LI Shuo, ZHANG Can, MA Ling, et al. Simultaneous Determination of 24 Sulfonamide Antibiotics in Fish Products by QuEChERS with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2022, 43(9): 301−308. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021080276.
Citation: LI Shuo, ZHANG Can, MA Ling, et al. Simultaneous Determination of 24 Sulfonamide Antibiotics in Fish Products by QuEChERS with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2022, 43(9): 301−308. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021080276.

Simultaneous Determination of 24 Sulfonamide Antibiotics in Fish Products by QuEChERS with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

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  • Received Date: August 24, 2021
  • Available Online: March 20, 2022
  • A method for the simultaneous determination of 24 sulfonamide antibiotics including sulfamethazine, sulfaguanidine, sulfanilamide and so on in fish products was established by QuEChERS coupled with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The optimal experimental conditions were determined by optimizing the chromatographic and mass spectrometric conditions and the QuEChERS pre-treatment technique. The samples were extracted by acetonitrile under ultrasonication, and then purified by C18 and anhydrous MgSO4. The solvent was detected by UPLC-MS/MS after filtering through 0.20 μm microporous membrane. The separation was performed on an Eclipse XDB-C18 column (4.6 mm × 100 mm, 1.8 μm) using acetonitrile −0.1% formic acid aqueous solution as the mobile phase, and determined with positive ion mode of electrospray ionization (ESI) under multiple reaction monitoring (MRM). Then the matrix matching external standard method was used for quantitative analysis. The results indicated that the 24 sulfonamide antibiotics showed good linearity in the respective linear range with the correlation coefficients (r) higher than 0.999. The average recoveries at three spiked levels of 5, 10 and 50 µg/kg ranged from 80.0% to 116.4% with the relative standard deviation (RSD) of 0.8%~9.4% (n=7). Moreover, the limits of detection (LOD) were 0.01~0.48 µg/kg and the limits of quantification (LOQ) were 0.02~1.59 µg/kg. The method was simple, rapid, selective and sensitive for the high-throughput detection of 24 sulfonamide antibiotics in fish products.
  • [1]
    张婧, 吴剑平, 贡松松, 等. 超高效液相色谱-四级杆-静电场轨道肼高分辨质谱同时快速筛查与确证猪粪中33种磺胺类及四环素类药物[J]. 上海畜牧兽医通讯,2019(6):28−32. [ZHANG J, WU J P, GONG S S, et al. Simultaneous rapid screening and confirmation of 33 sulfonamides and tetracyclines in swine manure by ultra performance liquid chromatography-quadruple rod-electrostatic field orbital hydrazine high resolution mass spectrometry[J]. Shanghai J Animal Husbandry Veterinary Med,2019(6):28−32.
    [2]
    王乐, 李海琴, 王美玲, 等. 基于纳米金-适体结构的智能手机补色波长法检测磺胺二甲嘧啶[J]. 分析测试学报,2018,37(8):967−971. [WANG L, LI H Q, WANG M L, et al. Rapid detection of sulfadimethoxine using a smartphone digital colorimetric method based on aptamer/aunps structure[J]. Instrum Anal,2018,37(8):967−971. doi: 10.3969/j.issn.1004-4957.2018.08.017
    [3]
    CHEN Y, XIA S, HAN X, et al. Simultaneous determination of malachite green, chloramphenicols, sulfonamides, and fluoroquinolones residues in fish by liquid chromatography-mass spectrometry[J]. J Anal Methods Chem,2020,2020:3725618.
    [4]
    赵巧灵, 张薇英, 汤海凤, 等. 快速溶剂萃取-超高效液相色谱-串联质谱法测定养殖鱼肌肉中19种磺胺类药物残留[J]. 食品科技,2019,44(12):335−341. [ZHAO Q L, ZHANG W Y, TANG H F, et al. Determination of 19 sulfonamides residues in cultured fish muscle with accelerated solvent extraction by high performance liquid chromatography-tandem mass spectrometry[J]. Food Sci Technol,2019,44(12):335−341.
    [5]
    李丹, 沈昕, 张玉洁, 等. 高效液相色谱法测定鸡肉中5种磺胺类药物及乙氧酰胺苯甲酯增效剂残留量[J]. 食品安全质量检测学报,2020,11(1):202−208. [LI D, SHEN X, ZHANG Y J, et al. Determination of 5 kinds of sulfonamides and ethopabate resid-usin chicken by high performance liquid chromatography[J]. J Food Saf Qual,2020,11(1):202−208.
    [6]
    刘桂英, 宋广军, 王召会, 等. 固相萃取-超高效液相色谱串联质谱法测定水产品中磺胺类药物残留[J]. 食品安全质量检测学报,2019,10(8):2240−2246. [LIU G Y, SONG G J, WANG Z H, et al. Determination of sulfonamide drugs residues in aquatic product by solid phase extraction-ultra performance liquid chromatography tandem mass spectrometry[J]. J Food Saf Qual,2019,10(8):2240−2246. doi: 10.3969/j.issn.2095-0381.2019.08.024
    [7]
    高振刚, 梁延鹏, 曾鸿鹄, 等. 固相萃取-超高效液相色谱-三重四极杆质谱法测定水中15种抗生素残留[J]. 分析试验室,2021,40(8):875−880. [GAO Z G, LIANG Y P, ZENG H H, et al. Detection of 15 antibiotics in water by solid phase extraction-ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry[J]. Chin J Anal Lab,2021,40(8):875−880.
    [8]
    宋焕杰, 谢卫民, 王俊, 等. SPE-UPLC-MS/MS同时测定水环境中4大类15种抗生素[J]. 分析试验室, 2022, 41(1):50-54.

    SONG H J, XIE W M, WANG J, et al. SPE-UPLC-MS/MS simultaneous determination of 15 antibiotics in four categories in water environment[J]. Chin J Anal Lab, 2022, 41(1):50-54..
    [9]
    ZHOU X, CHEN W Q, DING Y Q, et al. Rapid determination of sulfonamides in chicken using two-dimensional online cleanup mode with three columns coupled to liquid chromatography-tandem mass spectrometry[J]. J Chromatogr B Analyt Technol Biomed Life Sci,2019,1114−1115:110−118. doi: 10.1016/j.jchromb.2019.03.015
    [10]
    DI X, WANG X, LIU Y, et al. Microwave assisted extraction in combination with solid phase purification and switchable hydrophilicity solvent-based homogeneous liquid-liquid microextraction for the determination of sulfonamides in chicken meat[J]. J Chromatogr B Analyt Technol Biomed Life Sci,2019,1118−1119:109−115. doi: 10.1016/j.jchromb.2019.04.036
    [11]
    高洁, 陈达炜, 丁宇琦, 等. 固相萃取-超高效液相色谱-串联质谱法测定畜产品中残留的22种磺胺类药物[J]. 中国食品卫生杂志,2018,30(1):28−34. [GAO J, CHEN D W, DING Y Q, et al. Determination of 22 sulfonamides in livestock products by ultra high performance liquid chromatography-tandem mass spectrometry coupled with solid phase extraction[J]. Chin J Food Hyg,2018,30(1):28−34.
    [12]
    SAXENA S K, RANGASAMY R, KRISHNAN A A, et al. Simultaneous determination of multi-residue and multi-class antibiotics in aquaculture shrimps by UPLC-MS/MS[J]. Food Chem,2018,260:336−343. doi: 10.1016/j.foodchem.2018.04.018
    [13]
    国家市场监督管理总局. GB/T 31650—2019 食品安全国家标准 食品中兽药最大残留限量[S]. 北京: 中国农业出版社, 2019.

    State Administration of Market Supervision. GB/T 31650—2019 National food safety standard. Maximum residue limits for veterinary drugs in food[S]. Beijing: China Agriculture Press, 2019.
    [14]
    GUIDI L R, SANTOS F A, RIBEIRO A C, et al. A simple, fast and sensitive screening LC-ESI-MS/MS method for antibiotics in fish[J]. Talanta,2017,163:85−93. doi: 10.1016/j.talanta.2016.10.089
    [15]
    HELA W , BRANDTNER M , WIDEK R , et al. Determination of sulfonamides in animal tissues using cation exchange reversed phase sorbent for sample cleanup and HPLC-DAD for detection[J]. Food Chemistry,2003,83(4):601−608. doi: 10.1016/S0308-8146(03)00254−1
    [16]
    张林田, 陆奕娜, 黄学泓, 等. 通过式净化-高效液相色谱-串联质谱法测定动物源性食品中42种兽药残留[J]. 分析科学学报,2020,36(1):81−87. [ZHANG L T, LU Y N, HUANG X H, et al. Determination of 42 kinds of veterinary drug residues in animal-derived products by passing purification-high performance liquid chromatography-tandem mass spectrometry[J]. J Anal Sci,2020,36(1):81−87. doi: 10.2116/analsci.19SAP01
    [17]
    区敏霞. 高效液相色谱同时测定水产品中7种磺胺类药物残留的方法改进[J]. 食品安全导刊,2017(21):133−135. [QU M X. Improved method for simultaneous determination of 7 sulfonamides residues in aquatic products by high performance liquid chromatography[J]. Chin Food Saf Mag,2017(21):133−135. doi: 10.3969/j.issn.1674-0270.2017.21.097
    [18]
    ZHANG Y, LIAO W, DAI Y, et al. Covalent organic framework Schiff base network-1-based pipette tip solid phase extraction of sulfonamides from milk and honey[J]. J Chromatogr A,2020,1634:461665. doi: 10.1016/j.chroma.2020.461665
    [19]
    李清雪, 孙王茹, 汪庆. SPE-HPLC测定水中β-内酰胺类、喹诺酮类、磺胺类抗生素[J]. 中国给水排水,2019,35(18):118−122. [LI Q X, SUN W R, WANG Q. Determination of β-lactams, quinolones and sulfonamides antibiotics in water by SPE-HPLC[J]. Chin Water & Wastewater,2019,35(18):118−122.
    [20]
    HERRERA-HERRERA A V, HERNANDEZ-BORGES J, AFONSO M M, et al. Comparison between magnetic and non magnetic multi-walled carbon nanotubes-dispersive solid-phase extraction combined with ultra-high performance liquid chromatography for the determination of sulfonamide antibiotics in water samples[J]. Talanta,2013,116:695−703. doi: 10.1016/j.talanta.2013.07.060
    [21]
    MA J, FAN S, SUN L, et al. Rapid analysis of fifteen sulfonamide residues in pork and fish samples by automated on-line solid phase extraction coupled to liquid chromatography-tandem mass spectrometry[J]. Food Science and Human Wellness,2020,9(4):363−369. doi: 10.1016/j.fshw.2020.05.002
    [22]
    ABAFE O A, GATYENI P, MATIKA L. A multi-class multi-residue method for the analysis of polyether ionophores, tetracyclines and sulfonamides in multi-matrices of animal and aquaculture fish tissues by ultra-high performance liquid chromatography tandem mass spectrometry[J]. Food Addit Contam Part A Chem Anal Control Expo Risk Assess,2020,37(3):438−450. doi: 10.1080/19440049.2019.1705399
    [23]
    庞昕瑞, 曾鸿鹄, 梁延鹏, 等. 固相萃取-超高效液相色谱-串联质谱法测定地表水中10种磺胺类抗生素残留[J]. 分析科学学报,2019,35(4):461−466. [PANG X R, ZENG H H, LIANG Y P, et al. Determination of 10 sulfonamide antibiotic residues in surface water by solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry[J]. J Anal Sci,2019,35(4):461−466. doi: 10.2116/analsci.18N023
    [24]
    XU X, XU X, HAN M, et al. Development of a modified QuEChERS method based on magnetic multiwalled carbon nanotubes for the simultaneous determination of veterinary drugs, pesticides and mycotoxins in eggs by UPLC-MS/MS[J]. Food Chem,2019,276:419−426. doi: 10.1016/j.foodchem.2018.10.051
    [25]
    谭韬, 刘应杰, 唐倩, 等. 毛细管电泳对水体中多类抗生素的同时分离检测[J]. 重庆医学,2018,47(35):4530−4533. [TAN T, LIU Y J, TANG Q, et al. Simultaneous separation and detection of multiple classes of antibiotics in water by capillary electrophoresis[J]. Chongqing Med,2018,47(35):4530−4533. doi: 10.3969/j.issn.1671-8348.2018.35.023
    [26]
    WEN Y, LI J, ZHANG W, et al. Dispersive liquid-liquid microextraction coupled with capillary electrophoresis for simultaneous determination of sulfonamides with the aid of experimental design[J]. Electrophoresis,2011,32(16):2131−2138. doi: 10.1002/elps.201100142
    [27]
    HOFF R. Analysis of sulfonamide residues in bovine liver by liquid chromatography-tandem mass spectrometry without chemical extraction or clean-up procedures[J]. Anal Biochem,2020,611:114011. doi: 10.1016/j.ab.2020.114011
    [28]
    WANG J, XU J, JI X, et al. Determination of veterinary drug/pesticide residues in livestock and poultry excrement using selective accelerated solvent extraction and magnetic material purification combined with ultra-high-performance liquid chromatography-tandem mass spectrometry[J]. Journal of Chromatography A, 2020, 1617.
    [29]
    MARTINS M T, BARRETO F, HOFF R B, et al. Multiclass and multi-residue determination of antibiotics in bovine milk by liquid chromatography-tandem mass spectrometry: Combining efficiency of milk control and simplicity of routine analysis[J]. International Dairy Journal,2016,59:44−51. doi: 10.1016/j.idairyj.2016.02.048
    [30]
    吴利军, 何斌, 周源, 等. 固相萃取-高效液相色谱法同时检测奶牛粪污中5种磺胺类抗生素[J]. 中国兽药杂志,2020,54(10):24−29. [WU L J, HE B, ZHOU Y, et al. Simultaneous determination of five sulfonamide antibiotics in excrement and sewage of dairy farm using solid phase extraction and high performance liquid chromatograph[J]. Chin J Veterinary Drug,2020,54(10):24−29.
    [31]
    WANG K, ZHAO L, ZHANG C, et al. Determination of 12 insect growth regulator residues in foods of different matrixes by modified QuEChERS and UPLC-MS/MS[J]. RSC Advances,2021,11(20):12162−12171. doi: 10.1039/D1RA00046B
    [32]
    扈斌, 谢瑜杰, 蒋康丽, 等. QuEChERS结合高效液相色谱三重四极杆串联质谱法测定花椒中191种农药残留[J]. 分析试验室,2021,40(10):1154−1165. [HU B, XIE Y J, JIANG K L, et al. Quechers combined with high performance liquid chromatography-triple quadrupole tandem mass spectrometry for the determination of 191 pesticide residues in zanthoxylum bungeanum maxim[J]. ChinJ Anal Lab,2021,40(10):1154−1165.
    [33]
    童兰艳, 肖昭竞, 李根容, 等. 超高效液相色谱-三重四极杆质谱法测定化妆品中14种美白活性成分[J]. 分析试验室,2022,41(1):96−102. [TONG L Y, XIAO Z J, LI G R, et al. Determination of 14 whitening active components in cosmetics by ultra-high performance liquid chromatography triple quadrupole mass spectrometry[J]. Chin J Anal Lab,2022,41(1):96−102.
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