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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 |
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| DOI： |
| KeyWord:milk beverage phthalate esters salting-out assisted liquid－liquid extraction ultra performance liquid chromatography－tandem mass spectrometry |
| Author | Institution |
| WANG Dong-xu，WANG Xin-cai，HU Qi-jie，WANG Feng-li，LI Fen |
Huzhou Institute for Food and Drug Control，Huzhou ，China |
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| 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（NH4）2SO4 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（r2） 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. |
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