Determination of chlorate and perchlorate in liquid milk by ultra performance liquid chromatography-triple quadrupole mass spectrometry
Objective To establish an ultra performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-TQMS)method for rapid determination of chlorate and perchlorate in liquid milk.Methods The samples were ex-tracted with acetonitrile,purified by PRiME HLB solid-phase extraction column and separated with a Waters Torus DEA column(2.1 mm×100 mm,1.7 μm).Acetonitrile and 20 mmol/L ammonium acetate solution were used as mobile phases for gradient elution.The analytes were detected by UPLC-TQMS and quantified by the internal standard method.Results The calibration curves showed a good linear relationship in the range of 2-200 ng/ml for chlorate and 1-100 ng/ml for per-chlorate with the correlation coefficient greater than 0.99.The limit of detection was 1.0 μg/kg for chlorate and 0.5 μg/kg for perchlorate.The average recoveries of chlorate and perchlorate were 91.0％ -95.6％ and 92.5％ -95.4％ ,respectively.The relative standard deviations of chlorate and perchlorate were 4.55％ -5.70％ (n=6)and 4.34％ -5.81％ (n=6),re-spectively.Conclusion The method is simple and sensitive with high reproducibility,which is suitable for the determination of chlorate and perchlorate in liquid milk.Furthermore,it provides an accurate and effective data support for the establishment of the national food safety standards.
Liquid milkChloratePerchlorateSolid-phase extractionUltra performance liquid chromatography-triple quadrupole mass spectrometry
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