OCCUPATION AND HEALTH ›› 2024, Vol. 40 ›› Issue (9): 1190-1194.

• Experiment·Monitoring and Inspection • Previous Articles     Next Articles

Determination of chlorate and perchlorate in vegetables by ultra performance liquid chromatography-tandem mass spectrometry

HUANG Shunli, FAN Qing, HONG Yi   

  1. Department of Physics and Chemistry, Center for Disease Control and Prevention of Yubei District, Chongqing, 401120, China
  • Received:2023-08-22 Revised:2023-09-19 Published:2026-03-13
  • Contact: FAN Qing,Laboratorian in charge,E-mail:617906359@qq.com

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 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.

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

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