Accurate Determination, Matrix Effect Estimation, and Uncertainty Evaluation of Three Sulfonamides in Milk by Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry

Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is the most commonly used method for sulfonamide determination. Its accuracy, however, can be affected by many factors. In this study, sulfadiazine (SDZ), sulfadimidine (SMZ), and sulfadimethoxine (SDM) in milk were selected to investigate an...

Full description

Saved in:
Bibliographic Details
Main Authors: Chaonan Han, Xiuqin Li, Hui Jiao, Yan Gao, Qinghe Zhang
Format: Article
Language:English
Published: Wiley 2021-01-01
Series:Journal of Food Quality
Online Access:http://dx.doi.org/10.1155/2021/3910253
Tags: Add Tag
No Tags, Be the first to tag this record!
_version_ 1850176935498350592
author Chaonan Han
Xiuqin Li
Hui Jiao
Yan Gao
Qinghe Zhang
author_facet Chaonan Han
Xiuqin Li
Hui Jiao
Yan Gao
Qinghe Zhang
author_sort Chaonan Han
collection DOAJ
description Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is the most commonly used method for sulfonamide determination. Its accuracy, however, can be affected by many factors. In this study, sulfadiazine (SDZ), sulfadimidine (SMZ), and sulfadimethoxine (SDM) in milk were selected to investigate an accurate determination method and the potential influencing factors in the use of ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Milk samples were extracted by 25 mL perchloric acid solution (pH = 2) and cleaned up using HLB solid-phase extraction (SPE) cartridges. Four kinds of filters, including PTFE, GHP, nylon, and glass fiber, were compared, and PTFE was selected since it had the best recoveries of target sulfonamides (SAs). Three quantitative methods, including external standard (ES), matrix matching (MM), and isotope dilution mass spectrometry (IDMS), were compared, among which IDMS exhibited the best accuracy. The matrix effect under different mobile phase compositions and of different sample matrices were evaluated and discussed. Ion suppression effects were observed during the determination of all SAs, which got stronger with the increase of the methanol composition percent in the mobile phase. After correction by IDMS, the matrix effect could be neglected. Matrix spiked recoveries at three spiked levels (1 μg/kg, 10 μg/kg, and 20 μg/kg) ranged from 96.8% to 103.8% by IDMS. The expanded relative uncertainties were in the range of 2.02% to 5.75%. The method exhibited wide application range, high accuracy, good stability, and high sensitivity.
format Article
id doaj-art-b8901a302ed3441cb15ac0a9b2948f0d
institution OA Journals
issn 0146-9428
1745-4557
language English
publishDate 2021-01-01
publisher Wiley
record_format Article
series Journal of Food Quality
spelling doaj-art-b8901a302ed3441cb15ac0a9b2948f0d2025-08-20T02:19:07ZengWileyJournal of Food Quality0146-94281745-45572021-01-01202110.1155/2021/39102533910253Accurate Determination, Matrix Effect Estimation, and Uncertainty Evaluation of Three Sulfonamides in Milk by Isotope Dilution Liquid Chromatography-Tandem Mass SpectrometryChaonan Han0Xiuqin Li1Hui Jiao2Yan Gao3Qinghe Zhang4Division of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, ChinaDivision of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, ChinaDivision of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, ChinaDivision of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, ChinaDivision of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, ChinaLiquid chromatography-tandem mass spectrometry (LC-MS/MS) is the most commonly used method for sulfonamide determination. Its accuracy, however, can be affected by many factors. In this study, sulfadiazine (SDZ), sulfadimidine (SMZ), and sulfadimethoxine (SDM) in milk were selected to investigate an accurate determination method and the potential influencing factors in the use of ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Milk samples were extracted by 25 mL perchloric acid solution (pH = 2) and cleaned up using HLB solid-phase extraction (SPE) cartridges. Four kinds of filters, including PTFE, GHP, nylon, and glass fiber, were compared, and PTFE was selected since it had the best recoveries of target sulfonamides (SAs). Three quantitative methods, including external standard (ES), matrix matching (MM), and isotope dilution mass spectrometry (IDMS), were compared, among which IDMS exhibited the best accuracy. The matrix effect under different mobile phase compositions and of different sample matrices were evaluated and discussed. Ion suppression effects were observed during the determination of all SAs, which got stronger with the increase of the methanol composition percent in the mobile phase. After correction by IDMS, the matrix effect could be neglected. Matrix spiked recoveries at three spiked levels (1 μg/kg, 10 μg/kg, and 20 μg/kg) ranged from 96.8% to 103.8% by IDMS. The expanded relative uncertainties were in the range of 2.02% to 5.75%. The method exhibited wide application range, high accuracy, good stability, and high sensitivity.http://dx.doi.org/10.1155/2021/3910253
spellingShingle Chaonan Han
Xiuqin Li
Hui Jiao
Yan Gao
Qinghe Zhang
Accurate Determination, Matrix Effect Estimation, and Uncertainty Evaluation of Three Sulfonamides in Milk by Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry
Journal of Food Quality
title Accurate Determination, Matrix Effect Estimation, and Uncertainty Evaluation of Three Sulfonamides in Milk by Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry
title_full Accurate Determination, Matrix Effect Estimation, and Uncertainty Evaluation of Three Sulfonamides in Milk by Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry
title_fullStr Accurate Determination, Matrix Effect Estimation, and Uncertainty Evaluation of Three Sulfonamides in Milk by Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry
title_full_unstemmed Accurate Determination, Matrix Effect Estimation, and Uncertainty Evaluation of Three Sulfonamides in Milk by Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry
title_short Accurate Determination, Matrix Effect Estimation, and Uncertainty Evaluation of Three Sulfonamides in Milk by Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry
title_sort accurate determination matrix effect estimation and uncertainty evaluation of three sulfonamides in milk by isotope dilution liquid chromatography tandem mass spectrometry
url http://dx.doi.org/10.1155/2021/3910253
work_keys_str_mv AT chaonanhan accuratedeterminationmatrixeffectestimationanduncertaintyevaluationofthreesulfonamidesinmilkbyisotopedilutionliquidchromatographytandemmassspectrometry
AT xiuqinli accuratedeterminationmatrixeffectestimationanduncertaintyevaluationofthreesulfonamidesinmilkbyisotopedilutionliquidchromatographytandemmassspectrometry
AT huijiao accuratedeterminationmatrixeffectestimationanduncertaintyevaluationofthreesulfonamidesinmilkbyisotopedilutionliquidchromatographytandemmassspectrometry
AT yangao accuratedeterminationmatrixeffectestimationanduncertaintyevaluationofthreesulfonamidesinmilkbyisotopedilutionliquidchromatographytandemmassspectrometry
AT qinghezhang accuratedeterminationmatrixeffectestimationanduncertaintyevaluationofthreesulfonamidesinmilkbyisotopedilutionliquidchromatographytandemmassspectrometry