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[反相高效液相色谱法测定氯霉素残留量。在虹鳟鱼药代动力学研究中的应用及质谱法确证]

[Determination of chloramphenicol residues with reverse-phase high pressure liquid chromatography. Use in a pharmacokinetic study in rainbow trout with confirmation by mass spectrometry].

作者信息

Pochard M F, Burger G, Chevalier M, Gleizes E

机构信息

Laboratoire Central d'Hygiène Alimentaire, Ministère de l'Agriculture, Paris, France.

出版信息

J Chromatogr. 1987 Nov 13;409:315-23. doi: 10.1016/s0021-9673(01)86808-4.

DOI:10.1016/s0021-9673(01)86808-4
PMID:3693487
Abstract

A simple and rapid high-performance liquid chromatography (HPLC) method for the determination of chloramphenicol (CAP) residues in trout muscle tissue is described. After an acetonitrile-sodium chloride extraction followed by washing with hexane and purification through a Sep-Pak C18 cartridge, analysis is performed by reversed-phase HPLC on Spherisorb ODS-II (5 microgram) using water-methanol (1:1) as the mobile phase. The detection limit of the method is 5 micrograms/kg. The mean recovery from spiked muscle samples at the 10-micrograms/kg level is 56 +/- 7.4%. CAP residues are confirmed by gas chromatography-mass spectrometry at concentrations as low as 1 micrograms/kg. Residues were detected in trout muscle after oral administration during 15 days. On the tenth day after treatment, an average of CAP of less than 5 micrograms/kg was measured. No residues were detected after the twentieth day.

摘要

描述了一种用于测定鳟鱼肌肉组织中氯霉素(CAP)残留量的简单快速的高效液相色谱(HPLC)方法。采用乙腈 - 氯化钠萃取,接着用己烷洗涤,并通过Sep - Pak C18柱进行净化,然后使用水 - 甲醇(1:1)作为流动相,在Spherisorb ODS - II(5微米)柱上进行反相HPLC分析。该方法的检测限为5微克/千克。在10微克/千克添加水平下,加标肌肉样品的平均回收率为56±7.4%。通过气相色谱 - 质谱法在低至1微克/千克的浓度下确认CAP残留量。在口服给药15天期间,鳟鱼肌肉中检测到了残留量。在治疗后的第十天,测得的CAP平均含量低于5微克/千克。在第二十天后未检测到残留量。

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