超高效液相色谱-串联质谱法测定酸奶中的喹乙醇及其代谢物
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摘要
目的建立酸奶中的喹乙醇及其代谢物3-甲基-喹恶啉-2-羧酸(MQCA)残留量的超高效液相色谱-串联质谱测定方法。方法取混匀的酸奶样品先用乙酸乙酯-乙腈(1:1,V:V)提取,余下的蛋白质经0.3 mol/L盐酸水解后,再用乙酸乙酯-乙腈(1:1,V:V)提取,收集合并有机相后直接浓缩富集,用甲醇溶解残渣备用;分析样品以乙腈-0.05%氨水为流动相,经Inertsil ODS-3色谱柱分离,采用多反应检测正离子模式进行定性及定量分析。结果喹乙醇和3-甲基-喹恶啉-2-羧酸的定量限分别为0.2μg/kg、0.5μg/kg,酸奶中的喹乙醇在1.00μg/kg～5.00μg/kg添加水平的平均回收率为67.3%～119.4%,相对标准偏差为5.8%～9.7%;酸奶中的3-甲基-喹恶啉-2-羧酸在1.00μg/kg～3.00μg/kg添加水平的平均回收率为65.4%～113.9%,相对标准偏差为7.6%～11.6%。结论本方法操作简单、灵敏、稳定,适用于酸奶中喹乙醇及其代谢物残留的检测。
Objective To develop an ultra performance liquid chromatography-tandem mass spectrometry(LC-MS/MS) method for the determination of olaquindox residues and its related metabolite 3-methyl-quinoxaline-2-carboxylic acid(MQCA) in yoghourt. Methods The mixed yogurt sample was extracted with ethyl acetate-acetonitrile(1:1, V:V). The remaining protein was hydrolyzed with 0.3 mol/L of hydrochloric acid and extracted with ethyl acetate-acetonitrile(1:1, V:V). Organic phase was collected and concentrated directly, and methanol was used to dissolve the residue for later use; sample analysis was performed, with acetonitrile-0.05% ammonia as mobile phase, separation was conducted by Inertsil ODS-3 column, and multi-reaction detection positive ion mode was conducted for qualitative and quantitative analysis. Results The limit of quantitation(LOQ) of olaquindox and MQCA were 0.2 μg/kg and 0.5 μg/kg. At the spiked level of 1.00 μg/kg-5.00 μg/kg(Olaquindox) and 1.00 μg/kg-3.00 μg/kg(MQCA) in yoghourt, and the average recoveries were within 67.3%-119.4% and 65.4%-113.9%; and the relative standard deviation were within 5.8%-9.7% and 7.6%-11.6%. Conclusion This method is simple, sensitive and stable, and suitable for the detection of olaquindox and its related metabolite in yoghurt.
Objective To develop an ultra performance liquid chromatography-tandem mass spectrometry(LC-MS/MS) method for the determination of olaquindox residues and its related metabolite 3-methyl-quinoxaline-2-carboxylic acid(MQCA) in yoghourt. Methods The mixed yogurt sample was extracted with ethyl acetate-acetonitrile(1:1, V:V). The remaining protein was hydrolyzed with 0.3 mol/L of hydrochloric acid and extracted with ethyl acetate-acetonitrile(1:1, V:V). Organic phase was collected and concentrated directly, and methanol was used to dissolve the residue for later use; sample analysis was performed, with acetonitrile-0.05% ammonia as mobile phase, separation was conducted by Inertsil ODS-3 column, and multi-reaction detection positive ion mode was conducted for qualitative and quantitative analysis. Results The limit of quantitation(LOQ) of olaquindox and MQCA were 0.2 μg/kg and 0.5 μg/kg. At the spiked level of 1.00 μg/kg-5.00 μg/kg(Olaquindox) and 1.00 μg/kg-3.00 μg/kg(MQCA) in yoghourt, and the average recoveries were within 67.3%-119.4% and 65.4%-113.9%; and the relative standard deviation were within 5.8%-9.7% and 7.6%-11.6%. Conclusion This method is simple, sensitive and stable, and suitable for the detection of olaquindox and its related metabolite in yoghurt.
引文
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[2] 王旭, 谈自强, 黄伶利, 等. 兽用喹恶啉类遗传毒性研究进展[J]. 中国兽药杂志, 2013, 47(5): 62-65.
[3] 赵珊, 郭巧珍, 张晶, 等. 超高压液相色谱-串联质谱法测定鱼组织中卡巴氧及喹乙醇代谢物法[J].食品安全质量检测学报, 2013, 4(1): 124-128.
[4] 谢小华, 周德山, 宋向明, 等. 高效液相色谱法测定水产品中喹乙醇残留[J]. 理化检验: 化学分册, 2011, 47(1): 102-103.
[5] 姚蕴珊, 沈建忠, 吴聪明, 等. 高效液相色谱法测定猪肝组织中3甲基喹喔啉-2-羧酸[J]. 中国畜牧兽医, 2011, 38(2): 187-190.
[6] 全国水产标准化技术委员会. 农业部 1077号公告-5-2008 水产品中喹乙醇代谢物残留量的测定高效液相色谱法[S]. 北京: 中国农业出版社, 2008.
[7] 殷居易, 倪梅林, 寿成杰, 等. 鸡肉中喹乙醇、卡巴多及其代谢物的残留检测[J]. 中国兽药杂志, 2006, 40(1): 11-15.
[8] 中华人民共和国国家质量监督检验检疫总局. GB/T 22984—2008 牛奶和奶粉中卡巴氧和喹乙醇代谢物残留量的测定液相色谱-串联质谱法[S]. 北京: 中国标准出版社, 2008.
[9] 吴剑平, 张鑫, 李丹妮, 等. 在线固相萃取/液相色谱-串联质谱法检测饲料中5种喹恶啉药物残留量[J]. 分析测试学报, 2015, 34(5): 610-615.
[10] 郑玲, 吴玉杰, 赵永锋, 等. 高效液相色谱-串联质谱法测定动物源食品中喹乙醇与卡巴氧残留量[J]. 分析测试学报, 2014, 33(1): 21-26.
[11] 林黎, 谢丽琪, 欧阳姗, 等. 液相色谱-串联质谱法测定牛奶和奶粉中卡巴氧和喹乙醇代谢物的残留量[J]. 分析实验室, 2010, 29(2): 38-41.
[12] 赵东豪, 黎智广, 杨金兰, 等. 高效液相色谱-串联质谱测定水产品中残留的喹乙醇代谢物[J].分析实验室, 2010, 29(9): 19-22.
[13] 欧阳姗, 庞国芳, 谢丽琪, 等. 动物组织中卡巴氧和喹乙醇以及相关代谢产物的液相色谱-串联质谱检测方法[J]. 分析测试学报, 2008, 27(6): 590-594.
[14] 曾静, 朱宽正, 王鹏, 等. 高效液相色谱-串联质谱法测定水产品中的喹乙醇[J]. 中国食品卫生杂志, 2006, 18(5): 423-425.
[15] 徐英江, 任传博, 田秀辉, 等. 超高效液相色谱-串联质谱测定水产品中的卡巴氧、喹烯酮、乙酰甲喹及其代谢物[J]. 分析测试学报, 2011, 30(10): 1133-1137.
[2] 王旭, 谈自强, 黄伶利, 等. 兽用喹恶啉类遗传毒性研究进展[J]. 中国兽药杂志, 2013, 47(5): 62-65.
[3] 赵珊, 郭巧珍, 张晶, 等. 超高压液相色谱-串联质谱法测定鱼组织中卡巴氧及喹乙醇代谢物法[J].食品安全质量检测学报, 2013, 4(1): 124-128.
[4] 谢小华, 周德山, 宋向明, 等. 高效液相色谱法测定水产品中喹乙醇残留[J]. 理化检验: 化学分册, 2011, 47(1): 102-103.
[5] 姚蕴珊, 沈建忠, 吴聪明, 等. 高效液相色谱法测定猪肝组织中3甲基喹喔啉-2-羧酸[J]. 中国畜牧兽医, 2011, 38(2): 187-190.
[6] 全国水产标准化技术委员会. 农业部 1077号公告-5-2008 水产品中喹乙醇代谢物残留量的测定高效液相色谱法[S]. 北京: 中国农业出版社, 2008.
[7] 殷居易, 倪梅林, 寿成杰, 等. 鸡肉中喹乙醇、卡巴多及其代谢物的残留检测[J]. 中国兽药杂志, 2006, 40(1): 11-15.
[8] 中华人民共和国国家质量监督检验检疫总局. GB/T 22984—2008 牛奶和奶粉中卡巴氧和喹乙醇代谢物残留量的测定液相色谱-串联质谱法[S]. 北京: 中国标准出版社, 2008.
[9] 吴剑平, 张鑫, 李丹妮, 等. 在线固相萃取/液相色谱-串联质谱法检测饲料中5种喹恶啉药物残留量[J]. 分析测试学报, 2015, 34(5): 610-615.
[10] 郑玲, 吴玉杰, 赵永锋, 等. 高效液相色谱-串联质谱法测定动物源食品中喹乙醇与卡巴氧残留量[J]. 分析测试学报, 2014, 33(1): 21-26.
[11] 林黎, 谢丽琪, 欧阳姗, 等. 液相色谱-串联质谱法测定牛奶和奶粉中卡巴氧和喹乙醇代谢物的残留量[J]. 分析实验室, 2010, 29(2): 38-41.
[12] 赵东豪, 黎智广, 杨金兰, 等. 高效液相色谱-串联质谱测定水产品中残留的喹乙醇代谢物[J].分析实验室, 2010, 29(9): 19-22.
[13] 欧阳姗, 庞国芳, 谢丽琪, 等. 动物组织中卡巴氧和喹乙醇以及相关代谢产物的液相色谱-串联质谱检测方法[J]. 分析测试学报, 2008, 27(6): 590-594.
[14] 曾静, 朱宽正, 王鹏, 等. 高效液相色谱-串联质谱法测定水产品中的喹乙醇[J]. 中国食品卫生杂志, 2006, 18(5): 423-425.
[15] 徐英江, 任传博, 田秀辉, 等. 超高效液相色谱-串联质谱测定水产品中的卡巴氧、喹烯酮、乙酰甲喹及其代谢物[J]. 分析测试学报, 2011, 30(10): 1133-1137.