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饲料中尼卡巴嗪的液相色谱测定法

Liquid chromatographic determination of nicarbazin in feeds.

作者信息

Krabel B J, Dickson D A, Zimmermann A G, Coleman M R

机构信息

Elanco Animal Health, A Division of Eli Lilly and Company, Greenfield, IN 46140-0708, USA.

出版信息

J AOAC Int. 2000 Sep-Oct;83(5):1027-38.

Abstract

A new liquid chromatographic method has been developed for determination of nicarbazin in feeds. Approximately 40 g feed is extracted with 200 mL acetonitrile-water (80 + 20, v/v). An aliquot of the extract is filtered and assayed using a reversed-phase isocratic method that measures the 4,4'-dinitrocarbanilide moiety of nicarbazin at a wavelength of 340 nm. For medicated feeds, the method uses a standard linear range of 5 to 100 microg/mL. For lower levels, a linear range of 50 to 150 ng/mL can be used. The method has a limit of detection of 250 ng/g and a limit of quantitation of 500 ng/g in a 40 g feed sample. Recovery was 99.1%, with a range of 95.2 to 101.8%. In the typical U.S. dosing range of 27 to 113.5 g/ton, the precision of the method based on one analyst, one day, and 2 weighings ranged from 2.8% (113.5 g/ton) to 4.7% (27 g/ton).

摘要

已开发出一种新的液相色谱法用于测定饲料中的尼卡巴嗪。称取约40 g饲料,用200 mL乙腈 - 水(80 + 20,v/v)萃取。取一部分萃取液过滤,采用反相等度洗脱法进行测定,该方法在340 nm波长下测定尼卡巴嗪的4,4'-二硝基卡巴酰苯胺部分。对于加药饲料,该方法的标准线性范围为5至100 μg/mL。对于较低含量,可使用50至150 ng/mL的线性范围。在40 g饲料样品中,该方法的检测限为250 ng/g,定量限为500 ng/g。回收率为99.1%,范围为95.2%至101.8%。在美国典型的添加量范围为27至113.5 g/吨时,基于一名分析人员、一天和两次称重的该方法精密度范围为2.8%(113.5 g/吨)至4.7%(27 g/吨)。

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