| 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 |
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| 引用本文： | 林黎,谢丽琪,欧阳姗,梁宏,叶刚,廖菁菁,庞国芳.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].分析试验室,2010,29(2). |
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| 作者姓名： | 林黎 谢丽琪 欧阳姗 梁宏 叶刚 廖菁菁 庞国芳 |
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| 作者单位： | 1. 深圳出入境检验检疫局,深圳,518067
2. 秦皇岛出入境检验检疫局,秦皇岛,066000 |
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| 基金项目： | 国家质检总局制标(20079610-T-469)项目资助 |
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| 摘 要： | 建立了牛奶和奶粉中卡巴氧代谢物喹喔啉-2-羧酸(QCA)和喹乙醇代谢物3-甲基喹喔啉-2-羧酸(MQCA)残留量的液相色谱-串联质谱测定方法。将样品经0.6%(体积分数)的甲酸溶液进行消化,用Tris缓冲溶液调节pH后,加入Protease蛋白酶进行酶解,样品溶液用0.3 mol/L HCl溶液酸化后,采用阴离子交换固相萃取柱Oasis MAX进行净化和富集。分析样品以0.1%(体积分数)的甲酸溶液-甲醇-乙腈为流动相,经Inertsil ODS-3色谱柱分离,采用负离子扫描,在LC-MS/MS多反应监测模式下进行定性及定量分析。喹口恶啉-2-羧酸和3-甲基喹口恶啉-2-羧酸的方法测定下限牛奶为0.5μg/kg,奶粉为4.0μg/kg。对牛奶在0.5~5.0μg/kg,奶粉在4.0~40.0μg/kg添加水平的平均回收率为68.2%~82.5%,RSD为3.4%~12%。
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| 关 键 词： | 液相色谱-串联质谱 卡巴氧 喹乙醇 代谢产物 牛奶 奶粉 |
Determination of the residues of metabolites of carbadox and olaquindox in milk and milk powder-LC-MS-MS method |
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| LIN Li,XIE Li-qi,OU Yang-shan,LIANG Hong,YE Gang,LIAO Jing-jing,PANG Guo-fang.Determination of the residues of metabolites of carbadox and olaquindox in milk and milk powder-LC-MS-MS method[J].Chinese Journal of Analysis Laboratory,2010,29(2). |
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| Authors: | LIN Li XIE Li-qi OU Yang-shan LIANG Hong YE Gang LIAO Jing-jing PANG Guo-fang |
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| Institution: | 1.Shenzhen Entry-Exit Inspection and Quarantine Bureau;Shenzhen 518067;2.Qinhuangdao Entry-Exit Inspection and Quarantine Bureau;Qinhuangdao 066000 |
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| Abstract: | This study presented a liquid chromatography-tandam mass spectrometry(LC-MS/MS) method for determination of residues of Carbadox,Olaquindox and related metabolites quinoxalie-2-carboxylic acid(QCA) and 3-methylquinoxaline-2-carboxylic acid(MQCA) in milk and milk powder.As for the extraction of QCA and MQCA,milk and milk powder is first digested with 0.6% formic acid to deactivate naturally-occurring enzymes.After overnight enzymatic hydrolysis with protease,the tissue extract is acidified,centrifuged and fi... |
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| Keywords: | LC-MS/MS Carbadox Olaquindox Metabolites Milk Milk powder |
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