Citation: LI Rong, BO Yanna, LU Junwen, LIN Qinbao, HUANG Zhiqiang, CHEN Lisi. Determination of 28 phthalate esters in baked foods by gas chromatography-triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography, ;2016, 34(5): 502-511. doi: 10.3724/SP.J.1123.2015.12035 shu

Determination of 28 phthalate esters in baked foods by gas chromatography-triple quadrupole mass spectrometry

LI Rong ¹ ,
BO Yanna ^2,3 ,
LU Junwen ¹ ,
LIN Qinbao ³ ,
HUANG Zhiqiang ^2,, ,
CHEN Lisi ¹

1.
1. Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528400, China;
2.
2. Hunan Academy of Inspection and Quarantine, Changsha 410004, China;
3.
3. Key Laboratory of Product Packaging and Logistics of Guangdong Higher Education Institutes, Institute of Packaging Engineering, Jinan University, Zhuhai 519070, China

Corresponding author: HUANG Zhiqiang,
Received Date: 23 December 2015

Fund Project: 国家科技支撑计划课题(2012BAK08B01) (2012BAK08B01)广东省省级科技计划项目(2014A040401011) (2014A040401011)国家质检总局科技计划项目(2015IK260) (2015IK260)中山市社会公益重大专项(2015B2295). (2015B2295)

An efficient method using gas chromatography-triple quadrupole mass spectrometry for the determination of 28 phthalate ester residues in bakery foods was established. The samples were extracted with ethyl acetate, and cleaned up with neutral alumina. The separation was performed on a TR-5MS capillary column (30 m×0.25 mm×0.25 μ m) by programmed temperature vaporization (PTV) with splitless mode. Meanwhile the identification and quantification were performed by GC-MS/MS in selected reaction monitoring (SRM) mode and using the internal standard method. The calibration curves of the 27 phthalate esters showed good linearities in the range of 0.05-10 mg/L, except diisononyl ortho-phthalate (DINP) which was in the range of 0.1-20 mg/L, with the correlation coefficients not less 0.9962. The limits of detection (LODs) were 0.1-9.8 μ g/kg and the limits of quantification (LOQs) were 0.4-32.6 μ g/kg. With the proposed method, the spiked recoveries were evaluated in four types of baked foods (bread, biscuits, cakes, stuffing) at low, medium and high concentrations. The results showed that the average recoveries of the 28 PAEs were in the range of 81.0%-117%, and the relative standard deviations (RSDs, n=6) were in the range of 1.3%-13.6%. The method was successfully applied in the investigation of the PAEs distribution in baked foods. The method is suitable for the determination of the 28 PAEs in baked foods with easy operation, high accuracy and precision.
- gas chromatography-tandem mass spectrometry (GC-MS/MS),
- phthalate eaters (PAEs),
- plasticizer,
- baked foods
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