Determination of Chlorate and Perchlorate Amounts in Meat by High Performance Liquid Chromatography-Tandem Mass Spectrometry

Abstract

A method for simultaneous determination of chlorate and perchlorate amounts in meat by high performance liquid chromatography-tandem mass spectrometry was developed. Samples were extracted with acetonitrile/water (13:7, V:V ) and centrifuged. The obtained supernatants were purified on a PRiME HLB solid phase extraction column, followed by an Acclaim Trinity P1 ion exchange column with the gradient elution of acetonitrile and 20 mmol/L ammonium acetate as the mobile phase to afford chlorate and perchlorate. MS/MS was performed in ESI+ and multiple reaction monitoring mode with an internal standard for quantification. The results showed chlorate and perchlorate had calibration curves with good linearity in the ranges of 2~200.0 ng/mL and 1~100.0 ng/mL respectively, with corresponding correlation coefficients being 0.9983 and 0.9998. The detection limits of the method were 2.0 and 1.0 μg/kg, respectively. The recovery rates of chlorate and perchlorate were 91.0%~105.7% and 94.2%~110.5% respectively, at the addition levels of 6.0, 20, 40, 200 μg/kg, and 3.0, 10, 20, 100 μg/kg. The relative standard deviations for chlorate and perchlorate were 1.8%~9.7% and 0.7%~9.4% respectively. This method would be easy to use and has high detection sensitivity and good stability, and could well meet the requirements of determining chlorate and perchlorate amounts in meat.

Keywords

• chlorate
• perchlorate
• high performance liquid chromatography-tandem mass spectrometry
• meat