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

doi:10.3724/SP.J.1123.2017.12023

Abstract

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 n-hexane, and purified with a mixed anion-exchange solid-phase extraction cartridge. The chromatographic separation was performed on a reversed-phase C₁₈ 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 (r²) 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.

Key words: 3-methylquinoxaline-2-carboxylicacid, base hydrolysis, liquid chromatography-tandem mass spectrometry (LC-MS/MS), medicated chicken, residue, solid-phase extraction (SPE)

CLC Number:

O658

LI Erfen, ZHANG Meiyu, MA Heqin, ZHANG Jiahui, LIU Rong, ZENG Zhenling, HE Limin. Determination of 3-methylquinoxaline-2-carboxylic acid of olaquindox marker residue in chicken muscles by liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(5): 446-451.

References

[1] Chen Z L. Veterinary Pharmacology. 2nd ed. Beijing:China Agricultural Press, 2009:278 陈杖榴. 兽医药理学. 二版. 北京:中国农业出版社, 2009:278
[2] Chen Q, Tang S S, Jin X, et al. Food Chem Toxicol, 2009, 47(2):328
[3] Ministry of Agriculture. No 168 Bulletin of the Ministry of Agriculture of the People's Republic of China.(2015-11-26)http://www.ixumu.com/download-36101.html 农业部. 中华人民共和国农业部公告第168号. (2015-11-26)http://www.ixumu.com/download-36101.html
[4] Ministry of Agriculture. No 2638 Bulletin of the Ministry of Agriculture of the People's Republic of China. (2018-01-12)http://www.moa.gov.cn/govpublic/SYJ/201801/t20180112_6134888.htm 农业部. 中华人民共和国农业部公告第2638号. (2018-01-12)http://www.moa.gov.cn/govpublic/SYJ/201801/t20180112_6134888.htm
[5] Joint FAO/WHO Expert Committee on Food Additives. Evaluation of Certain Veterinary Drug Residues in Food, WHO Technical Report Series, 1995, 851:19
[6] Sestakova I, Kopanica M. Talanta, 1988, 35(10):816
[7] Wu Y J, Yu H, Wang Y L, et al. J Chromatogr A, 2007, 1146(1):1
[8] Lü H L, Wu C M, Cheng L L, et al. Chinese Journal of Chromatography, 2012, 30(1):45 吕海鸾, 吴聪明, 程林丽, 等. 色谱, 2012, 30(1):45
[9] Zheng L, Wu Y J, Li Y, et al. Chinese Journal of Chromatography, 2012, 30(7):660 郑玲, 吴玉杰, 李湧, 等. 色谱, 2012, 30(7):660
[10] Guo X, Sun Z Z, Qi J Y, et al. Journal of China Agricultural University, 2014, 19(1):156 郭霞, 孙振中, 戚隽渊, 等. 中国农业大学学报, 2014, 19(1):156
[11] Li Y S, Liu K L, Beier R C, et al. Food Chem, 2014, 160(10):171
[12] Yi X B, Qiu L Q, Liu S Q, et al. Journal of Instrumental Analysis, 2015, 34(3):346 易锡斌, 裘立群, 刘世琦, 等. 分析测试学报, 2015, 34(3):346
[13] SN/T 0197-2014
[14] GB/T 20746-2006
[15] Zhao D H, Li Z G, Yang J L, et al. Chinese Journal of Analytical Laboratory, 2010, 29(9):19 赵东豪, 黎智广, 杨金兰, 等. 分析试验室, 2010, 29(9):19
[16] Liu Z C, Yang F, Yu K J, et al. Food Science, 2012, 33(12):210 刘正才, 杨方, 余孔捷, 等. 食品科学, 2012, 33(12):210
[17] Bei Y J, Wang Y, He F, et al. Food Science, 2013, 34(10):255 贝亦江, 王扬, 何丰, 等. 食品科学, 2013, 34(10):255
[18] Boison J O, Lee S C, Gedir R G. Anal Chim Acta, 2009, 637(1/2):128
[19] Zhang X J, Zheng B, Zhang H, et al. J Sep Sci, 2011, 34(4):469
[20] Huang L L, Xiao A G, Fan S X, et al. J AOAC Int, 2005, 88(2):472
[21] Huang L L, Wang Y L, Tao Y F, et al. J Chromatogr B, 2008, 874(1/2):7
[22] Achille C, Giorgio F, Pierangela P, et al. Anal Chem, 2008, 80:9343