Determination of 15 Organophosphate Esters in Meat Products by Dispersive Solid Phase Extraction-gas Chromatography-triple Quadrupole Tandem Mass Spectrometry
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Abstract:
In this study, an analytical method for the determination of 15 organophosphate esters (OPEs) in meat products was established based on dispersive solid phase extraction-gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS). The organophosphates in the sample was extracted with acetonitrile, purified with enhanced matrix removal adsorbent (enhanced matrix removal-lipid, EMR-Lipid), separated by HP-5MS column, determined by GC-MS/MS dynamic multi-reaction ion monitoring (dMRM) mode, and quantified by the matrix matching external standard method. The results showed that chromatographic separation and analysis of 15 OPEs were completed within 21 min, and good linear relationship of the target substances was obtained in the range of 0.01~100 ng/mL, with the correlation coefficients greater than 0.999. The average spike recoveries of 15 kinds of organic phosphate esters at different spiking levels (1.25, 12.5 and 25 ng/g) were 72.8%~123.8%, with the relative standard deviations (RSDs) (n=6) being1.6%~14.7%, the detection limit (LOD) of the method being 0.25~0.40 ng/g and the limit of quantification (LOQ) being 0.80~1.25 ng/g. The method was applied to 70 commercial meat products samples. The results showed that 7 organophosphate esters were detected in 58 samples with a detection rate of 82.8%. Among which, the three organophosphate esters with higher detection rates were tri (2-chloro-1-(chloromethyl) ethyl) phosphate, tri (2-chloro-ethyl) phosphate and triphenyl phosphate. The method established in this study has the advantages of simple operation, high speed and good purification effect, and can be used for the rapid detection of 15 organophosphate esters in meat products.
