一步式QuEChERS方法结合高效液相色谱-串联质谱法测定牛肉中25种磺胺类药物残留

谢瑜杰 李铁梅 牛相涛 张艳侠 扈斌 吴兴强 范春林 陈辉

谢瑜杰,李铁梅,牛相涛,等. 一步式QuEChERS方法结合高效液相色谱-串联质谱法测定牛肉中25种磺胺类药物残留[J]. 食品工业科技,2021,42(20):268−278. doi:  10.13386/j.issn1002-0306.2021010156
引用本文: 谢瑜杰,李铁梅,牛相涛,等. 一步式QuEChERS方法结合高效液相色谱-串联质谱法测定牛肉中25种磺胺类药物残留[J]. 食品工业科技,2021,42(20):268−278. doi:  10.13386/j.issn1002-0306.2021010156
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

一步式QuEChERS方法结合高效液相色谱-串联质谱法测定牛肉中25种磺胺类药物残留

doi: 10.13386/j.issn1002-0306.2021010156
基金项目: 中国检科院基本科研业务费项目(2020JK010)
详细信息
    作者简介:

    谢瑜杰(1994−),女,硕士研究生,实习研究员,研究方向:食品安全检测,E-mail:1443908316@qq.com

    通讯作者:

    陈辉(1984−),男,博士,副研究员,研究方向:食品安全检测,E-mail:ciqhuichen@163.com

  • 中图分类号: TD207.5+3

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

  • 摘要: 建立了一种基于一步式QuEChERS自动提取和净化的技术,结合高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)同时检测牛肉中25种磺胺类药物残留的检测方法。样品经1%乙酸-乙腈提取,以C18、PSA和无水硫酸镁为净化吸附剂,采用一步式QuEChERS自动化前处理设备提取、净化、离心,经C18色谱柱进行分离,以0.2%甲酸甲醇−0.2%甲酸水(含2 mmol/L乙酸铵)为流动相梯度洗脱,ESI正离子模式扫描,多反应监测(Multi-reaction monitoring, MRM)测定,外标法定量。结果表明,所有化合物在0.1~20 μg/L的浓度范围内线性关系良好,相关系数不低于0.990,检出限(LOD)为0.1~3 μg/kg,定量限(LOQ)为1~10 μg/kg。在1、2和10倍LOQ三个加标浓度水平下,目标化合物的平均回收率范围为70.14%~116.93%,相对标准偏差(RSD)范围为0.95%~13.74%(n=5)。该方法简单快速、准确可靠、可用于检测牛肉中磺胺类药物的残留。
  • 图  1  一步式QuEChERS整合管装置

    Figure  1.  One-step QuEChERS centrifuge tube

    图  2  不同提取液对化合物回收率的影响

    Figure  2.  Effect of different extracts on compound recovery

    图  3  不同提取方式对化合物回收率的影响

    Figure  3.  Effect of different extraction methods on compound recovery

    图  4  不同填料对化合物回收率的影响

    Figure  4.  Effect of different adsorbents on compound recovery

    图  5  不同填料用量对化合物回收率的影响

    Figure  5.  Effect of different adsorbent dosage on compound recovery

    图  6  不同定容液对化合物的影响

    Figure  6.  Influence of different constant volume solutions on compounds

    表  1  25种磺胺类药物的质谱参数

    Table  1.   MS parameters for the 25 sulfonamides

    序号中文名称英文名称母离子(m/z)子离子(m/z)保留时间(min)碎裂电压(V)碰撞能(eV)
    1苯甲酰磺胺Sulfabenzamide277.1156.0*
    108.0
    12.139010
    25
    2磺胺醋酰Sulfacetamide215.1156.1*
    92.0
    5.58705
    20
    3磺胺氯哒嗪Sulfachloropyridazine285.1156.0*
    108.0
    10.459510
    20
    4磺胺氯吡嗪Sulfaclozine285.0108.1*
    155.9
    12.869520
    20
    5磺胺嘧啶Sulfadiazine251.1156.0*
    108.0
    6.558510
    20
    6磺胺间二甲氧嘧啶Sulfadimethoxine311.1156.1*
    108.2
    13.3010020
    20
    7磺胺二甲嘧啶Sulfadimidine279.1186.1*
    156.1
    9.299015
    15
    8磺胺邻二甲氧嘧啶Sulfadoxine311.192.0*
    156.0
    11.3510015
    30
    9磺胺脒Sulfaguanidine215.1156.0*
    108.0
    2.047010
    20
    10磺胺甲基嘧啶Sulfamerazine265.1172.0*
    156.0
    8.089010
    15
    11磺胺对甲氧嘧啶Sulfameter281.1108.1*
    156.2
    10.859525
    15
    12磺胺甲噻二唑Sulfamethizole271.0156.0*
    108.0
    9.219010
    20
    13磺胺甲噁唑Sulfamethoxazole254.1156.0*
    108.0
    10.658510
    25
    14磺胺甲氧哒嗪Sulfamethoxypyridazine281.1156.0*
    108.0
    9.059515
    25
    15磺胺间甲氧嘧啶Sulfamonomethoxine281.1108.1*
    156.1
    9.829525
    15
    16磺胺恶唑Sulfamoxole268.1108.0*
    155.9
    9.038920
    20
    17磺胺Sulfanilamide172.992.0*
    65.0
    3.424510
    25
    18磺胺苯吡唑Sulfaphenazole315.0158.0*
    222.0
    12.7710530
    15
    19磺胺吡啶Sulfapyridine250.1156.0*
    184.0
    7.558010
    15
    20磺胺喹噁啉Sulfaquinoxaline301.1156.0*
    108.0
    13.7410010
    20
    21磺胺噻唑Sulfathiazole256.0156.0*
    108.0
    7.068510
    20
    22磺胺二甲异嘧啶Sulfisomidine279.0124.0*
    186.0
    6.639020
    15
    23磺胺异噁唑Sulfisoxazole268.1113.1*
    156.0
    11.359015
    15
    24磺胺吡唑Sulfapyrazole329.1172.0*
    145.0
    13.6411030
    50
    25甲氧苄啶Trimethoprim291.1123.0*
    230.1
    8.7510025
    25
    注:*表示定量离子。
    下载: 导出CSV

    表  2  牛肉中25种磺胺类化合物的基质效应

    Table  2.   Matrix effect for 25 sulfonamides in beef

    化合物基质效应化合物基质效应
    苯甲酰磺胺3.76磺胺甲氧哒嗪2.10
    磺胺醋酰0.85磺胺间甲氧嘧啶2.48
    磺胺氯哒嗪1.61磺胺恶唑4.29
    磺胺氯吡嗪1.85磺胺4.33
    磺胺嘧啶1.83磺胺苯吡唑2.58
    磺胺间二甲氧嘧啶1.85磺胺吡唑2.09
    磺胺二甲嘧啶1.55磺胺吡啶1.51
    磺胺邻二甲氧嘧啶1.05磺胺喹噁啉1.43
    磺胺脒2.21磺胺噻唑2.43
    磺胺甲基嘧啶1.71磺胺二甲异嘧啶1.97
    磺胺对甲氧嘧啶2.14磺胺异噁唑2.11
    磺胺甲噻二唑1.81甲氧苄啶1.73
    磺胺甲噁唑2.01
    下载: 导出CSV

    表  3  磺胺类药物线性范围、回归方程、相关系数、检出限和定量限

    Table  3.   Linear range, regression equation, correlation coefficient, LOD and LOQ of SAs

    化合物线性范围(μg/L)回归方程相关系数(r检出限(μg/kg)定量限(μg/kg)
    苯甲酰磺胺1~200y=1047.07x+419.600.9960.31
    磺胺醋酰1~200y=91.06x−35.590.99825
    磺胺氯哒嗪1~200y=685.69x−134.790.99715
    磺胺氯吡嗪1~200y=114.38x−57.610.99825
    磺胺嘧啶1~200y=988.77x−318.320.9950.31
    磺胺间二甲氧嘧啶1~200y=2069.12x−1010.290.9960.11
    磺胺二甲嘧啶1~200y=724.42x−148.800.9940.21
    磺胺邻二甲氧嘧啶1~200y=1091.03x−420.120.99715
    磺胺脒1~200y=598.72x+3.380.99715
    磺胺甲基嘧啶1~200y=762.33x−112.500.9990.51
    磺胺对甲氧嘧啶1~200y=1118.66x−1108.480.9990.51
    磺胺甲噻二唑1~200y=675.59x−662.650.9990.11
    磺胺甲噁唑1~200y=787.62x−179.810.9940.11
    磺胺甲氧哒嗪1~200y=638.87x+124.880.9980.11
    磺胺间甲氧嘧啶1~200y=2135.73x−1426.860.9980.11
    磺胺恶唑1~200y=567.95x−853.350.9970.31
    磺胺1~200y=19.38x−34.350.998310
    磺胺苯吡唑1~200y=606.08x+159.990.99413
    磺胺吡唑1~200y=1388.18x−332.400.9960.11
    磺胺吡啶1~200y=954.06x+688.180.9990.11
    磺胺喹噁啉1~200y=922.01x−705.480.9970.11
    磺胺噻唑1~200y=830.06x−460.600.99912
    磺胺二甲异嘧啶1~200y=1602.76x−937.510.9970.11
    磺胺异噁唑1~200y=529.81x−163.950.9980.51
    甲氧苄啶1~200y=817.83x+100.290.9990.51
    下载: 导出CSV

    表  4  准确性和精密度实验结果(n=5)

    Table  4.   Accuracy and precision of the method (n=5)

    化合物添加水平(μg/kg)平均回收率(%)RSD(%)
    苯甲酰磺胺179.227.39
    286.9411.32
    1073.313.48
    磺胺醋酰589.449.98
    1072.204.25
    5077.294.63
    磺胺氯哒嗪575.714.9
    1080.336.09
    5072.251.18
    磺胺氯吡嗪575.414.48
    1083.7213.74
    5073.204.9
    磺胺嘧啶180.613.53
    273.2710.96
    1086.763.35
    磺胺间二甲氧嘧啶174.777.55
    286.2311
    1073.983.61
    磺胺二甲嘧啶198.1410.6
    282.427.66
    1087.398.96
    磺胺邻二甲氧嘧啶589.828.66
    1085.045.27
    5086.133.78
    磺胺脒587.3912.14
    1090.778.29
    5085.015.61
    磺胺甲基嘧啶188.890.95
    282.427.66
    1082.996.39
    磺胺对甲氧嘧啶194.718.63
    290.5410.49
    1090.896.36
    磺胺甲噻二唑176.964.15
    275.426.35
    1072.142.97
    磺胺甲噁唑171.2911.08
    277.919.08
    1079.433.4
    磺胺甲氧哒嗪186.952.13
    286.785.59
    1080.677.49
    磺胺间甲氧嘧啶173.695.72
    273.888.68
    1091.254.4
    磺胺恶唑1116.936.65
    280.9413.26
    1082.6010.74
    磺胺1086.026.4
    2070.146.23
    10093.626.67
    磺胺苯吡唑378.4912.17
    685.1412.06
    3072.814.81
    磺胺吡唑175.825.6
    274.987.77
    1073.893.56
    磺胺吡啶179.957.7
    291.738.16
    1080.164.77
    磺胺喹噁啉170.535.85
    271.3310.83
    1075.096.85
    磺胺噻唑275.212.82
    470.774.07
    2072.205.45
    磺胺二甲异嘧啶191.899.75
    286.477.16
    1085.364.02
    磺胺异噁唑170.449.13
    271.058.61
    1080.565.46
    甲氧苄啶172.846.93
    286.1711.84
    1081.334.48
    下载: 导出CSV
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  • 收稿日期:  2021-01-20
  • 网络出版日期:  2021-09-03
  • 刊出日期:  2021-10-11

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