Determination of Niclosamide-olamine Residue in 22 Kinds of Agricultural Products by UPLC-MS/MS

JIANG Shu-fan; HE Yan; LI Bei; ZHANG Xin-zhong; HAN Bing-jun

doi:10.12452/j.fxcsxb.23081303

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Determination of Niclosamide-olamine Residue in 22 Kinds of Agricultural Products by UPLC-MS/MS

Scientific Papers | 更新时间：2024-02-21

- Determination of Niclosamide-olamine Residue in 22 Kinds of Agricultural Products by UPLC-MS/MS
- Journal of Instrumental Analysis Vol. 43, Issue 2, Pages: 278-284(2024)
- 作者机构：
  
  1.天津农学院园艺园林学院，天津 300392
  2.中国热带农业科学院分析测试中心农业农村部亚热带果品蔬菜质量安全控制重点实验室海南省热带果蔬产品质量安全重点实验室，海南海口 571101
  3.中国农业科学院茶叶研究所，浙江杭州 310008
  4.海南省食品检验检测中心国家市场监管重点实验室（热带果蔬质量与安全），海南海口 570311
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.23081303
  CLC： O657.7;TS207.3
- Published：15 February 2024，
  
  Received：13 August 2023，
  
  Revised：21 November 2023，
- 稿件说明：
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蒋舒帆,何燕,李备等.UPLC-MS/MS法测定22种农产品中杀螺胺乙醇胺盐残留[J].分析测试学报,2024,43(02):278-284.

JIANG Shu-fan,HE Yan,LI Bei,et al.Determination of Niclosamide-olamine Residue in 22 Kinds of Agricultural Products by UPLC-MS/MS[J].Journal of Instrumental Analysis,2024,43(02):278-284.
蒋舒帆,何燕,李备等.UPLC-MS/MS法测定22种农产品中杀螺胺乙醇胺盐残留[J].分析测试学报,2024,43(02):278-284. DOI： 10.12452/j.fxcsxb.23081303.

JIANG Shu-fan,HE Yan,LI Bei,et al.Determination of Niclosamide-olamine Residue in 22 Kinds of Agricultural Products by UPLC-MS/MS[J].Journal of Instrumental Analysis,2024,43(02):278-284. DOI： 10.12452/j.fxcsxb.23081303.

摘要

建立了超高效液相色谱-串联质谱（UPLC-MS/MS）测定22种农产品中杀螺胺乙醇胺盐残留的分析方法。样品采用改进的QuEChERS方法进行前处理，使用1%甲酸乙腈提取，利用弗罗里硅土进行净化，采用C

色谱柱进行分离，电喷雾离子源负电离方式和多反应监测模式检测，基质外标法定量。结果表明，22种农产品基质中杀螺胺乙醇胺盐在0.005~0.10 μg/mL范围内均呈现良好的线性关系；在茶叶中的检出限为0.003 mg/kg，定量下限为0.01 mg/kg，在其它基质中的检出限为0.002 mg/kg，定量下限均为0.005 mg/kg。在低、中、高3个加标水平下，平均回收率为77.3%~115%，相对标准偏差（RSD）小于10%，符合残留分析方法要求。该方法简单快速，试剂消耗较小，可满足农产品中杀螺胺乙醇胺盐的检测需求。

Abstract

An ultra-high performance liquid chromatography-tandem mass spectrometry method（UPLC-MS/MS） was established to determine niclosamide-olamine residue in 22 kinds of agricultural products. With acetonitrile containing 1% formic acid as the extraction solvent and florisil as purificant，a modified QuEChERS method was chosen to purify the analytes from the different samples. The target niclosamide-olamine was separated by a C

UPLC column，then detected by negative electro-spray ionization（ESI-） and multiple reaction monitoring（MRM） mode. Quantification was performed by peak area external standard methods using matrix-matched calibration curves，with good linear relationships in the range of 0.005-0.10 μg/mL. The limit of detection（LOD） and limit of quantitation（LOQ） of niclosamide-olamine were 0.003 mg/kg and 0.01 mg/kg in tea sample，and 0.002 mg/kg and 0.005 mg/kg in other samples. At three spiked levels in different food samples，the average recoveries were between 77.3% and 115% with relative standard deviations（RSDs） lower than 10%. The method is simple and rapid with low usage of reagents. It is suitable for the determination of niclosamide-olamine in a variety of matrices for agricultural products.

关键词

UPLC-MS/MSQuEChERS杀螺胺乙醇胺盐残留农产品

Keywords

UPLC-MS/MSQuEChERSniclosamide-olamineresidueagricultural products

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