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中国精品科技期刊2020 食品青年科学家峰会

QuEChERS EMR Lipid净化结合同位素稀释-超高效液相色谱-串联质谱法同时测定畜肉中17种β-受体激动剂

毛锐 林浩 刘川 姚静 肖全伟 戴琴

毛锐,林浩,刘川,等. QuEChERS EMR Lipid净化结合同位素稀释-超高效液相色谱-串联质谱法同时测定畜肉中17种β-受体激动剂[J]. 新宝登录入口(中国)有限公司,2023,44(15):323−331. doi:  10.13386/j.issn1002-0306.2022090195
引用本文: 毛锐,林浩,刘川,等. QuEChERS EMR Lipid净化结合同位素稀释-超高效液相色谱-串联质谱法同时测定畜肉中17种β-受体激动剂[J]. 新宝登录入口(中国)有限公司,2023,44(15):323−331. doi:  10.13386/j.issn1002-0306.2022090195
MAO Rui, LIN Hao, LIU Chuan, et al. Simultaneous Determination of 17 β-Receptor Agonists in Meat by QuEChERS EMR-Lipid with Isotope Dilution-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2023, 44(15): 323−331. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2022090195
Citation: MAO Rui, LIN Hao, LIU Chuan, et al. Simultaneous Determination of 17 β-Receptor Agonists in Meat by QuEChERS EMR-Lipid with Isotope Dilution-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2023, 44(15): 323−331. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2022090195

QuEChERS EMR Lipid净化结合同位素稀释-超高效液相色谱-串联质谱法同时测定畜肉中17种β-受体激动剂

doi: 10.13386/j.issn1002-0306.2022090195
详细信息
    作者简介:

    毛锐(1989−),女,硕士,工程师,研究方向:食品安全与质量检测,E-mail:maorui0428@126.com

    通讯作者:

    戴琴(1984−),女,硕士,高级工程师,研究方向:食品安全与质量检测,E-mail:740747208@qq.com

  • 中图分类号: O657.63

Simultaneous Determination of 17 β-Receptor Agonists in Meat by QuEChERS EMR-Lipid with Isotope Dilution-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

  • 摘要: 目的:建立了一种采用QuEChERS EMR Lipid净化结合同位素稀释-超高效液相色谱-串联质谱技术同时测定畜肉中17种β-受体激动剂药物残留的检测方法。方法:样品加入pH为5.2的乙酸铵缓冲溶液,以β-葡萄糖醛苷酶/芳基硫酸酯酶酶解,经5%甲酸乙腈提取,QuEChERS EMR Lipid净化,采用CORTECS™ UPLC® C18柱(3.0 mm×100 mm,1.6 μm),0.1%甲酸水和甲醇梯度洗脱,在分时段多反应监测(scheduled MRM,sMRM)模式下测定,内标法定量。结果:17种β-受体激动剂在0~20 ng/mL浓度范围内线性相关系数均大于0.99,方法检出限为0.01~0.09 μg/kg,定量限为0.05~0.31 μg/kg。在0.5、2.0、5.0 μg/kg 3个加标浓度水平下的平均回收率为81.7%~111.8%,RSD为0.8%~10.3%(n=6)。100批市售生鲜畜肉中未检出β-受体激动剂。结论:该法前处理步骤简便,净化效果良好,缩短酶解时间,提高了样品检测效率,内标法定量精准可靠,适用于大批量畜肉样品中多种β-受体激动剂药物残留的同时检测。
  • 图  1  17种β-受体激动剂的提取离子流色谱图

    Figure  1.  Extracted ion chromatogram of 17 β-receptor agonists

    注:1.特布他林;2.沙丁胺醇;3.西布特罗;4.非诺特罗;5.羟甲基克伦特罗;6.莱克多巴胺;7.氯丙那林;8.克伦特罗;9.福莫特罗;10.妥布特罗;11.溴布特罗;12.马布特罗;13.克仑潘特;14.班布特罗;15.马喷特罗;16.苯乙醇胺A;17.喷布特罗。

    图  2  牛肉、猪肉、羊肉样品中17种β-受体激动剂的绝对萃取回收率

    Figure  2.  Absolute extraction recovery of 17 β-receptor agonists in beef, pork and mutton

    图  3  牛肉、猪肉、羊肉样品中17种β-受体激动剂的基质效应

    Figure  3.  Matrix effect of 17 β-receptor agonists in beef, pork and mutton

    图  4  牛肉样品QuEChERS法与MCX法基质效应对比图

    Figure  4.  Matrix effect comparison between QuEChERS method and MCX method in beef samples

    图  5  牛肉样品QuEChERS法与MCX法绝对萃取回收率对比图

    Figure  5.  Absolute extraction recovery comparison between QuEChERS method and MCX method in beef samples

    表  1  17种β-受体激动剂的质谱参数

    Table  1.   Mass spectrometric parameters of 17 β-receptor agonists

    分析物内标保留时间(min)监测离子(m/z)去簇电压(V)碰撞能量 (eV)
    羟甲基克伦特罗克伦特罗-D97.25293.1>203.1*,293.1>275.16527,17
    马喷特罗马布特罗-D912.26324.8>237.1*,324.8>217.16525,37
    喷布特罗喷布特罗-D914.49292.3>236.2*,292.3>201.16522,28
    克伦特罗克伦特罗-D99.48277.1>203.1*,277.1>259.16522,16
    特布他林特布他林-D93.43226.1>152.1*,226.1>125.16523,32
    溴布特罗溴布特罗-D911.05367.0>293.0*,367.0>348.96526,17
    苯乙醇胺A苯乙醇胺A-D312.74345.2>150.2*,345.2>327.26533,19
    非诺特罗莱克多巴胺-D34.91304.2>107.1*,304.2>135.16547,25
    莱克多巴胺莱克多巴胺-D38.24302.1>163.9*,302.1>107.06523,56
    克仑潘特马布特罗-D911.51291.1>202.8*,291.1>273.16524,15
    氯丙那林氯丙那林-D78.90214.1>154.1*,214.1>195.96527,18
    福莫特罗莱克多巴胺-D310.13345.1>148.9*,345.1>326.86527,19
    妥布特罗妥布特罗-D910.94228.1>153.8*,228.1>172.26522,16
    沙丁胺醇沙丁胺醇-D33.57240.1>148.2*,240.1>222.16527,15
    班布特罗班布特罗-D911.69368.2>294.1*,368.2>312.16527,21
    马布特罗马布特罗-D911.28311.0>237.1*,311.0>217.16524,37
    西布特罗西布特罗-D94.38234.2>159.8*,234.2>143.26521,35
    马布特罗-D911.22320.2>238.16526
    班布特罗-D911.66377.2>295.26531
    妥布特罗-D910.87237.2>155.16521
    氯丙那林-D78.84221.1>155.16526
    喷布特罗-D914.47301.2>237.16526
    特布他林-D93.38235.3>153.26525
    溴布特罗-D910.99376.1>294.06529
    莱克多巴胺-D38.08305.2>167.26522
    苯乙醇胺A-D312.71348.2>153.36533
    克伦特罗-D99.38286.2>204.26524
    沙丁胺醇-D33.53243.2>151.26528
    西布特罗-D9 4.31243.2>161.16515
    注:*为定量离子对。
    下载: 导出CSV

    表  2  17种β-受体激动剂线性范围、回归方程、相关系数、检出限及定量限

    Table  2.   Linear equation, correlation coefficient, LOD, LOQ of 17 β-receptor agonists

    组分名称线性范围(μg/L)回归方程相关系数检出限(μg/kg)定量限(μg/kg)
    克仑潘特0~20y=0.0919x+−2.12e−013r=0.99570.070.22
    羟甲基克伦特罗0~20y=0.0435x+−1.16e−013r=0.99840.090.31
    马喷特罗0~20y=0.15x+1.45e−014r=0.99910.040.12
    喷布特罗0~20y=0.172x+−3.34e−014r=0.99960.020.08
    克伦特罗0~20y=0.0753x+3.28e−014r=0.99990.080.25
    特布他林0~20y=0.182x+1.5e−013r=0.99900.050.16
    溴布特罗0~20y=0.123x+−2.23e−013r=0.99860.060.20
    苯乙醇胺A0~20y=0.101x+−1.74e−014r=0.99930.040.12
    非诺特罗0~20y=0.273x+1.16e−012r=0.99870.040.12
    莱克多巴胺0~20y=0.199x+3.65e−013r=0.99970.050.16
    氯丙那林0~20y=0.105x+−3.54e−014r=0.99980.040.14
    福莫特罗0~20y=0.32x+7.85e−013r=0.99950.030.09
    妥布特罗0~20y=0.2x+7.87e−013r=0.99810.050.15
    沙丁胺醇0~20y=0.117x+−2.95e−013r=0.99890.050.15
    班布特罗0~20y=0.236x+−2.49e−013r=0.99750.010.05
    马布特罗0~20y=0.162x+4.56e−013r=0.99800.030.11
    西布特罗0~20y=0.164x+−6.21e−013r=0.99820.080.28
    下载: 导出CSV

    表  3  17种β-受体激动剂回收率及精密度(n=6)

    Table  3.   Recoveries and RSD of 17 β-receptor agonists (n=6)

    组分名称加标水平
    (μg/kg)
    猪肉 牛肉 羊肉
    回收率(%)RSD(%)回收率(%)RSD(%)回收率(%)RSD(%)
    克仑潘特0.588.25.9 88.64.9 88.55.8
    288.64.988.93.387.83.1
    590.25.289.45.888.94.7
    羟甲基克伦特罗0.596.26.794.26.093.35.4
    294.35.493.77.793.54.5
    596.89.896.18.899.51.5
    马喷特罗0.592.91.295.77.891.21.7
    292.34.690.85.198.54.2
    589.13.291.03.294.72.4
    喷布特罗0.5100.04.5102.56.7102.93.3
    2102.94.8103.74.4108.01.4
    5104.72.5105.31.7108.24.6
    克伦特罗0.599.83.195.42.8103.36.4
    2102.03.4101.98.0100.84.9
    5100.61.799.84.098.34.2
    特布他林0.5100.32.596.88.399.05.4
    2101.12.591.44.897.89.3
    597.93.099.24.699.62.4
    溴布特罗0.5100.81.0106.53.3106.93.6
    2109.32.9111.83.6108.64.1
    5107.02.9110.85.7103.44.6
    苯乙醇胺A0.5101.97.2101.48.3105.56.7
    2101.14.1101.54.699.35.5
    5100.33.9103.08.0101.81.5
    非诺特罗0.584.13.681.71.586.53.1
    283.92.484.84.292.26.7
    583.13.686.72.290.310.3
    莱克多巴胺0.591.01.693.14.695.57.6
    298.14.4100.33.593.96.3
    5100.43.5100.14.597.36.6
    氯丙那林0.5105.34.394.77.398.96.6
    2101.92.8103.73.999.51.4
    5101.93.7104.64.4103.13.3
    福莫特罗0.596.32.7 99.36.6 99.65.5
    292.54.699.95.092.47.8
    593.86.0105.01.098.52.7
    妥布特罗0.593.94.296.310.292.73.3
    292.24.391.84.492.54.7
    595.33.699.37.597.16.1
    沙丁胺醇0.5102.34.290.92.794.33.7
    2100.91.993.42.394.42.9
    599.30.8105.04.4102.95.2
    班布特罗0.5100.41.1100.84.1100.71.5
    298.71.8101.15.099.95.7
    5102.36.0100.76.798.57.0
    马布特罗0.598.30.899.84.8106.62.9
    298.22.299.91.1111.61.0
    5105.81.8101.55.6104.91.6
    西布特罗0.5100.65.899.26.6106.42.6
    2100.64.198.47.799.92.7
    597.06.5103.38.2111.21.4
    下载: 导出CSV
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  • 收稿日期:  2022-09-20
  • 网络出版日期:  2023-06-19

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