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液相色谱-串联质谱法测定鸡肉中喹乙醇标记残留3-甲基喹喔啉-2-羧酸

[Determination of 3-methylquinoxaline-2-carboxylic acid of olaquindox marker residue in chicken muscles by liquid chromatography-tandem mass spectrometry].

作者信息

Li Erfen, Zhang Meiyu, Ma Heqin, Zhang Jiahui, Liu Rong, Zeng Zhenling, He Limin

机构信息

National Reference Laboratory of Veterinary Drug Residues(SCAU), College of Veterinary Medicine, South China Agricultural University, Guangzhou 510642, China.

Foshan Shunde District Agricultural Integrated Service Center, Foshan 528333, China.

出版信息

Se Pu. 2018 May 8;36(5):446-451. doi: 10.3724/SP.J.1123.2017.12023.

Abstract

A simple, sensitive, scientific and reproducible liquid chromatography-tandem mass spectrometric method was developed to determine 3-methylquinoxaline-2-carboxylic acid (MQCA) of olaquindox marker residue in chicken muscle tissues. The chickens were administered orally with olaquindox and used as positive samples. The approaches, enzyme, acid, and base hydrolysis, were adopted to digest MQCA in the medicated chicken muscles. The amounts of MQCA in the medicated chicken were determined and compared using different hydrolysis approaches. It was shown that the highest amount of MQCA was obtained for the base hydrolysis approach. Here, the sample was hydrolyzed with 1.0 mol/L NaOH solution, defatted with -hexane, and purified with a mixed anion-exchange solid-phase extraction cartridge. The chromatographic separation was performed on a reversed-phase C column and detected using mass spectrometry in selected reaction monitoring mode. The analyte showed good linearity in the range 1.0-100 μg/L. The correlation coefficient () was greater than 0.99. The limit of detection of the proposed method was 0.4 μg/kg. At the three spiked levels of 1.0, 5.0 and 50.0 μg/kg, the average recoveries of MQCA were in range 71.7%-82.4% obtained using external standard calibration, and in range 96.3%-103.7% for internal standard calibration, with relative standard deviations below 6.0%. The proposed method is suitable for routinely monitoring of MQCA residues in animal-derived foods.

摘要

建立了一种简单、灵敏、科学且可重复的液相色谱-串联质谱法,用于测定鸡肉组织中喹乙醇标记物残留3-甲基喹喔啉-2-羧酸(MQCA)。给鸡口服喹乙醇,将其作为阳性样本。采用酶解、酸解和碱解方法对用药鸡肌肉中的MQCA进行消化。使用不同的水解方法测定并比较用药鸡中MQCA的含量。结果表明,碱解方法获得的MQCA含量最高。在此,样品用1.0 mol/L氢氧化钠溶液水解,用正己烷脱脂,并用混合阴离子交换固相萃取柱纯化。色谱分离在反相C柱上进行,并采用质谱选择反应监测模式进行检测。分析物在1.0 - 100 μg/L范围内呈良好线性。相关系数()大于0.99。所提方法的检测限为0.4 μg/kg。在1.0、5.0和50.0 μg/kg三个加标水平下,采用外标校准法时,MQCA的平均回收率在71.7% - 82.4%范围内,采用内标校准法时,平均回收率在96.3% - 103.7%范围内,相对标准偏差低于6.0%。所提方法适用于动物源性食品中MQCA残留的常规监测。

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