Determination of chlorate and perchlorate in vegetables by ultra performance liquid chromatography-tandem mass spectrometry
Objective To develop a method for the determination of chlorate and perchlorate in vegetables by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS-MS).Methods The sample was extracted by ultrapure water+acetonitrile(1+2,v/v)vortex ultrasonic extraction.After high-speed centrifugation,the supernatant was purified by MCX solid phase extraction column,filterated by 0.22 μm hydrophilic polytetrafluoroethylene membrane,determined by UPLC-MS-MS and quantified by internal standard method.The chromatographic column was Waters TorusTM DEA Column 130A 1.7 μm 2.1 mm×100 mm,the mobile phase was 10 mmol/L ammonium acetate solution-acetonitrile,and the gradient elution was carried out for 6 min.The mass spectrometry analysis adopted the electrospray ion source(negative ion scanning)mode and the multi reaction monitoring(MRM)mode.Results The linear range of chlorate was 1.0-100.0 ng/mL,the linear range of perchlorate was 0.5-50.0 ng/mL,and the correlation coefficients(r)were＞0.999.The limit of detection and limit of quantitation for chlorate was 1.0 μg/kg and 3.0 µg/kg respectively.The limit of detection and limit of quantitation for perchlorate was 0.1 μg/kg and 0.3 μg/kg respectively.Under the three concentrations of high,medium and low,the recoveries ranged from 95.6％to 102.0％,and the relative standard deviations(RSD)ranged from 2.1％to 5.8％.Conclusions The study adopts 10 mmol/L ammonium acetate solution-acetonitrile as the mobile phase and gradient elution mode,all target substances are separated within 6 minutes,with high response and good linearity.The method is simple,accurate and suitable for the determination of chlorate and perchlorate in vegetables.
ChloratePerchlorateVegetablesUltra performance liquid chromatography-tandem mass spectrometry
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