质量浓度范围内线性良好，相关系数（,r,2,）不小于0.997，检出限为0.03 ~ 0.6 μg/kg，定量下限为0.1 ~ 2.0 μg/kg；4种加标浓度下的回收率为70.8% ~ 111%，相对标准偏差为0.30% ~ 7.2%。同时考察了不同温度及光照下聚对苯二甲酸乙二醇酯（PET）包装材质含乳饮料中邻苯二甲酸酯的迁移量，结果表明高温（80 ℃）下邻苯二甲酸二丁酯（DBP）迁移最为显著。该方法操作简捷、成本低、准确度高，可以满足含乳饮料中12种邻苯二甲酸酯的分析要求。

Abstract

An ultra performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） with salting-out assisted liquid－liquid extraction（SALLE） was established for the simultaneous determination of 12 phthalate esters in milk beverage．The sample was firstly extracted with acetonitrile，then salted out with（NH,4,）,2,SO,4, and separated on a phenyl column，and finally analyzed by electrospray tandem mass spectrometry in positive ion and multiple reaction monitoring（MRM） mode．The extraction parameters affecting the SALLE procedure such as kind and volume of extracting solvent，type and amount of salt were optimized．Under the optimal conditions，the method showed a good linearity for 12 phthalate esters in the corresponding mass concentration ranges，with correlation coefficients（,r,2,） not less than 0.997．The detection limits and the quantitation limits for 12 phthalate esters were in the range of 0.03－0.6 μg/kg and 0.1－2.0 μg/kg，respectively．The spiked recoveries for 12 phthalate esters in milk beverage ranged from 70.8% to 111%，with the relative standard deviations of 0.30%－7.2%．The effects of temperature and light on phthalate esters migration from polythylene terephthalate（PET） plastic bottle were investigated．The results showed that the migration level of dibutyl phthalate（DBP） at high temperature（80 ℃） was significantly higher than that under other conditions．With simple operation，low cost and good accuracy，the established method could meet the requirements for monitoring the level of 12 phthalate esters in milk beverage.

关键词

含乳饮料邻苯二甲酸酯盐析辅助液液萃取超高效液相色谱－串联质谱

Keywords

milk beveragephthalate esterssalting-out assisted liquid－liquid extractionultra performance liquid chromatography－tandem mass spectrometry

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