超高效液相色谱-三重四极杆/复合线性离子阱质谱法同时测定蔬果中的氯酸盐和高氯酸盐  

Simultaneous determination of chlorate and perchlorate in vegetables and fruits using ultra-performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry

作　　者：方晓丽 李瑞芬[1] 杨舒然 陈炳奔 郑三燕[1] FANG Xiaoli;LI Ruifen;YANG Shuran;CHEN Bingben;ZHENG Sanyan(Wenzhou Center for Disease Control and Prevention,Zhejiang Wenzhou 325000,China)

机构地区：[1]温州市疾病预防控制中心,浙江温州325000

出　　处：《中国食品卫生杂志》2024年第3期278-283,共6页Chinese Journal of Food Hygiene

基　　金：温州市科技局基础性科研项目(Y20220311)。

摘　　要：目的建立超高效液相色谱-三重四极杆/复合线性离子阱质谱(UPLC-Qtrap MS)同时检测蔬果中氯酸盐和高氯酸盐的方法。方法样品中氯酸盐和高氯酸盐用乙腈-水提取,经GCB+PSA净化,以乙腈和20 mmol/L甲酸铵为流动相,在Waters Anionic Polar Pesticide(100 mm×2.1 mm,5μm)色谱柱上分离,经UPLC-Qtrap MS检测,内标法定量。结果氯酸盐和高氯酸盐分别在2.0~200和0.5~100μg/L范围内线性关系良好,相关系数均>0.999,方法检出限分别为0.006、0.001 mg/kg。低、中、高三种加标水平的回收率为83.3%~105.5%,相对标准偏差为0.97%~3.80%。结论此法快速、简单、准确、精密度好,可应用于蔬果中氯酸盐和高氯酸盐的检测。Objective A method was developed to simultaneously determine chlorate and perchlorate in vegetables and fruits using ultra-performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry(UPLC-Qtrap MS).Methods The chlorate and perchlorate residues in samples were extracted using acetonitrile and water,and the supernatant was purified using GCB and PSA.The analytes were separated on a Waters Anionic Polar Pesticide(100 mm×2.1 mm,5μm)column using a mobile phase comprising acetonitrile and 20 mmol/L ammonium formate solution and detected using UPLC-Qtrap MS.The internal standard method was used for quantification.Results The linear relationship of chlorate and perchlorate ranged from 2.0-200 and 0.5-100μg/L,with correlation coefficients>0.999.The limits of detection were 0.006 and 0.001 mg/kg.The recoveries in spiked samples ranged from 83.3%-105.5%,and the relative standard deviations ranged from 0.97%-3.80%.Conclusion A rapid,simple,accurate,and precise method was developed for the simultaneous analysis of chlorate and perchlorate in vegetables and fruits.

关 键 词：超高效液相色谱-三重四极杆/复合线性离子阱质谱 氯酸盐 高氯酸盐 蔬菜 水果 食品污染物 

分 类 号：R155[医药卫生—营养与食品卫生学]