Determination of Dapsone and Its Metabolites in Aquatic Products by Solid Phase Extraction with High Performance Liquid Chromatography－Tandem Mass Spectrometry

WU Zi; HUANG Dong-mei; LOU Xiao-yi; ZHENG Rong; TANG Yun-yu; ZHANG Xuan; ZHANG Jun

doi:10.19969/j.fxcsxb.21110501

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Determination of Dapsone and Its Metabolites in Aquatic Products by Solid Phase Extraction with High Performance Liquid Chromatography－Tandem Mass Spectrometry

Experimental Techniques and Methods | 更新时间：2022-06-22

- Determination of Dapsone and Its Metabolites in Aquatic Products by Solid Phase Extraction with High Performance Liquid Chromatography－Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 41, Issue 6, Pages: 882-888(2022)
- 作者机构：
  
  1.中国水产科学研究院东海水产研究所农业农村部水产品质量监督检验测试中心（上海）农业农村部水产品质量安全控制重点实验室（上海），上海 200090
  2.上海海洋大学食品学院，上海 201306
  3.钛和检测认证集团股份有限公司，上海 200060
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.21110501
  CLC：
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伍姿,黄冬梅,娄晓祎等.固相萃取/高效液相色谱－串联质谱法测定水产品中氨苯砜及其代谢物残留量[J].分析测试学报,2022,41(06):882-888.

WU Zi,HUANG Dong-mei,LOU Xiao-yi,et al.Determination of Dapsone and Its Metabolites in Aquatic Products by Solid Phase Extraction with High Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(06):882-888.
伍姿,黄冬梅,娄晓祎等.固相萃取/高效液相色谱－串联质谱法测定水产品中氨苯砜及其代谢物残留量[J].分析测试学报,2022,41(06):882-888. DOI： 10.19969/j.fxcsxb.21110501.

WU Zi,HUANG Dong-mei,LOU Xiao-yi,et al.Determination of Dapsone and Its Metabolites in Aquatic Products by Solid Phase Extraction with High Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(06):882-888. DOI： 10.19969/j.fxcsxb.21110501.

摘要

建立了高效液相色谱－串联三重四极杆质谱（HPLC－MS/MS）测定水产品中氨苯砜及其代谢物残留量的方法。样品加入D,8,－氨苯砜内标，经1%氨化乙腈提取，正己烷去脂后，采用MCX阳离子固相萃取柱进行富集和净化，氮吹浓缩至0.2 mL左右。用甲醇和水作为流动相，以CAPCELL PAK C,18,色谱柱（2.0 mm × 100 mm，3 µm）进行分离，在质谱多反应监测（MRM）、正离子电离模式下测定，采用内标法定量。氨苯砜和N-乙酰氨苯砜在0.1 ~ 5.0 μg/kg范围内线性关系良好，相关系数（,r,2,）均大于0.99，方法检出限（LOD）为0.1 μg/kg，定量下限（LOQ）为0.2 μg/kg。以不同类型的水产品为空白基质，在0.2、1.0、2.0 μg/kg加标水平下，平均加标回收率为94.0% ~ 109%，相对标准偏差（RSD）为2.7% ~ 11%。用该法对药代实验中获得的阳性肌肉样品进行测定，通过对化合物的保留时间和离子对信息进行鉴别，鉴定出氨苯砜的代谢产物为N-乙酰氨苯砜。该方法的检出限低、精密度好、准确度高，能够实现对不同水产品中氨苯砜残留量的准确定性与定量检测。

Abstract

It is of great significance to develop novel analysis techniques for simultaneous determination of dapsone and its metabolites in aquatic products，so as to realize the simultaneous supervision of dapsone and its metabolites in aquatic products and the comprehensive control of illegal drug use．In this study，a high performance liquid chromatography－tandem triple quadrupole mass spectrometric（HPLC－MS/MS） method was established for the determination of dapsone and its metabolite residues in aquatic products．In the process of sample pre-treatment，the samples were extracted by using 10 mL 1% ammoniated acetonitrile with dapsone-D,8, as the internal standard，followed by fat removal with ,n,-hexane．Meanwhile，MCX cationic solid phase extraction column was used for enrichment and purification．The eluent was concentrated to about 0.2 mL by nitrogen blowing at 45 ℃，and then fixed with 10% methanol solution to 1 mL．After mixing，the eluent was filtered through a 0.22 μm aqueous phase membrane into an injection vial for detection by HPLC－MS/MS．The separation was carried out on a CAPCELL PAK C,18,（2.0 mm × 100 mm，3 µm） by gradient elution using methanol－water as mobile phases．The quantitative analysis of target compounds was performed by the internal standard method under multiple reaction monitoring（MRM） and positive ion ionization modes．The results showed that the calibration curves for dapsone and N-acetyl dapsone were linear in the mass concentration range of 0.1－5.0 μg/kg，with correlation coefficients（,r,2,） all greater than 0.99．The limits of detection（LODs） were 0.1 μg/kg and the limits of quantitation（LOQs） were 0.2 μg/kg．The average recoveries at three spiked levels of 0.2，1.0，2.0 μg/kg ranged from 94.0% to 109%，with relative standard deviations（RSDs） of 2.7%－11%．The positive muscle samples obtained in the drug substitution experiment were determined，and the metabolite of dapsone was identified as N-acetyl dapsone by identifying the retention time of the compound and the ion pair information．This method has low detection limit，good precision and high accuracy，which could realize the accurate qualitative and quantitative determination of dapsone residues in fish，shrimp，crab，shellfish and other aquatic products．

关键词

高效液相色谱－串联质谱（HPLC－MS/MS）氨苯砜N-乙酰氨苯砜MCX固相萃取水产品

Keywords

high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）dapsoneN-acetyl dapsoneMCX solid phase extractionaquatic products

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