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鲶鱼(斑点叉尾鮰)肌肉组织中磺胺二甲氧嘧啶的基质固相分散分离及液相色谱测定

Matrix solid phase dispersion isolation and liquid chromatographic determination of sulfadimethoxine in catfish (Ictalurus punctatus) muscle tissue.

作者信息

Long A R, Hsieh L C, Malbrough M S, Short C R, Barker S A

机构信息

Louisiana State University, School of Veterinary Medicine, Department of Veterinary Physiology, Pharmacology, and Toxicology, Baton Rouge 70803.

出版信息

J Assoc Off Anal Chem. 1990 Nov-Dec;73(6):868-71.

PMID:2289916
Abstract

A method for the isolation and liquid chromatographic determination of sulfadimethoxine in catfish (Ictalurus punctatus) muscle tissue is presented. Blank control and sulfadimethoxine-fortified fish muscle tissue samples (0.5 g) were blended with octadecyisilyl (C18, 40 micrograms, 18% load, endcapped) derivatized silica packing material. A column made from the C18/fish tissue blend was first washed with hexane (8 mL), following which the sulfadimethoxine was eluted with dichloromethane (8 mL). The eluant contained sulfadimethoxine analyte that was free from interfering compounds when analyzed by liquid chromatography with UV detection (photodiode array, 270 nm). Standard curves for sulfadimethoxine isolated from fortified samples were linear (0.999 +/- 0.001) with an average relative percentage recovery of 101.1 +/- 4.2% for the concentration range (50, 100, 200, 400, 800, and 1600 ng/g) examined using sulfamethoxazole as the internal standard. The interassay variability was 10.7 +/- 8.2% with an intra-assay variability of 2.2%.

摘要

本文介绍了一种从鲶鱼(斑点叉尾鮰)肌肉组织中分离磺胺二甲氧嘧啶并进行液相色谱测定的方法。将空白对照和添加了磺胺二甲氧嘧啶的鱼肌肉组织样品(0.5克)与十八烷基硅烷(C18,40微克,18%负载量,封端)衍生化硅胶填充材料混合。由C18/鱼组织混合物制成的柱子先用己烷(8毫升)冲洗,然后用二氯甲烷(8毫升)洗脱磺胺二甲氧嘧啶。当通过配有紫外检测(光电二极管阵列,270纳米)的液相色谱分析时,洗脱液中含有不含干扰化合物的磺胺二甲氧嘧啶分析物。从添加样品中分离出的磺胺二甲氧嘧啶标准曲线呈线性(0.999±0.001),以磺胺甲恶唑为内标,在所检测的浓度范围(50、100、200、400、800和1600纳克/克)内,平均相对回收率为101.1±4.2%。批间变异为10.7±8.2%,批内变异为2.2%。

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