Simultaneous determination of 3-chloro-1,2-propanediol (3-MCPD) esters residues in foods by solid phase extraction-ultra performance liquid chromatography-electrospray tandem mass spectrometry
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(Shenzhen Center for Disease Control and Prevention,Guangdong Shenzhen 518055,China)

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    Abstract:

    To establish a sensitive quantitative method for the simultaneous determination of 3-chloro-1,2-propanediol (3-MCPD) esters in foods by ultra performance liquid chromatography coupled with electrospray tandem mass spectrometry (UPLC-MS/MS) with the pretreatment of solid phase extraction, and investigate ten types of 3-MCPD esters residues in some greasy foods from supermarket.Methods About 0.100 0 g oil sample was accurately weighted and dissolved in a mixture of 10 ml tert-butyl methyl ether (MTBE)-ethyl acetate (8∶2, V/V) and spiked with internal standard. After vortex, the analyte of the extraction were purified by a Sep-pak silica cartridge and a OASIS HLB C18 cartridge (preconditioned with methanol) in turn. The sample extract was separated on an acquity BEH C18 column (2.1 mm×150 mm,1.7 μm), identified by electrospray ionization (ESI) in positive mode using multiple reaction monitoring (MRM), and then detected by ultra performance liquid chromatography-tandem mass spectrometry and quantified with internal standards. Results By the quantification of internal standard, the 18 types of 3-MCPD esters were linear in the range of 1.0~200.0 μg/L with correlation coefficient of 0.999 1~ 0.999 8. The detection limit of the method was ranged from 1.17 to 30.1 μg/kg for edible oils. The recovery of spiked samples at three levels (0.10,1.0 and 10.0 mg/kg) was ranged from 80.2%~98.5% (n=7). And the relative standard derivations (RSD) were lower than 8.1%. In 50 edible oils and 12 greasy foods, 3-MCPD esters were detected at the range of 7.55~5 360 μg/kg with a detection rate of 92.0% (46/50), and in 12 greasy foods, 3-MCPD esters was detected at the range of 6.62~ 1 569.8 μg/kg with a detection rate of 75.0% (9/12).Conclusion The method could be used to detect 3-MCPD esters in edible oils and greasy foods.

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LIU Hong-he, CHEN Hui-ling, XU Xin-xin, KANG Li, LIAO Shi-cheng, MAO Li-sha. Simultaneous determination of 3-chloro-1,2-propanediol (3-MCPD) esters residues in foods by solid phase extraction-ultra performance liquid chromatography-electrospray tandem mass spectrometry[J].中国食品卫生杂志,2016,28(3):327-333.

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  • Received:October 10,2015
  • Revised:
  • Adopted:
  • Online: June 02,2016
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