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中国精品科技期刊2020
孟春杨,吴玉田,彭蕾,等. 超高效液相色谱-串联质谱法检测卤肉中4种β-受体激动剂残留[J]. 食品工业科技,2024,45(1):277−283. doi: 10.13386/j.issn1002-0306.2023030044.
引用本文: 孟春杨,吴玉田,彭蕾,等. 超高效液相色谱-串联质谱法检测卤肉中4种β-受体激动剂残留[J]. 食品工业科技,2024,45(1):277−283. doi: 10.13386/j.issn1002-0306.2023030044.
MENG Chunyang, WU Yutian, PENG Lei, et al. Determination of 4 Kinds of β-Agonists Residues in Braised Meat by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2024, 45(1): 277−283. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2023030044.
Citation: MENG Chunyang, WU Yutian, PENG Lei, et al. Determination of 4 Kinds of β-Agonists Residues in Braised Meat by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2024, 45(1): 277−283. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2023030044.

超高效液相色谱-串联质谱法检测卤肉中4种β-受体激动剂残留

Determination of 4 Kinds of β-Agonists Residues in Braised Meat by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

  • 摘要: 建立了一种超高效液相色谱串联质谱(ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS)检测卤肉中4种β-受体激动剂(特布他林、克仑特罗、莱克多巴胺、沙丁胺醇)的方法。样品经β-盐酸葡萄糖醛酸苷酶/芳基硫酸酯酶解后,经SLS固相萃取柱净化。以0.1%甲酸水和乙腈为流动相梯度洗脱,用Thermo Hypersil Gold C18色谱柱分离,ESI+进行多反应监测(MRM),内标法定量。4种β-受体激动剂在浓度为0.5~9.5 μg/L范围内线性关系良好,相关系数(r)均大于0.9988,检出限(LOD)为0.1 μg/kg,定量限(LOQ)为0.3 μg/kg。3个加标水平下(1、5、9 μg/kg)的回收率在87.9%~113.7%之间,RSD为1.48%~9.32%。162批次卤肉样品,有一份卤猪蹄样品检出克伦特罗含量为1.51 μg/kg,莱克多巴胺为3.65 μg/kg;另外一份卤羊肉样品检出克伦特罗含量11.5 μg/kg。本方法快速准确,可用于卤肉中4种β-受体激动剂(特布他林、克仑特罗、莱克多巴胺、沙丁胺醇)的定性、定量检测。

     

    Abstract: An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS) method was developed for the determination of four β-agonists (terbutaline, clenbuterol, ractopamine, salbutamol) in braised meat. Samples were hydrolyzed by β-glucuronidase and cleaned up by an SLS solid phase extraction column. The separation was performed on a Thermo Hypersil Gold C18 column with a gradient elution of 0.1% formic acid water and acetonitrile as mobile phases, ESI+ was used for multiple response monitoring (MRM) and quantitative analysis by internal standard method. The linear relationship of the four β-agonists was good in the concentration range of 0.5 μg/L to 9.5 μg/L, and the correlation coefficient (r) was greater than 0.9988. The limit of detection (LOD) was 0.1 μg/kg, and the limit of quantitation (LOQ) was 0.3 μg/kg. The recoveries were 87.9%~113.7% and RSDs were 1.48%~9.32% at three spiked levels (1, 5 and 9 μg/kg). In a total of 162 batches of braised meat samples, one sample of braised pig’s trotter was found to contain 1.51 μg/kg of clenbuterol and 3.65 μg/kg of ractopamine. Additionally, another sample of braised lamb was found to contain 11.5 μg/kg of clenbuterol. The method is rapid and accurate, and can be used for qualitative and quantitative determination of four β-agonists (terbutaline, clenbuterol, ractopamine, salbutamol) in braised meat.

     

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