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建立离子色谱-电感耦合等离子体质谱法测定罗硝唑处理鸡肝中无机砷。

Development of an ion chromatography-inductively coupled plasma-mass spectrometry method to determine inorganic arsenic in liver from chickens treated with roxarsone.

机构信息

Office of Regulatory Science, Center for Food Safety and Applied Nutrition, United States Food and Drug Administration, College Park, Maryland 20740, United States.

出版信息

J Agric Food Chem. 2012 Sep 19;60(37):9394-404. doi: 10.1021/jf302366a. Epub 2012 Sep 5.

DOI:10.1021/jf302366a
PMID:22897610
Abstract

Roxarsone, (4-hydroxy-3-nitrophenyl)arsonic acid, is an arsenic-containing compound that has been approved as a feed additive for poultry and swine since the 1940s; however, little information is available regarding residual arsenic species present in edible tissues. We developed a novel method for the extraction and quantification of arsenic species in chicken liver. A strongly basic solution solubilized the liver, and ultrafiltration removed macromolecules and particulate material. Ion chromatography separated the species [arsenite, arsenate, monomethylarsonic acid, dimethylarsinic acid, (4-hydroxy-3-aminophenyl)arsonic acid, (4-hydroxy-3-acetaminophenyl)arsonic acid, and roxarsone] in the extracts, which were then detected by inductively coupled plasma-mass spectrometry. The extraction oxidized most arsenite to arsenate. For fortification concentrations at 2 μg kg(-1) and above, recoveries ranged from 70 to 120%, with relative standard deviations from 7 to 34%. We detected roxarsone, its 3-amino and 3-acetamido metabolites, inorganic arsenic, and additional unknown arsenic species in livers from roxarsone-treated chickens. Both the originating laboratory and a second laboratory validated the method.

摘要

罗沙胂酸,(4-羟基-3-硝基苯)胂酸,是一种含砷化合物,自 20 世纪 40 年代以来已被批准作为家禽和猪的饲料添加剂;然而,对于可食组织中存在的残留砷形态,信息却很少。我们开发了一种从鸡肝中提取和定量砷形态的新方法。强堿溶液溶解肝脏,超滤除去大分子和颗粒物质。离子色谱将形态[亚砷酸盐、砷酸盐、一甲基胂酸、二甲基胂酸、(4-羟基-3-氨基苯)胂酸、(4-羟基-3-乙酰胺基苯)胂酸和罗沙胂酸]从提取物中分离出来,然后用电感耦合等离子体质谱法进行检测。提取过程中将大部分亚砷酸盐氧化为砷酸盐。对于添加浓度为 2μgkg(-1)及以上的情况,回收率在 70%至 120%之间,相对标准偏差在 7%至 34%之间。我们在罗沙胂酸处理过的鸡的肝脏中检测到了罗沙胂酸、它的 3-氨基和 3-乙酰胺代谢物、无机砷和其他未知的砷形态。原产实验室和第二个实验室都验证了该方法。

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