关键词: 氯酸盐, 高氯酸盐, 蔬菜, 超高效液相色谱-串联质谱

Abstract: 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 Torus^TM 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.

Key words: Chlorate, Perchlorate, Vegetables, Ultra performance liquid chromatography-tandem mass spectrometry