通过型固相萃取净化-超高效液相色谱-串联质谱法检测鸡肉中23种磺胺类药物残留

杨坤 刘桂琼 管春成 陈光静

杨坤,刘桂琼,管春成,等. 通过型固相萃取净化-超高效液相色谱-串联质谱法检测鸡肉中23种磺胺类药物残留[J]. 食品工业科技,2021,42(18):284−291. doi:  10.13386/j.issn1002-0306.2020120074
引用本文: 杨坤,刘桂琼,管春成,等. 通过型固相萃取净化-超高效液相色谱-串联质谱法检测鸡肉中23种磺胺类药物残留[J]. 食品工业科技,2021,42(18):284−291. doi:  10.13386/j.issn1002-0306.2020120074
YANG Kun, LIU Guiqiong, GUAN Chuncheng, et al. Determination of 23 Sulfonamide Drugs Residues in Chicken by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry with Pass-through Solid Phase Extraction[J]. Science and Technology of Food Industry, 2021, 42(18): 284−291. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2020120074
Citation: YANG Kun, LIU Guiqiong, GUAN Chuncheng, et al. Determination of 23 Sulfonamide Drugs Residues in Chicken by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry with Pass-through Solid Phase Extraction[J]. Science and Technology of Food Industry, 2021, 42(18): 284−291. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2020120074

通过型固相萃取净化-超高效液相色谱-串联质谱法检测鸡肉中23种磺胺类药物残留

doi: 10.13386/j.issn1002-0306.2020120074
详细信息
    作者简介:

    杨坤(1988−),男,本科,工程师,研究方向:食品质量与安全,E-mail:15158135065@126.com

    通讯作者:

    陈光静(1989−),男,博士,副教授,研究方向:食品化学与营养学、食品质量与安全控制,E-mail:gjchen1989@126.com

  • 中图分类号: TS251.7

Determination of 23 Sulfonamide Drugs Residues in Chicken by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry with Pass-through Solid Phase Extraction

  • 摘要: 建立了通过型固相萃取净化超高效液相色谱-串联质谱法同时检测鸡肉中23种磺胺类药物残留的分析方法。鸡肉样品经80%乙腈溶液(含0.2%甲酸)提取,Oasis PRiME HLB固相萃取柱进行净化,用Waters Acquity UPLC CSH C18色谱柱(100 mm×2.1 mm,1.7 μm)分离,以甲醇和0.1%甲酸溶液为流动相梯度洗脱,电喷雾源正离子扫描及依赖保留时间的多反应监测模式下(Scheduled MRM)检测,外标法定量。结果表明:23种磺胺类药物在线性范围0.2~20 ng/mL上有良好的线性关系,相关系数均大于0.9996;检出限为0.1~2.0 μg/kg,定量限为0.25~5.0 μg/kg;在1.0、2.0、5.0 μg/kg三个加标水平上平均回收率为66.12%~99.83%,相对标准偏差(RSD,n=6)为0.72%~10.36%;该方法操作简单、灵敏度高、重现性好,适用于鸡肉中多种磺胺类药物残留的检测。
  • 图  1  不同提取剂对磺胺药物的平均回收率比较

    Figure  1.  Comparison of average recovery rates of sulfonamides by different extracters

    注:A为60%乙腈水溶液;B为70%乙腈水溶液;C为80%乙腈水溶液;D为90%乙腈水溶液;E为80%乙腈水溶液(含0.2%甲酸);F为80%乙腈水溶液(含0.2%氨水)。

    图  2  混合标准溶液的质谱图

    Figure  2.  Mass spectrogram of mixed standard solution

    注:1、磺胺脒;2、磺胺醋酰;3、磺胺索嘧啶;4、磺胺嘧啶;5、甲氧苄氨嘧啶;6、磺胺噻唑;7、磺胺吡啶;8、磺胺甲基嘧啶;9、磺胺噁唑;10、磺胺对甲氧嘧啶;11、磺胺二甲基嘧啶;12、磺胺甲噻二唑;13、磺胺甲氧哒嗪;14、磺胺氯哒嗪;15、磺胺甲基异噁唑;16、磺胺间甲氧嘧啶;17、磺胺邻二甲氧嘧啶;18、磺胺异恶唑;19、磺胺苯甲酰;20、磺胺苯吡唑;21、磺胺间二甲氧嘧啶;22、磺胺喹恶啉;23、磺胺硝苯。混合标准溶液的质量浓度为20 ng/mL。

    图  3  3种磺胺的同分异构体色谱图

    Figure  3.  Chromatograms of three sulfonamides

    注:A代表有机相为乙腈,B代表有机相为甲醇。

    图  4  23种磺胺化合物在鸡肉中的基质效应图

    Figure  4.  Matrix effect diagram of 23 sulfonamides in chicken

    表  1  23种磺胺类药物的质谱参数

    Table  1.   Mass spectrometric parameters of 23 sulfonamides

    序号.化合物保留时间(min)定量/定性离子(m/z)去蔟电压(V)碰撞能量(eV)
    1磺胺脒1.28215.0/156.0*,215.0/108.05215,29
    2磺胺醋酰2.52215.0/156.0*,215.0/108.05215,29
    3磺胺索嘧啶2.74279.1/124.1*,279.1/186.18030,23
    4磺胺嘧啶3.18251.1/156.0*,251.1/108.16322,34
    5甲氧苄氨嘧啶3.31291.1/230.1*,291.1/123.19533,34
    6磺胺噻唑3.65256.1/156.1*,256.1/108.16022,35
    7磺胺吡啶3.86250.1/156.0*,250.1/184.16523,23
    8磺胺甲基嘧啶4.33265.1/156.1*,265.1/172.07324,24
    9磺胺噁唑5.10268.1/156.0*,268.1/113.17021,23
    10磺胺对甲氧嘧啶5.32281.1/156.1*,281.1/108.17025,35
    11磺胺二甲基嘧啶5.41279.1/156.0*,279.1/186.07527,25
    12磺胺甲噻二唑5.49271.0/156.1*,271.0/108.06521,40
    13磺胺甲氧哒嗪5.91281.0/156.0*,281.0/108.17525,36
    14磺胺氯哒嗪6.72285.1/156.0*,285.1/108.16522,37
    15磺胺甲基异噁唑7.07254.1/156.0*,254.1/108.07023,32
    16磺胺间甲氧嘧啶7.41281.1/156.0*,281.1/108.17525,36
    17磺胺邻二甲氧嘧啶7.83311.0/156.0*,311.0/108.18026,44
    18磺胺异恶唑8.24268.1/156.0*,268.1/113.17021,23
    19磺胺苯甲酰8.89277.1/156.0*,277.1/108.16019,32
    20磺胺苯吡唑9.06315.0/156.0*,315.0/222.18429,28
    21磺胺间二甲氧嘧啶9.16311.0/156.1*,311.0/108.18031,38
    22磺胺喹恶啉9.26301.0/156.1*,301.0/108.08024,36
    23磺胺硝苯9.64336.1/294.0*,336.1/198.07521,26
    注:*代表定量离子。
    下载: 导出CSV

    表  2  23种磺胺类兽药在鸡肉样品中标准曲线、相关系数、检出限及定量限

    Table  2.   Standard curve, correlation coefficient, detection limit and quantitative limit of 23 sulfonamides in chicken samples

    序号.化合物线性范围
    (ng/mL)
    标准曲线相关系数检出限
    (μg/kg)
    定量限
    (μg/kg)
    1磺胺脒0.4~20y=2.3e3x−6.65e20.99960.502.00
    2磺胺醋酰0.2~20y=1.77e4x+1.42e30.99980.200.60
    3磺胺索嘧啶0.2~20y=4.5e4x+5.02e30.99990.100.30
    4磺胺嘧啶0.2~20y=1.35e4x+2.13e20.99980.220.60
    5甲氧苄氨嘧啶0.2~20y=1.65e4x+2.13e30.99980.200.65
    6磺胺噻唑0.2~20y=1.39e4x+4.09e20.99990.250.50
    7磺胺吡啶0.2~20y=1.66e4x+1.82e30.99980.180.50
    8磺胺甲基嘧啶0.2~20y=8.5e3x+9.67e20.99980.250.60
    9磺胺噁唑0.2~20y=1.08e4x+6.50e20.99990.250.62
    10磺胺对甲氧嘧啶0.2~20y=1.14e4x+8.13e20.99980.200.50
    11磺胺二甲基嘧啶0.2~20y=9.44e3x+9.25e20.99990.200.60
    12磺胺甲噻二唑0.2~20y=1.18e4x+1.78e30.99960.130.40
    13磺胺甲氧哒嗪0.2-20y=1.37e4x+1.37e30.99980.150.50
    14磺胺氯哒嗪0.2~20y=9.64e3x+5.83e20.99980.200.60
    15磺胺甲基异噁唑0.2~20y=6.34e3x+6.35e20.99960.100.25
    16磺胺间甲氧嘧啶0.2~20y=8.08e3x+7.95e20.99970.200.50
    17磺胺邻二甲氧嘧啶0.2~20y=2.19e4 x+2.52e30.99990.150.40
    18磺胺异恶唑0.2~20y=8.87e3x+1.37e30.99970.150.40
    19磺胺苯甲酰0.2~20y=9.16e3x+1.58e30.99960.200.50
    20磺胺苯吡唑0.2~20y=3.45e3x+5.94e20.99980.250.70
    21磺胺间二甲氧嘧啶0.2~20y=1.35e4x+2.18e30.99990.120.30
    22磺胺喹恶啉0.2~20y=3.30e3x+8.11e20.99980.200.65
    23磺胺硝苯1.0~20y=1.64e2x+5.82e20.99982.005.00
    下载: 导出CSV

    表  3  实际空白样品中23种磺胺类药物的加标回收率和相对标准偏差(n=6)

    Table  3.   Spiked recoveries rate and relative standard deviations of 23 sulfonamide drugs in real blank samples (n=6)

    序号.
    化合物
    1.0 μg/kg 2.0 μg/kg 5.0 μg/kg
    Rec(%)RSD(%)Rec(%)RSD(%)Rec(%)RSD(%)
    1磺胺脒79.64.07 92.523.73 90.771.53
    2磺胺醋酰98.128.8599.830.7294.073.82
    3磺胺索嘧啶88.892.6597.512.7393.850.64
    4磺胺嘧啶91.672.2495.421.2395.452.21
    5甲氧苄氨嘧啶92.973.4696.403.9696.071.83
    6磺胺噻唑90.941.1594.580.9583.032.20
    7磺胺吡啶95.765.4785.641.8891.982.97
    8磺胺甲基嘧啶94.975.0080.803.3791.203.86
    9磺胺噁唑83.804.6378.333.3688.084.41
    10磺胺对甲氧嘧啶87.682.7788.583.2589.972.43
    11磺胺二甲基嘧啶89.595.9785.924.7992.225.43
    12磺胺甲噻二唑84.146.6878.314.9488.016.01
    13磺胺甲氧哒嗪85.983.7984.473.6689.034.98
    14磺胺氯哒嗪83.636.1878.843.6083.426.26
    15磺胺甲基异噁唑88.864.5882.303.6492.615.72
    16磺胺间甲氧嘧啶85.992.7286.354.8885.854.21
    17磺胺邻二甲氧嘧啶88.493.8085.301.7588.044.08
    18磺胺异恶唑85.416.1475.554.9682.467.42
    19磺胺苯甲酰89.142.1182.445.9282.517.45
    20磺胺苯吡唑72.032.7383.893.9480.556.12
    21磺胺间二甲氧嘧啶84.203.8576.513.6679.544.48
    22磺胺喹恶啉84.306.0972.726.7369.002.24
    23磺胺硝苯N/AN/A66.126.7687.6810.36
    下载: 导出CSV
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出版历程
  • 收稿日期:  2020-12-09
  • 网络出版日期:  2021-08-06
  • 刊出日期:  2021-09-14

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