食品与发酵工业 >

2022 , Vol. 48 >Issue 18: 244 - 248

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.029579

分析与检测

液相色谱-串联质谱法快速测定苋菜和菠菜中赤霉素残留

  • 叶倩 ,
  • 唐雪妹 ,
  • 高毓文 ,
  • 黄健祥
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  • 1(广东省农业科学院农业质量标准与监测技术研究所, 广东 广州,510640)
    2(农业农村部农产品质量安全风险评估实验室(广州), 广东 广州,510640)
    3(广东农科监测科技有限公司,广东 广州,510640)
第一作者:硕士,高级实验师(黄健祥副研究员为通信作者,E-mail: hjxjason@163.com)

收稿日期: 2021-10-09

  修回日期: 2021-11-24

  网络出版日期: 2022-10-17

基金资助

国家重点研发计划(2019YFC1605600);广东省基础与应用基础研究基金项目(2020A1515010620);广东省农业科学院科技创新战略专项资金(高水平农科院建设)

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Fast determination of gibberellin(GA3)residues in edible amaranth and spinach by liquid chromatography-tandem mass spectrometry

  • YE Qian ,
  • TANG Xuemei ,
  • GAO Yuwen ,
  • HUANG Jianxiang
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  • 1(Institute of Quality Standard and Monitoring Technology for Agro-products of Guangdong Academy of Agricultural Sciences, Guangzhou 510640, China)
    2(Laboratory of Quality and Safety Risk Assessment of Agro-product (Guangzhou), Ministry of Agriculture and Rural, Guangzhou 510640, China)
    3(Guangdong Agricultural Monitoring Technology Co.Ltd.,Guangzhou 510640, China)

Received date: 2021-10-09

  Revised date: 2021-11-24

  Online published: 2022-10-17

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摘要

该文建立了苋菜和菠菜中赤霉素残留的分析方法。样品以QuEChERS法进行前处理,用含1%(体积分数)乙酸的甲醇溶液提取,液相色谱-串联质谱法测定。对提取溶剂、提取时间、吸附剂、盐的种类和稀释倍数等条件进行了优化。赤霉素在0.001~1.0 mg/L质量浓度范围内均有良好的线性关系。赤霉素的检出限为0.001 mg/kg;在0.010、0.10和0.50 mg/kg 3个添加量下,苋菜和菠菜中赤霉素回收率为82%~91%,相对标准偏差为2%~6%;方法定量限为最低添加量0.010 mg/kg。应用该方法对市售131个苋菜样品、331个菠菜样品进行赤霉素的风险监测,结果显示,赤霉素检出最大值为0.16 mg/kg,以日本肯定列表中赤霉素在蔬菜中残留限量判定,无超标样品。该方法快速、简便、准确,满足苋菜和菠菜等叶菜中赤霉素残留分析的要求。

关键词： 赤霉素; QuEChERS; 液相色谱-串联质谱法; 苋菜; 菠菜; 残留

本文引用格式

叶倩 , 唐雪妹 , 高毓文 , 黄健祥 . 液相色谱-串联质谱法快速测定苋菜和菠菜中赤霉素残留[J]. 食品与发酵工业, 2022 , 48(18) : 244 -248 . DOI: 10.13995/j.cnki.11-1802/ts.029579

Abstract

An analytical method was developed for determination of gibberellin (GA3) residues in edible amaranth and spinach. Sample preparation method was based on QuEChERS. GA3 was extracted by methanol containing 1% (volume ratio) acetic acid and detected with liquid chromatography-tandem mass spectrometry (LC-MS/MS). The optimization of extraction solvent, extraction time, adsorbent, type of salt and dilution factor was studied. The results showed that the linear ranges of GA3 were between 0.001and 1.0 mg/L. The limit of detection was 0.001 mg/kg. Furthermore, under the addition of 0.010, 0.10 and 0.50 mg/kg, the recovery of GA3 in edible amaranth and spinach reached 82%-91%, and the relative standard deviation was 2%-6%. The limit of quantification was 0.010 mg/kg which was the lowest spiked concentration. Then, the risk of GA3 in 131 amaranth and 331 spinach samples were monitored by this method. The results showed that the maximum residue of GA3 was 0.16 mg/kg. According to the maximum residue limit of GA3 in edible amaranth in vegetables in Japan positive list, no samples exceeded the standard. The method is fast, easy and accurate, which can meet the requirements for the determination of GA3 residues in edible amaranth and spinach.

Key words： gibberellin; QuEChERS; liquid chromatography-tandem mass spectrometry; edible amaranth; spinach; residue

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