Determination Perfluorinated Compounds In Egg By HPLC-MS/MS Combine Dispersive Solid Phase Extration

Perfluorinated compounds(PFCs) is a new kind of persistent organic pollutants. Animal derived food is the main way to the human intake of PFCs.Egg is one of the typical representative of animal derived food, so it is very urgent to establish the method for determination of PFCs in egg. The results are as follows:(1) A method was developed for the determination of 17 perfluorinated compounds in egg by high performance liquid chromatography-electrospray ionization-tandem mass spectrometry(HPLC-ESI-MS/MS). The mass spectrometry and chromatographic conditions were optimized, using the Agilent poroshell 120 EC-C18 column; the mobile phase was 5 mmol/L ammonium acetate in methanol and 5mmol/L ammonium acetate water. The limits of detection of PFCs were between 0.0010 and 0.093 μg/kg, and the limits of quantitation were between 0.0030 and 0.31μg/kg.The preparation method was optimized. Compared three kinds of preparation methods, After comparing three kinds of preparation methods, it was selected for the dispersive solid phase extraction method using ultrasonic of acetonitrile, which is due to its good recovery, convenient, affordable. Then the ultrasonic temperature, time and graphitized carbon black content were optimized so that the recovery of the long carbon chain carboxylic acids in PFCs was significant increased. The analysis method was evaluated. The mean recoveries of 17 PFCs at the spiked levels of 0.5, 1.0 and 2.0 μg/kg were in range of 79%- 125% with relative standard deviations(RSDs, n=6) of 0.26%- 14%. The precision and accuracy of the method is well. The method was suitable for the identification and quantification of 17 perfluorinated compounds in egg due to its advantages of simplicity, accuracy and high sensitivity.(2)A method was developed for the determination precursor of 7 perfluorinated compounds in egg by high performance liquid chromatography-electrospray ionization-tandem mass spectrometry(HPLC-ESI-MS/MS). The limits of detection precursor of PFCs were between 0.00074 and 0.13 μg/kg, and the limits of quantitation were between 0.0024 and 0.44 μg/kg. The mean recoveries of 7 PFCs precursor at the spiked levels of 0.5, 2.0 and 5.0 μg/kg were in range of 82%- 116% with relative standard deviations(RSDs, n=6) of 0.39%- 9.3%. The precision and accuracy of the method is well.It was selected for the solid phase extraction method using ultrasonic dispersive of acetonitrile. Then the ultrasonic temperature, p H parameter were optimized.(4) The method was applied to determine the 17 PFCs of egg in many provinces of China. The results show that the total concentration range of 17 PFCs for the sampled provinces in China is between 0.0741μg/kg and 1.39 μg/kg. The highest concentration of PFCs in egg appeared in Anhui province(1.39 μg/kg); the lowest concentration of PFCs in egg appeared in Heilongjiang(0.0741 μg/kg). The results indicated that PFPe A(0.102 μg/kg), PFOA(0.0821 μg/kg) and PFOS(0.0793 μg/kg) were the main residue species in eggs. The health risk assessment to PFOS and PFOA showed that consuming eggs would not cause immediate dangers.