色谱

色谱

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高效液相色谱法分析牛和猪肌肉组织中残留的安乃近药物的三种代谢物

沈金灿1,庞国芳2,谢丽琪1,陈沛金1,韩瑞阳1

  

  1. 1. Inspection Center of Import and Export Food, Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518067, China; 2.Qinhuangdao Entry-Exit Inspection and Quarantine Bureau, Qinhuangdao 066002, China
  • 收稿日期:2007-04-13 修回日期:2007-06-28 出版日期:2007-11-30 发布日期:1984-12-25
  • 通讯作者: 沈金灿

Analysis of Three Metabolite Residues of Dipyrone in Bovine Muscle and Pork Muscle Using High Performance Liquid Chromatography

SHEN Jincan1, PANG Guofang2, XIE Liqi1, CHEN Peijin1, HAN Ruiyang1

  

  1. 1. Inspection Center of Import and Export Food, Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518067, China; 2.Qinhuangdao Entry-Exit Inspection and Quarantine Bureau, Qinhuangdao 066002, China
  • Received:2007-04-13 Revised:2007-06-28 Online:2007-11-30 Published:1984-12-25
  • Contact: Shen Jin-Can

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摘要：

建立了牛和猪肌肉组织中残留的安乃近药物的3种代谢物 4-甲酰氨基安替比林（FAA）、4-氨基安替比林（AA）和 4-甲基氨基安替比林（MAA）的高效液相色谱测定法。肌肉组织样品均质后采用硫酸钠-亚硫酸钠溶液提取,过滤后经C18固相萃取柱净化,采用Inertsil ODS-3色谱柱分离，甲醇和水梯度洗脱，于265 nm波长下检测，外标法定量FAA,内标法定量AA和MAA（以 4-异丙基氨基安替比林作为内标物）。FAA的检出限为12.5 μg/L,AA的检出限为15.0 μg/L,MAA的检出限为20.0 μg/L;3种代谢物的测定低限均为50 μg/L;在添加水平为50～400 μg/kg范围内,FAA的回收率为81.3%~92.5%,AA的回收率为82.0%~96.0%,MAA的回收率为80.4%~90.6%,相对标准偏差均在7%以内。

关键词: 安乃近, 代谢物, 高效液相色谱法, 牛肉, 猪肉

Abstract:

A method for the determination of metabolite residues of dipyrone, 4-formylaminoantipyrine （FAA）, 4-aminoantipyrine （AA） and 4-methylaminoantipyrine （MAA） in bovine muscle and pork muscle has been developed. Homogenized muscle sample was extracted with Na2SO4-Na2SO3 solution. After filtration, the extract was cleaned-up by a C18 solid phase extraction cartridge. Prepared sample was determined using high performance liquid chromatography under the following conditions: Inertsil ODS-3 column, methanol and water as mobile phase with gradient elution, detection wavelength of 265 nm. FAA was quantified by external standard method, while AA and MAA were quantified by internal standard method using isopropylaminoantipyrine as internal standard. Limits of detection of FAA was 12.5 μg/L, while those of AA and MAA were 15.0 μg/L and 20.0 μg/L, respectively. The limit of detection of this method was 50 μg/L for all the three metabolites. The recoveries of FAA, AA and MAA were 81.3%-92.5%, 82.0%-96.0%, and 80.4%-90.6%, respectively, at the spiked levels of 50-400 μg/kg. The relative standard deviations of the method were less than 7%.

Key words: bovine muscle, dipyrone, metabolites, pork muscle , high performance liquid chromatography （HPLC）