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
作者:
作者单位:

温州市疾病预防控制中心,浙江 温州 325000

作者简介:

方晓丽 女 主管技师 研究方向为食品安全检测 E-mail:326514344@qq.com

通讯作者:

中图分类号:

R155

基金项目:

温州市科技局基础性科研项目(Y20220311)


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

Wenzhou Center for Disease Control and Prevention, Zhejiang Wenzhou 325000, China

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    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,5 μm)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0.5~100 μg/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。

    Abstract:

    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, 5 μm) 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 0.5-100 μg/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.

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方晓丽,李瑞芬,杨舒然,陈炳奔,郑三燕.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[J].中国食品卫生杂志,2024,36(3):278-283.

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  • 收稿日期:2023-03-08
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  • 在线发布日期: 2024-06-17
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