Determination of Perchlorate Content and Exposure Level in Milk by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry
Objective:Perchlorate has been widely present in milk.A method for the determination of perchlorate content in milk by ultra-high performance liquid chromatogre-tandem mass spectrometry was established,and the exposure level of perchlorate was briefly evaluated.Methods:By optimizing the selection conditions of chromatographic column,mobile phase,solid phase extraction column and microporous filter membrane,the retention time,peak shape and response intensity of perchlorate peak were improved.Results:When pure water and acetonitrile were used as mobile phases,the retention time of C18 chromatographic column has a shorter retention time.The T3 chromatographic column provided a sharp peak shape,and pure water is environmentally friendly and suitable for the detection of single components of perchlorate,while the P1 chromatographic column has no retention for perchlorate.When 20 mmol/L ammonium formate and acetonitrile were used as mobile phases,the P1 column had better retention time,sharp peak shape,and a response value to perchlorate that was about twice that of the T3 chromatographic column.Using C18 as solid phase extraction column,the price is relatively low,and the column efficiency after mixing and dispersing the target substance is better(the rate of recovery＞90％).Choosing the cost-effective Agilent ValueLab fltr PTFE-Q microporous filter membrane resulted in a recovery rate of over 92％for the target substance,meeting the experimental requirements.Conclusion:Under P1 complex ion exchange column separation,20 mmol/L ammonium formate and acetonitrile gradient elution and AJS ion source conditions,the perchlorate showed a good linear relationship in the range of 1-200 μg/L,with R2 of 0.9997.The recoveries of perchlorate at low,medium,and high spiked levels ranged from 96.6％to 103.3％,with relative standard deviations(RSD)of 1.16％to 1.74％(n=6).The method was applied to detect perchlorate in 68 different milk samples,and the results showed the overall detection rate of perchlorate was 29.4％(20/68)and the detection value was ND(not detected)-18.6 μg/kg.The hazard quotient of the four age groups is far less than 1,indicating that milk is not the main intake object of perchlorate.
ultra-high performance liquid chromatogre-tandem mass spectrometryperchloratemilk
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