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反相高效液相色谱法测定肥鹅肝中氯霉素残留量

Determination of chloramphenicol residues by reverse phase high performance liquid chromatography in foies gras.

作者信息

Chevalier M, Pochard M F, Bel B

机构信息

Centre National d'Etudes Vétérinaires et Alimentaires, Laboratoire Central d'Hygiène Alimentaire, Ministère de l'Agriculture, Paris, France.

出版信息

Food Addit Contam. 1995 Jan-Feb;12(1):101-6. doi: 10.1080/02652039509374284.

Abstract

A reverse phase liquid chromatographic (LC) method for the determination of chloramphenicol (CAP) residues in foies gras was tested. The method was based on acetonitrile-sodium chloride extraction, sample clean-up with hexane and purification on a Sep-Pak C18 cartridge. Acceptable chromatographic separation was obtained for thawed samples with two sample clean-up steps with hexane, a purification step with acetonitrile + water (87.5 + 12.5) (v/v) before the elution of CAP residues by a mixture of acetonitrile + water (70 + 30) (v/v) with a chromatographic separation on Spherisorb ODS-2 (5 microns) column using sodium acetate buffer (pH 4.3) + acetonitrile (78 + 22) (v/v) as mobile phase. The detection limit of the method was 2.5 micrograms/kg. The mean recovery from spiked samples at the 10 micrograms/kg level was 55.7 +/- 8.7%.

摘要

测试了一种用于测定鹅肝中氯霉素(CAP)残留量的反相液相色谱(LC)方法。该方法基于乙腈 - 氯化钠萃取、用己烷净化样品以及在Sep - Pak C18柱上进行纯化。对于解冻后的样品,通过两个用己烷净化步骤以及在CAP残留量用乙腈 + 水(70 + 30)(v/v)混合物洗脱之前用乙腈 + 水(87.5 + 12.5)(v/v)进行纯化步骤,在使用醋酸钠缓冲液(pH 4.3)+ 乙腈(78 + 22)(v/v)作为流动相的Spherisorb ODS - 2(5微米)柱上进行色谱分离,获得了可接受的色谱分离效果。该方法的检测限为2.5微克/千克。在10微克/千克水平下加标样品的平均回收率为55.7 +/- 8.7%。

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