Determination of Ethoxyquinoline and Ethoxyquinoline Dimer in Aquatic Products by High Performance Liquid Chromatography－Tandem Mass Spectrometry

WANG Meng-ru; YIN Yao; NING Xiao-pan; ZHANG Ping; PENG Jun; LOU Yun; DING Tao; WU Li-na; LIU Han; ZHANG Xiao-yan

doi:10.19969/j.fxcsxb.22103101

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Determination of Ethoxyquinoline and Ethoxyquinoline Dimer in Aquatic Products by High Performance Liquid Chromatography－Tandem Mass Spectrometry

Experimental Techniques and Methods | 更新时间：2023-04-17

- Determination of Ethoxyquinoline and Ethoxyquinoline Dimer in Aquatic Products by High Performance Liquid Chromatography－Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 42, Issue 3, Pages: 344-350(2023)
- 作者机构：
  
  1.南京海关动植物与食品检测中心，江苏南京 210019
  2.南京师范大学食品与制药工程学院，江苏南京 210023
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22103101
  CLC：
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王梦茹,殷耀,宁晓盼等.高效液相色谱－串联质谱法测定水产品中的乙氧基喹啉和乙氧基喹啉二聚体[J].分析测试学报,2023,42(03):344-350.

WANG Meng-ru,YIN Yao,NING Xiao-pan,et al.Determination of Ethoxyquinoline and Ethoxyquinoline Dimer in Aquatic Products by High Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(03):344-350.
王梦茹,殷耀,宁晓盼等.高效液相色谱－串联质谱法测定水产品中的乙氧基喹啉和乙氧基喹啉二聚体[J].分析测试学报,2023,42(03):344-350. DOI： 10.19969/j.fxcsxb.22103101.

WANG Meng-ru,YIN Yao,NING Xiao-pan,et al.Determination of Ethoxyquinoline and Ethoxyquinoline Dimer in Aquatic Products by High Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(03):344-350. DOI： 10.19969/j.fxcsxb.22103101.

摘要

建立了检测鱼、虾、泥鳅和螃蟹等水产品中乙氧基喹啉和乙氧基喹啉二聚体残留的高效液相色谱－串联质谱（HPLC－MS/MS）方法。在样品制备时加入适量维生素C，以乙腈作为提取溶剂，正己烷进行液液萃取。上清液经Oasis PRiME HLB固相萃取柱净化后旋蒸至近干，乙腈定容后采用Agela Phenomenex Kinetex C,18,色谱柱（100 mm × 4.6 mm × 2.6 μm）分离，在电喷雾电离源正离子模式下采用选择反应监测（SRM）模式进行检测，外标法定量。乙氧基喹啉和乙氧基喹啉二聚体在1 ~ 100 μg/L质量浓度范围内线性关系良好，相关系数（,r,2,）均大于0.994，检出限（LOD）均为0.5 μg/kg，定量下限（LOQ）均为1.5 μg/kg。两种目标物质在1.5、5、10、100 μg/kg 4个加标浓度下的平均回收率为75.8% ~ 103%，相对标准偏差（RSD）为0.58% ~ 9.6%。该方法灵敏度高，准确度和精密度好，适用于鱼、虾、泥鳅和螃蟹等水产品中乙氧基喹啉及乙氧基喹啉二聚体的检测。

Abstract

An analytical method was developed for the simultaneous determination of ethoxyquinoline and ethoxyquinoline dimer residues in aquatic products such as fishes，shrimps，loaches and crabs by high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）．An appropriate amount of vitamin C was added in the sample preparation．Acetonitrile was used as the extraction solvent，and hexane was used for liquid－liquid extraction．The supernatant was cleaned up on an Oasis PRiME HLB solid-phase extraction column and spun to near dryness，acetonitrile was used to fix the volume．Then the sample was separated on an Agela Phenomenex Kinetex C,18, column（100 mm ×4.6 mm × 2.6 μm），and subsequently detected with electrospray ionization source in positive ionization mode under selected reaction monitoring（SRM） mode，and quantified by external standard method. There were good linear relationships for both ethoxyquinoline and ethoxyquinoline dimer in concentration range of 1－100 μg/L，with their correlation coefficients（,r,2,） greater than 0.994. The limits of detection（LODs） and limits of quantitation（LOQs） of the method were 0.5 μg/kg and 1.5 μg/kg，respectively. The average recoveries for two target substances at four spiked levels of 1.5，5，10 and 100 μg/kg ranged from 75.8% to 103%，with relative standard deviations（RSDs） of 0.58%－9.6%. The developed method is sensitive，accurate and precise，and it could be applied to the determination of ethoxyquinoline and ethoxyquinoline dimer in aquatic products such as fishes，shrimps，loaches and crabs.

关键词

高效液相色谱－串联质谱水产品乙氧基喹啉乙氧基喹啉二聚体固相萃取

Keywords

high performance liquid chromatography－tandem mass spectrometryaquatic productsethoxyquinolineethoxyquinoline dimersolid-phase extraction

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