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基质固相分散萃取法分离及液相色谱法测定强化牛肉肝中五种苯并咪唑驱虫药

Matrix solid phase dispersion isolation and liquid chromatographic determination of five benzimidazole anthelmintics in fortified beef liver.

作者信息

Long A R, Malbrough M S, Hsieh L C, 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):860-3.

PMID:2289914
Abstract

A multiresidue method for isolation and liquid chromatographic determination of 5 benzimidazole anthelmintics (thiabendazole, oxfendazole, mebendazole, albendazole, and fenbendazole) in beef liver tissue is presented. Blank or benzimidazole-fortified liver samples (0.5 g) were blended with octadecylsilyl derivatized silica packing material (C18, 18% load, endcapped, 2 g). A column made from the C18/liver matrix was first washed with hexane (8 mL), following which the benzimidazoles were eluted with acetonitrile. The acetonitrile extract was then passed through an activated alumina column. The eluate contained benzimidazole analytes that were free from interfering compounds as determined by UV detection (photodiode array, 290 nm). Correlation coefficients of standard curves for individual benzimidazoles isolated from fortified samples, using internal standardization, were linear (0.996 +/- 0.002 to 0.999 +/- 0.001) with average relative percentage recoveries from 62.0 +/- 6.7 to 86.8 +/- 8.6% for the concentration range (100-3200 ng/g) examined. The interassay variability was 7.0 +/- 4.1 to 12.9 +/- 10.2% with an intra-assay variability from 2.2 to 4.0%.

摘要

本文介绍了一种用于分离和液相色谱测定牛肉肝组织中5种苯并咪唑驱虫药(噻苯达唑、奥芬达唑、甲苯达唑、阿苯达唑和芬苯达唑)的多残留方法。将空白或添加苯并咪唑的肝样品(0.5 g)与十八烷基硅烷衍生化硅胶填充材料(C18,18%负载量,封端,2 g)混合。由C18/肝基质制成的柱先用己烷(8 mL)冲洗,然后用乙腈洗脱苯并咪唑。然后将乙腈提取物通过活性氧化铝柱。通过紫外检测(光电二极管阵列,290 nm)测定,洗脱液中含有的苯并咪唑分析物不含干扰化合物。使用内标法从加标样品中分离出的各苯并咪唑标准曲线的相关系数呈线性(0.996±0.002至0.999±0.001),在所检测的浓度范围(100 - 3200 ng/g)内,平均相对回收率为62.0±6.7%至86.8±8.6%。批间变异为7.0±4.1%至12.9±10.2%,批内变异为2.2%至4.0%。

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