高效液相色谱-串联质谱法检测猪肉中3-甲基喹喔啉-2-羧酸残留

引用本文: 魏敏芝, 万建春, 张富生, 潘华. 高效液相色谱-串联质谱法检测猪肉中3-甲基喹喔啉-2-羧酸残留[J]. 色谱, 2019, 37(10): 1059-1063. doi: 10.3724/SP.J.1123.2019.04050 shu

Citation: WEI Minzhi, WAN Jianchun, ZHANG Fusheng, PAN Hua. Determination of 3-methyl-quinoxaline-2-carboxylic acid residue in pork by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2019, 37(10): 1059-1063. doi: 10.3724/SP.J.1123.2019.04050 shu

高效液相色谱-串联质谱法检测猪肉中3-甲基喹喔啉-2-羧酸残留

1.
江西省农产品质量安全检测中心, 江西南昌 330012;
2.
江西省食品检验检测研究院, 江西南昌 330001
基金项目:
江西省重点研发计划项目（20181BBF60027）.

摘要: 建立了高效液相色谱-串联质谱同时定量和确证猪肉中3-甲基喹喔啉-2-羧酸（MQCA）残留量的检测方法。试样用0.3 mol/L盐酸溶液水解提取，加入乙腈和乙酸乙酯萃取，再用0.1 mol/L氢氧化钠溶液反萃取，阴离子交换固相萃取柱净化，经Agilent Eclipse Plus C₁₈柱（50 mm×3.0 mm，1.8 μm）分离，采用液相色谱-串联质谱仪检测，基质匹配添加标准曲线定量。MQCA在1.0~50 μg/L范围内线性相关系数大于0.99，在0.5、1.0、5.0 μg/kg加标水平下其回收率为90.5%~119.6%，相对标准偏差为3.14%~4.22%。方法可用于猪肉中MQCA残留量的快速定量和确证检测。

关键词:

English

Determination of 3-methyl-quinoxaline-2-carboxylic acid residue in pork by high performance liquid chromatography-tandem mass spectrometry

1.
Test Center for Agriculture Product Quality and Safety of Jiangxi Province, Nanchang 330012, China;
2.
Jiangxi Food Inspection and Testing Research Institute, Nanchang 330001, China
Received Date: 30 April 2019
Fund Project:
Key Science and Technology Program Project of Jiangxi Province (No. 20181BBF60027).

Abstract: A method was developed for the simultaneous quantitative and confirmatory determination of 3-methylquinoxaline-2-carboxylic acid (MQCA) residues in pork by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was hydrolyzed with 0.3 mol/L hydrochloric acid solution, and MQCA was extracted by water bath oscillation. MQCA was first extracted with acetonitrile and ethyl acetate and then re-extracted from the extraction solution with 0.1 mol/L sodium hydroxide solution. Then MQCA was purified by an anion exchange solid phase extraction column. The chromatographic separation was performed using an Agilent Eclipse Plus C18 column (50 mm×3.0 mm, 1.8 μm). The quantitative analysis was performed by the matrix matching addition method. The correlation coefficient of MQCA in the range of 1.0-50 μg/L was greater than 0.99. The recovery was 90.5%-119.6% at the spiked levels of 0.5, 1.0 and 5.0 μg/kg, and the relative standard deviation was 3.14%-4.22%. The method can be used for the rapid quantitative determination of 3-methylquinoxaline-2-carboxylic acid residues in pork.

Key words:

high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)
/ triggered multi-reaction monitoring
/ confirmation
/ 3-methyl-quinoxaline-2-carboxylic acid
/ pork

1. [1] 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
2. [2] Zheng L, Wu Y J, Li Y, et al. Chinese Journal of Chromatography, 2012, 30(7):660
3. [3] Li P P, Zhang X J, Zhang J M, et al. J Chromatogr B, 2018, 1074/1075:39
4. [4] Merou A, Kaklamanos K, Theodoridis G, J Chromatogr B, 2012, 881/882:90
5. [5] Li G P, Zhao L, Zhou F, et al. Food Chem, 2016, 209:279
6. [6] Tao L, Zhu L Q, Yu H. Food Chem, 2016, 199:70
7. [7] Sin D W M, Chung L P K, Lai M M C, et al. Anal Chim Acta, 2004, 508:147
8. [8] Duan Z J, Yi J H, Fang G Z, et al. Food Chem, 2013, 139:274
9. [9] Sniegocki T, Gbylik-Sikorska M, Posyniak A, et al. J Chromatogr B, 2014, 944:25
10. [10] Li E F, Zhang M Y, Ma H Q, et al. Chinese Journal of Chromatography, 2018, 36(5):446 李二粉, 张媚玉, 马合勤, 等. 色谱, 2018, 36(5):446
11. [11] Lu 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
12. [12] Zhang J, Gao Y S, Tang M J, et al. Journal of Food Safety and Quality, 2019, 10(2):469 张静, 高玉时, 唐梦君, 等. 食品安全质量检测学报, 2019, 10(2):469
13. [13] Geng N, Lu J. Meat Research, 2017, 31(8):39 耿宁, 卢剑. 肉类研究, 2017, 31(8):39
14. [14] Li P P, Zhang X J, Yan Z Y, et al. Food Science, 2016, 37(24):257 李佩佩, 张小军, 严忠雍, 等. 食品科学, 2016, 37(24):257
15. [15] Ma X N, Zhang X Q, Zhang R Y, et al. Chinese Journal of Food Hygiene, 2018, 30(6):602 马晓年, 张秀清, 张瑞雨, 等. 中国食品卫生杂志, 2018, 30(6):602
16. [16] Zhang X J, Zheng B, Zhang H, et al. J Sep Sci, 2011, 34:469
17. [17] Yan Z X, Li T X, Lv P, et al. J Chromatogr B, 2013, 928:22

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高效液相色谱-串联质谱法检测猪肉中3-甲基喹喔啉-2-羧酸残留

English

Determination of 3-methyl-quinoxaline-2-carboxylic acid residue in pork by high performance liquid chromatography-tandem mass spectrometry

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

高效液相色谱-串联质谱法检测猪肉中3-甲基喹喔啉-2-羧酸残留

English

Determination of 3-methyl-quinoxaline-2-carboxylic acid residue in pork by high performance liquid chromatography-tandem mass spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

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