Citation: XU Bingbing, LI Xiaomin, ZHANG Qinghe, ZHU Weihuang. Determination of 16 phthalate acid esters in infant formula by gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2018, 36(8): 786-794. doi: 10.3724/SP.J.1123.2018.03010 shu

Determination of 16 phthalate acid esters in infant formula by gas chromatography-tandem mass spectrometry

1.
School of Environmental and Municipal Engineering, Xi'an University of Architecture & Technology, Xi'an 710055, China;
2.
Division of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, China

Received Date: 8 March 2018

Fund Project: Financing Funding of National Institute of Metrology, China (No.21-AKY1619).

A method was established for the determination of 16 phthalate acid esters (PAEs) in infant formula by gas chromatography-tandem mass spectrometry (GC-MS/MS). PAEs in infant formula samples were homogenized by deionized water, extracted with acetonitrile, and purified by a solid-phase extraction (SPE) method using primary secondary amine (PSA) sorbents. The separation was performed on a DB-5 MS UI (30 m×0.25 mm×0.25 μm) capillary column. Effects of different elution solvents on alumina/PSA and PSA SPE columns were investigated. Fair recoveries of 16 PAEs were achieved on the PSA column upon elution by mixed n-hexane-acetone (60:40, v/v). All the 16 PAEs were quantified by matrix-matched isotopic-dilution mass spectrometry (IDMS); the 16 PAEs showed linear relationships in the concentration range of 0.01-2.0 mg/kg with linear coefficients (R²) greater than 0.9996. The limits of detection (LODs) and quantification (LOQs) were in the range of 0.15-2.5 μg/kg and 0.50-8.33 μg/kg, respectively. The recoveries of the 16 PAEs, obtained using the IDMS method, were 96.1%-104.0% with relative standard deviations (RSDs) lower than 3.3% (n=5). These results established the method described here as sensitive and precise for the simultaneous determination of 16 PAEs in infant formula, even at trace concentrations.
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沈阳化工大学材料科学与工程学院沈阳 110142