碱水解-SPE-LC-MS/MS法快速测定动物源食品中喹乙醇代谢物残留量
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(1. 湖北省食品质量安全监督检验研究院,湖北 武汉 430075;2. 湖北省食品质量安全检测工程技术研究中心,湖北 武汉 430075)

作者简介:

刘迪,男,湖北省食品质量安全监督检验研究院工程师,硕士。

通讯作者:

余婷婷(1985—),女,湖北省食品质量安全监督检验研究院工程师,博士。E-mail:271377735@qq.com

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国家重点研发计划(编号:2018YFC1602302)


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Affiliation:

(1. Hubei Provincial Institute for Food Supervision and Test, Wuhan, Hubei 430075, China; 2. Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan, Hubei 430075, China)

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    摘要:

    建立了一种快速准确定性定量检测动物源性食品中喹乙醇代谢物3-甲基-喹喔啉-2-羧酸(MQCA)残留量的液相色谱—串联质谱(LC-MS/MS)检测方法。样品组织通过碱水解提取MQCA,阴离子固相萃取柱净化,LC-MS/MS检测,内标法定量。结果显示,在0.5~50.0 ng/mL 浓度范围内,MQCA线性关系良好,相关系数R2为0.999 7。MQCA检出限为0.1 μg/kg,方法在0.1,0.2,1.0 μg/kg的添加水平下,回收率为95.6%~108.2%,相对标准偏差为3.4%~14.3%(n=6)。该检测方法准确、快速、灵敏度高,适用于动物源食品中MQCA残留量的检测和确证。

    Abstract:

    A rapid quasi-deterministic quantitative method for the determination of 3-methyl-quinoxaline-2-carboxylic acid (MQCA) residues in olaquindox metabolites of animal-derived foods was developed, by using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The sample tissue was extracted by alkaline hydrolysis to extract MQCA, purified by anion solid phase extraction column, and detected by LC-MS/MS, and then quantified by internal standard method. The results showed that MQCA had a good linear relationship in the concentration range of 0.5~50.0 ng/mL, and the correlation coefficient was 0.999 7. The detection limit of MQCA was 0.1 μg/kg. The recovery rate was 95.6%~108.2% at the addition level of 0.1, 0.2 and 1.0 μg/kg, and the relative standard deviation was 3.4%~14.3% (n=6). In conclusion, the detection method above was accurate, rapid and sensitive, and suitable for detecting and confirming the residual amount of MQCA in animal foods.

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刘迪,韩莉,曾妮,等.碱水解-SPE-LC-MS/MS法快速测定动物源食品中喹乙醇代谢物残留量[J].食品与机械,2019,(11):70-74.
LIU Di, HAN Li, ZENG Ni, et al.[J]. Food & Machinery,2019,(11):70-74.

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  • 收稿日期:2019-08-04
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  • 在线发布日期: 2022-11-24
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