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Simultaneous determination of ten macrolides drugs in feeds by high performance liquid chromatography with evaporation light scattering detection

机译:用高效液相色谱法同时测定饲料中饲料中的10种大类药物,蒸发光散射检测

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摘要

A sensitive and reproducible method based on high performance liquid chromatography with evaporation light scattering detection (ELSD) was developed for the simultaneous determination of 10 macrolides drugs such as azithromycin, tulathromycin, spiramycin, tilmicosin, tylosin, erythromycin, clarithromycin, roxithromycin, midecamycin and josamycin in feeds. Feed samples were extracted with a sodium borate buffer solution (pH 10.0) ethyl acetate. The dry extracts were dissolved in a phosphate buffer solution (pH 8.0), and then applied to an Oasis HLB solidphase extraction cartridge for cleanup. The residues were reconstituted in 0.5 mL of the mobile phase. By optimizing the main operational parameters of ELSD and chromatographic conditions, all target compounds were well separated on an Ecosil C-a - SH column (250 mm x 4.6 mm, 5 mm) using a gradient elution program. The calibration curves showed good linearity (r > 0.9985) in the range of 1200 mu g mL(-1) for ten analytes. The average recoveries of all analytes from five kinds of feeds spiked at three levels were between 60.2% and 112%, with intraday and inter day relative standard deviations below 11% and 15%, respectively. The limits of detection ranged from 0.4 to 0.8 mg kg(-1) for ten macrolides.
机译:开发了一种基于高效液相色谱法的敏感性和可再现的方法,用于同时测定10种大氯化萘药物,如十四霉素,坦拉霉素,斯皮霉素,蒂米康辛,替辛苷,红霉素,克拉霉素,罗西霉素,中霉素和josamycin在饲料中。用硼酸钠缓冲溶液(pH10.0)乙酸乙酯萃取进料样品。将干燥的提取物溶解在磷酸盐缓冲溶液(pH8.0)中,然后施加到Oasis HLB固相萃取盒中以进行清理。将残余物重构在0.5ml流动相中。通过优化ELSD和色谱条件的主要操作参数,使用梯度洗脱计划在EcosIL C-A-SH柱(250mm×4.6mm,5mm)上均匀地分离所有目标化合物。校准曲线显示出10个分析物的1200μg(-1)的良好线性(R> 0.9985)。在三个水平下掺入的五种饲料的所有分析物的平均回收率在60.2%和112%之间,与盘中和日间相对标准偏差分别低于11%和15%。检测限为10至0.8mg kg(-1)的10至0.8mg kg(-1)。

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  • 来源
    《RSC Advances》 |2015年第2期|共9页
  • 作者单位

    South China Agr Univ Coll Vet Med Natl Reference Lab Vet Drug Residues SCAU Guangzhou 510642 Guangdong Peoples R China;

    South China Agr Univ Coll Vet Med Natl Reference Lab Vet Drug Residues SCAU Guangzhou 510642 Guangdong Peoples R China;

    South China Agr Univ Coll Vet Med Natl Reference Lab Vet Drug Residues SCAU Guangzhou 510642 Guangdong Peoples R China;

    South China Agr Univ Coll Vet Med Natl Reference Lab Vet Drug Residues SCAU Guangzhou 510642 Guangdong Peoples R China;

    South China Agr Univ Ctr Vet Drug Residues MOA Guangzhou 510642 Guangdong Peoples R China;

    South China Agr Univ Coll Vet Med Natl Reference Lab Vet Drug Residues SCAU Guangzhou 510642 Guangdong Peoples R China;

    South China Agr Univ Coll Vet Med Natl Reference Lab Vet Drug Residues SCAU Guangzhou 510642 Guangdong Peoples R China;

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  • 正文语种 eng
  • 中图分类 化学;
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