Determination of Nine Kinds of Sulfonamides Residues in Gizzard Pepsin by Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry

XU Xiao-hui; WANG Xiao-qiao; DONG Wei; WU Fu-xiang; DU Rui-hu; ZHU Ren-yuan; SHI Xiao-feng

doi:10.19969/j.fxcsxb.21020302

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Determination of Nine Kinds of Sulfonamides Residues in Gizzard Pepsin by Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry

Experimental Techniques and Methods | 更新时间：2023-02-13

- Determination of Nine Kinds of Sulfonamides Residues in Gizzard Pepsin by Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 40, Issue 10, Pages: 1497-1502(2021)
- 作者机构：
  
  1.兰州市食品药品检验检测研究院，甘肃兰州 730050
  2.甘肃省医学科学研究院，甘肃兰州 730050
  3.兰州中检科测试技术有限公司，甘肃兰州 730070
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.21020302
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许晓辉,王小乔,董蔚等.超高效液相色谱－串联质谱法测定鸡内金中9种磺胺类药物残留[J].分析测试学报,2021,40(10):1497-1502.

XU Xiao-hui,WANG Xiao-qiao,DONG Wei,et al.Determination of Nine Kinds of Sulfonamides Residues in Gizzard Pepsin by Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2021,40(10):1497-1502.
许晓辉,王小乔,董蔚等.超高效液相色谱－串联质谱法测定鸡内金中9种磺胺类药物残留[J].分析测试学报,2021,40(10):1497-1502. DOI： 10.19969/j.fxcsxb.21020302.

XU Xiao-hui,WANG Xiao-qiao,DONG Wei,et al.Determination of Nine Kinds of Sulfonamides Residues in Gizzard Pepsin by Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2021,40(10):1497-1502. DOI： 10.19969/j.fxcsxb.21020302.

摘要

采用超高效液相色谱－串联三重四极杆质谱（UPLC－MS/MS）技术，建立了动物源性中药鸡内金中磺胺甲𫫇,唑等9种磺胺类药物残留的检测方法。样品经QuEChERS法提取，离心后上清液经PRiME HLB固相萃取柱净化，采用ACQUITY BEH C,18,柱（2.1 mm × 100 mm，1.7 μm）分离，以含0.1%甲酸－2 mmol/L乙酸铵的水溶液和含0.1%甲酸的乙腈溶液为流动相进行梯度洗脱，在电喷雾正离子模式下，以动态多反应监测模式（d－MRM）进行检测，外标法定量。结果表明9种磺胺类药物在0～50 ng/mL范围内呈良好的线性关系，相关系数（,r,2,）均不小于0.996 0，方法检出限（LOD，,S/N = ,3）和定量下限（LOQ，,S/N = ,10）分别为0.065 4～0.715 7 µg/kg和0.212 2～2.478 µg/kg；在3个加标水平下的回收率为63.2%～88.7%，相对标准偏差（RSD）为0.90%～7.1%。该方法简单、快速、准确，应用该方法筛查10批鸡内金样品，有1批检出磺胺甲𫫇,唑残留。

Abstract

In order to evaluate the risk of sulfonamides residues in Gizzard Pepsin， a comprehensive analytical method was developed for the qualitative and quantitative determination of nine kinds of sulfonamides in Gizzard Pepsin by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry（UPLC－MS/MS） in this paper.The sample was extracted by QuEChERS with ultrasonic method，then purified with PRiME HLB．The chromatographic separation was performed on an ACQUITY BEH C,18, chromatographic column（2.1 mm × 100 mm，1.7 μm），with 0.1% formic acid－2 mmol/L ammonium acetate aqueous solution and acetonitrile containing 0.1% formic acid as mobile phases by gradient elution.The analytes were detected by electrospray ionization mass spectrometry in positive mode under dynamic multiple reaction monitoring（d－MRM） mode，and quantified by external standard method．Results showed that the nine sulfonamides showed good linearities in the concentration range of 0－50 ng/mL with their correlation coefficients（,r,2,） not less than 0.996 0．The limits of detection（LOD，,S/N = ,3） and limits of quantitation（LOQ，,S/N = ,10） were in the ranges of 0.065 4－0.715 7 µg/kg and 0.212 2－2.478 µg/kg，respectively.The recoveries for the analytes at three spiked levels were in the range of 63.2%－88.7%，with relative standard deviations（RSD） of 0.90%－7.1%．The developed method was simple，rapid and accurate，and was applied to the detection on 10 batches of Gizzard Pepsin samples，among which one was found to contain sulfamethoxazole residue．

关键词

鸡内金磺胺类药物超高效液相色谱－串联质谱QuEChERSPRiME HLB

Keywords

Gizzard Pepsinsulfonamidesultra-performance liquid chromatography－tandem mass spectrometryQuEChERSPRiME HLB

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