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液相色谱法测定鸡皮中拉沙洛西钠:实验室间研究

Liquid chromatographic determination of lasalocid sodium in chicken skin: interlaboratory study.

作者信息

Frank L R, Barnes C J

机构信息

Food and Drug Administration, Center for Veterinary Medicine, Rockville, MD 20857.

出版信息

J Assoc Off Anal Chem. 1989 Jul-Aug;72(4):584-6.

PMID:2759991
Abstract

The U.S. Food and Drug Administration (FDA) sponsored an interlaboratory study of a liquid chromatographic determinative procedure for lasalocid sodium in chicken skin with adhering fat. Four laboratories analyzed 35 dosed tissue samples and 82 fortified tissue samples containing lasalocid at levels ranging from 0.1 to 0.6 ppm. Samples were homogenized with acetonitrile, washed with hexane, and partitioned into the mobile phase prior to analysis liquid chromatography with fluorescence detection. The results of the interlaboratory study showed good reproducibility for fortified samples. Fortification levels, average recoveries, and interlaboratory percent coefficients of variation were as follows: 0.6 ppm, 0.57 ppm, and 9.7; 0.3 ppm, 0.25 ppm, and 9.1; and 0.15 ppm, 0.14 ppm, and 7.0, respectively. Data for analysis of the dosed tissue also showed good agreement among the laboratories.

摘要

美国食品药品监督管理局(FDA)发起了一项针对鸡肉皮及附着脂肪中拉沙洛西钠液相色谱测定程序的实验室间研究。四个实验室分析了35个给药组织样本和82个加标组织样本,这些样本中拉沙洛西的含量范围为0.1至0.6 ppm。样本用乙腈匀浆,用己烷洗涤,然后在进行带有荧光检测的液相色谱分析之前被分配到流动相中。实验室间研究结果表明加标样本具有良好的重现性。加标水平、平均回收率和实验室间变异系数百分比分别如下:0.6 ppm时,为0.57 ppm和9.7;0.3 ppm时,为0.25 ppm和9.1;0.15 ppm时,为0.14 ppm和7.0。给药组织的分析数据在各实验室之间也显示出良好的一致性。

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