XIE Yujie, LI Tiemei, NIU Xiangtao, et al. Determination of Sulfonamides in Beef by One Step QuEChERS Method Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(20): 268−278. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021010156.
Citation: XIE Yujie, LI Tiemei, NIU Xiangtao, et al. Determination of Sulfonamides in Beef by One Step QuEChERS Method Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(20): 268−278. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021010156.

Determination of Sulfonamides in Beef by One Step QuEChERS Method Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry

More Information
  • Received Date: January 19, 2021
  • Available Online: August 18, 2021
  • The method for simultaneous determination of 25 sulfonamides residues in beef was established by one-step automatic extraction and purification technology of QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was extracted with 1% acetonitrile acetate, C18, PSA and anhydrous magnesium sulfate were used as purification adsorbents, and the one-step QuEChERS automatic pretreatment equipment was used for extraction, purification and centrifugation. The analytes were separated by a reversed phase C18 column and eluted with 0.2% formic acid methanol and 0.2% formic acid water (containing 2 mmol/L ammonium acetate). The beef sample was analyzed under the multiple reaction monitoring (MRM) mode with positive electrospray ionization (ESI+) and quantify by external standard. The results showed that good linearities were obtained for the 25 sulfonamides in 0.1~20 μg/L with the linear correlation coefficients more than 0.990. The limits of detection (LOD) and the limits of quantification (LOQ) for sulfonamides were 0.1~3 μg/kg and 1~10 μg/kg, respectively. The recoveries at three levels were in the range of 70.14%~116.93%. The repeatability expressed as relative standard deviations (RSD) was ranged from 0.95% to 13.74%(n=5). The method was simple, rapid, accurate and reliable, and could be used to detect the residues of sulfonamides in beef.
  • [1]
    许旭, 肖远灿, 耿丹丹, 等. 在线柱后衍生-高效液相色谱-荧光检测法同时测定牛肉中16种磺胺类药物残留[J]. 色谱,2016,34(4):422−428. [Xu X, Xiao Y C, Geng D D, et al. Simultaneous determination of 16 sulfonamide residues in beef with online post-column derivatization-high performance liquid chromatography-fluorescence detection method[J]. Chinese Journal of Chromatography,2016,34(4):422−428. doi: 10.3724/SP.J.1123.2015.11020
    [2]
    龙举, 马剑锋, 张小军. 荧光胺柱前衍生-高效液相色谱法同时测定水产品中8种磺胺的残留量[J]. 食品安全质量检测学报,2020,11(14):4737−4743. [Long J, Ma J F, Zhang X J. Simultaneous determination of 8 sulfonamide residues in aquatic products by high performance liquid chromatography with fluorescein pre-column derivatization[J]. Journal of Food Safety and Quality Inspection,2020,11(14):4737−4743.
    [3]
    张鸣珊, 李腾崖, 曹小聪, 等. 液液萃取-超高效液相色谱-三重四级杆质谱测定地表水中19种磺胺类药物残留[J]. 环境污染与防治,2020,42(7):838−842. [Zhang M S, Li T Y, Cao X C, et al. Determination of 19 sulfonamide residues in surface water by liquid-liquid extraction-ultra high performance liquid chromatography-triple quadrupole mass spectrometry[J]. Environmental Pollution and Control,2020,42(7):838−842.
    [4]
    Cai Z, Zhang Y, Pan H, et al. Simultaneous determination of 24 sulfonamide residues in meat by ultra-performance liquid chromatography tandem mass spectrometry[J]. Journal of Chromatography A,2008,1200(2):144−155. doi: 10.1016/j.chroma.2008.05.095
    [5]
    庞国芳. 农药兽药残留现代分析技术[M]. 科学出版社, 2007: 366−367.

    Pang Guofang. Modern analysis technology of pesticide and veterinary drug residues[M]. Science Press, 2007: 366−367.
    [6]
    刘志科, 张秋雨, 陈创夫. 一例犊牛磺胺药中毒症状的观察与分析[J]. 广东畜牧兽医科技,2017,42(5):13−16. [Liu Z K, Zhang Q Y, Chen C F. Observation and analysis of a case of calf sulfa poisoning symptoms[J]. Guangdong Animal Husbandry and Veterinary Science and Technology,2017,42(5):13−16. doi: 10.3969/j.issn.1005-8567.2017.05.005
    [7]
    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 sulfonamides and ethoxyamide benzyl synergist residues in chicken by high performance liquid chromatography[J]. Journal of Food Safety and Quality Testing,2020,11(1):202−208.
    [8]
    Xiaoyun D, Xiaofeng L, Yue D, et al. A green HPLC method for determination of nine sulfonamides in milk and beef, and its greenness assessment with analytical eco-scale and greenness profile[J]. Journal of AOAC International, 2020, 103(4).
    [9]
    农业部, 国家卫生和计划生育委员会. GB 29694-2013 食品安全国家标准 动物性食品中13种磺胺类药物多残留的测定 高效液相色谱法[S]. 北京: 国家标准出版社, 2013.

    Ministry of Agriculture, National Health and Family Planning. GB 29694-2013 National Food Safety Standard. Determination of 13 sulfonamide multi-residues in animal foods by high performance liquid chromatography[S]. Beijing: National Standards Press, 2013.
    [10]
    Xiaolei Z, Junying W, Junping W, et al. Development of water-compatible molecularly imprinted solid-phase extraction coupled with high performance liquid chromatography–tandem mass spectrometry for the detection of six sulfonamides in animal-derived foods[J]. Journal of Chromatography A,2018,1574:9−17. doi: 10.1016/j.chroma.2018.08.044
    [11]
    汤云瑜, 杨光昕, 娄晓祎, 等. 液相色谱-串联质谱法测定水产品中8种磺胺类药物残留的不确定度评定[J]. 农产品质量与安全,2020(1):42−48. [Tang Y Y, Yang G X, Lou X Y, et al. Uncertainty evaluation for the determination of 8 sulfonamide residues in aquatic products by liquid chromatography-tandem mass spectrometry[J]. Quality and Safety of Agricultural Products,2020(1):42−48.
    [12]
    国家标准化管理委员会, 国家质量监督检验检疫总局. GB/T 21316-2007 动物源性食品中磺胺类药物残留量的测定 液相色谱-质谱/质谱法[S]. 北京: 国家标准出版社, 2007.

    National Standardization Management Committee, General Administration of Quality Supervision, Inspection and Quarantine. GB/T 21316-2007 Determination of sulfonamide residues in food of animal origin liquid chromatography-mass spectrometry/mass spectrometry[S]. Beijing: National Standards Press, 2007.
    [13]
    李晓雯, 迟秋池, 夏苏捷, 等. 高效液相色谱-四极杆-飞行时间质谱法检测猪肉中22种磺胺类兽药残留[J]. 食品安全质量检测学报,2015(5):1735−1742. [Li X W, Chi Q C, Xia S J, et al. Determination of 22 sulfonamide veterinary drug residues in pork by high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry[J]. Journal of Food Safety and Quality Inspection,2015(5):1735−1742.
    [14]
    于慧娟, 汪洋, 孔聪, 等. 超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查鱼和虾样品中200种药物残留[J]. 质谱学报,2019,40(2):97−108. [Yu H J, Wang Y, Kong C, et al. Rapid screening of 200 drug residues in fish and shrimp samples by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry[J]. Chinese Journal of Mass Spectrometry,2019,40(2):97−108. doi: 10.7538/zpxb.2017.0182
    [15]
    黄鑫, 栾庆祥, 金晓峰, 等. 超高效液相色谱串联质谱法检测鸡肉组织中磺胺氯吡嗪残留量方法的考查[J]. 黑龙江畜牧兽医,2019,565(1):133−136. [Huang X, Luan Q X, Jin X F, et al. Investigation on the detection of sulfaclopyrazine residues in chicken tissues by ultra performance liquid chromatography-tandem mass spectrometry[J]. Heilongjiang Animal Science and Veterinary Medicine,2019,565(1):133−136.
    [16]
    赵金, 常俊斌, 宁凡盛, 等. 高效液相色谱-串联质谱法测定牛奶中磺胺类药物残留测量结果的不确定度评定[J]. 计量技术,2018(11):64−67. [Zhao J, Chang J B, Ning F S, et al. Evaluation of uncertainty of measurement results for the determination of sulfonamide residues in milk by high performance liquid chromatography-tandem mass spectrometry[J]. Metrology Technology,2018(11):64−67.
    [17]
    冯静, 邹淼, 陈曦, 等. 超高效液相色谱-串联质谱法检测牛肉中16种镇静剂类药物残留[J]. 食品安全质量检测学报,2019,10(10):273−278. [Feng J, Zou M, Chen X, et al. Determination of 16 sedative drug residues in beef by ultra performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety Quality Inspection,2019,10(10):273−278.
    [18]
    刘佳佳, 佘永新, 刘洪斌, 等. 高效液相色谱-串联质谱法同时测定动物源性食品中24种磺胺类药物残留[J]. 分析试验室,2011,30(2):9−13. [Liu J J, She Y X, Liu H B, et al. Simultaneous determination of 24 sulfonamide residues in animal-derived foods by high performance liquid chromatography-tandem mass spectrometry[J]. Analytical Laboratory,2011,30(2):9−13. doi: 10.3969/j.issn.1000-0720.2011.02.003
    [19]
    马晓斐, 宋炜, 郭峰, 等. QuEChERS-液相色谱-串联质谱法同时测定蔬菜中16种磺胺类药物[J]. 河北省科学院学报,2019(4):50−57. [Ma X F, Song W, Guo F, et al. Simultaneous determination of 16 sulfonamides in vegetables by QuEChERS-liquid chromatography-tandem mass spectrometry[J]. Journal of Hebei Academy of Sciences,2019(4):50−57.
    [20]
    Te-An K, Chung-Wei T, Bing Chang K, et al. A generic and rapid strategy for determining trace multiresidues of sulfonamides in aquatic products by using an improved QuEChERS method and liquid chromatography-electrospray quadrupole tandem mass spectrometry[J]. Food Chemistry,2015,175(1):189−196.
    [21]
    贝峰, 路川, 王乐勇, 等. QuEChERS-液相色谱串联质谱仪检测猪肉中102种农兽药残留及非法添加物方法的研究[J]. 山东畜牧兽医,2020,41(2):1−3. [Bei F, Lu C, Wang L Y, et al. QuEChERS-liquid chromatography tandem mass spectrometer for detection of 102 pesticides and veterinary drug residues and illegal additives in pork[J]. Shandong Animal Husbandry and Veterinary Medicine,2020,41(2):1−3.
    [22]
    Zhang X, Liu Y, Zhang Z, et al. A novel QuEChERS-like method and automatic sample pre-treatment apparatus for fast determination of mercury speciation in aquatic animal samples[J]. Journal of Analytical Atomic Spectrometry,2019,34(2):292−300. doi: 10.1039/C8JA00323H
    [23]
    Stubbings G, Bigwood T. The development and validation of a multiclass liquid chromatography tandem mass spectrometry (LC-MS/MS) procedure for the determination of veterinary drug residues in animal tissue using a QuEChERS (Quick, easy, cheap, effective, rugged and safe) approach[J]. Analytica Chimica Acta,2009,637(1-2):68−78. doi: 10.1016/j.aca.2009.01.029
    [24]
    农业部. 农业农村部公告第197号-10-2019 畜禽血液和尿液中160种兽药及其它化合物的测定 液相色谱-串联质谱法[S]. 北京: 国家标准出版社, 2019.

    Ministry of Agriculture. Ministry of Agriculture and Rural Affairs Announcement No. 197-10-2019 Determination of 160 veterinary drugs and other compounds in livestock and poultry blood and urine liquid chromatography-tandem mass spectrometry[S]. Beijing: National Standards Press, 2019.
    [25]
    任丹丹, 谢云峰, 李少晖, 等. 超高效液相色谱-串联质谱法测定畜禽肉中17种磺胺类药物残留[J]. 食品安全质量检测学报,2018(4):858−863. [Ren D D, Xie Y F, Li S H, et al. Determination of 17 kinds of sulfonamide residues in livestock and poultry meat by ultra performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety and Quality Testing,2018(4):858−863. doi: 10.3969/j.issn.2095-0381.2018.04.029
    [26]
    罗辉泰, 谢梦婷, 黄晓兰, 等. 分散固相萃取-高效液相色谱-串联质谱法同时测定畜禽肉中63种兽药残留[J]. 色谱,2015,33(4):354−362. [Luo H T, Xie M T, Huang X L, et al. Simultaneous determination of 63 veterinary drug residues in livestock and poultry meat by dispersive solid phase extraction-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography,2015,33(4):354−362. doi: 10.3724/SP.J.1123.2014.12005
    [27]
    黄泽玮, 闵宇航, 杜钢, 等. QuEChERS EMR-Lipid技术结合LC/MS/MS快速筛查与确证猪肉中55种兽药残留[J]. 食品工业科技,2019,40(11):270−276, 283. [Huang Z W, Min Y H, Du G, et al. QuEChERS EMR-Lipid technology combined with LC/MS/MS for rapid screening and confirmation of 55 veterinary drug residues in pork[J]. Food Industry Science and Technology,2019,40(11):270−276, 283.
    [28]
    戴尽波, 沈洁, 何啸峰, 等. QuEChERS-超高效液相色谱-串联质谱法检测禽源性食品中氟虫腈及其代谢物[J/OL]. 食品科学: 1−12[2021-01-17]. http://kns.cnki.net/kcms/detail/11.2206.TS.20200330.1359.046.html.

    Dai J B, Shen J, He X F, et al. Optimization of a QuEChERS based method by response surface methodology for fipronil and its metabolites determination in poultry food by UHPLC-MS/MS [J/OL]. Food Science: 1−12[2021-01-17]. http://kns.cnki.net/kcms/detail/11.2206.TS.20200330.1359.046.html.
  • Cited by

    Periodical cited type(12)

    1. 王潇,李栋,张立攀. 杜仲叶不同溶剂萃取物对ACE酶活的抑制作用. 河南化工. 2024(01): 25-30 .
    2. 李硕,尼格尔热依·亚迪卡尔,朱金芳,冯作山,邓术升. 小白杏生理落果中多酚提取及体外抗氧化活性分析. 新疆农业科学. 2024(03): 623-631 .
    3. 梅瀚,曹金凤,刘世巍,马建龙,丁建海. 超声辅助提取葡萄籽中原花青素工艺及抗氧化活性研究. 广东化工. 2023(05): 38-41 .
    4. 徐兰程,杨佳燕,徐惠,陈金玉,何碧梅,王晓平,辛桂瑜. 响应面法优化芒果核黄酮提取工艺研究. 中国饲料. 2023(08): 18-22 .
    5. 马嘉洁,赵端端,全世航,郇淇童,郝帅,李坤,朴春香,李官浩,李红梅,牟柏德. 紫苏叶黄酮、多酚提取工艺优化及不同品种抗氧化活性比较. 食品工业科技. 2023(12): 344-352 . 本站查看
    6. 杨郑州,李曦,谢晓娜. 芒果皮多酚提取工艺的优化及抗氧化能力分析. 江西农业学报. 2023(05): 103-108 .
    7. 陈徐回,熊财智,梅瀚,马建龙,曹金凤,刘世巍,丁建海. 葡萄籽抗氧化活性成分研究. 广州化工. 2023(09): 77-80 .
    8. 康超,聂辉,黄双全,伍淑婕,刘凤听. 芒果不同部位多酚化合物抗氧化和抑菌活性研究. 食品科技. 2023(07): 170-175 .
    9. 万荣,农斯伟,杨郑州,卢春静,朱正杰,侯宪斌. 芒果皮核生物学功能及其在动物养殖中的应用研究进展. 饲料研究. 2022(08): 147-149 .
    10. 高国燕,蒋林树,年芳,王慧. 不同省份小果沙棘叶中黄酮类化合物含量测定及体外抗氧化能力评价. 中国饲料. 2022(10): 30-35 .
    11. 郭荣珍,梁茂文,刘纯友,杨锋,丘静. 芒果核提取物对冷藏过程中水牛肉品质的影响. 广西科技大学学报. 2022(04): 100-106 .
    12. 关淑文,潘予琮,寇伟,年芳,蒋林树. 基于高效液相色谱特征指纹图谱法探究不同品种苜蓿中黄酮抗氧化活性的谱-效关系. 动物营养学报. 2022(12): 8086-8096 .

    Other cited types(4)

Catalog

    Article Metrics

    Article views (276) PDF downloads (25) Cited by(16)

    /

    DownLoad:  Full-Size Img  PowerPoint
    Return
    Return