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经过连续湿消化、干灰化、与吡咯烷二硫代氨基甲酸铵共沉淀以及石墨炉原子吸收光谱法处理后食品中的总砷含量。

Total arsenic in foods after sequential wet digestion, dry ashing, coprecipitation with ammonium pyrrolidine dithiocarbamate, and graphite-furnace atomic absorption spectrometry.

作者信息

Dabeka R W, Lacroix G M

机构信息

Food Research Division, Health and Welfare Canada, Ottawa, Ontario.

出版信息

J Assoc Off Anal Chem. 1987 Sep-Oct;70(5):866-70.

PMID:3680127
Abstract

A graphite-furnace atomic absorption (GFAAS) method is described for determining total arsenic (organic and inorganic compounds) in foods. Samples ranging from 1 to 40 g (depending on moisture content) were digested with HNO3 and dry-ashed at 500 degrees C overnight after addition of MgO. After dissolution in HCl, the arsenic was reduced with iodide and ascorbic acid and precipitated with ammonium pyrrolidine dithiocarbamate (APDC) in the presence of nickel carrier. Precipitates were collected on 0.3 micron cellulose acetate filters and dissolved in 10% HNO3 containing modifier. Ba(NO3)2 was added to remove a sulfate interference resulting from decomposition of APDC. Arsenic was determined using GFAAS. Accuracy of the method was good for 7 U.S. National Bureau of Standards (NBS) Standard Reference Materials and 3 National Research Council of Canada (NRCC) round-robin samples. Recovery of arsenic(V) from foods averaged 99.2% for peak heights and 97.1% for peak areas, with relative standard deviations (RSD) of 2.2% for peak heights and 3.3% for peak areas for all NBS and NRCC materials. Detection limit of the method was ca 10 ng arsenic.

摘要

本文描述了一种石墨炉原子吸收法(GFAAS),用于测定食品中的总砷(有机和无机化合物)。称取1至40克样品(取决于水分含量),用硝酸消化,加入氧化镁后在500℃下干灰化过夜。用盐酸溶解后,用碘化物和抗坏血酸将砷还原,并在镍载体存在下用吡咯烷二硫代氨基甲酸铵(APDC)沉淀。沉淀收集在0.3微米的醋酸纤维素滤膜上,并用含基体改进剂的10%硝酸溶解。加入硝酸钡以消除因APDC分解产生的硫酸根干扰。采用GFAAS测定砷。该方法对7种美国国家标准局(NBS)标准参考物质和3种加拿大国家研究委员会(NRCC)循环样品的准确度良好。食品中砷(V)的峰高回收率平均为99.2%,峰面积回收率平均为97.1%,所有NBS和NRCC物质的峰高相对标准偏差(RSD)为2.2%,峰面积相对标准偏差为3.3%。该方法的检测限约为10纳克砷。

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