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建立一种用冷蒸气原子荧光光谱法测定脂肪组织中超痕量汞的方法。

Development of a method for the determination of ultra-trace level mercury in adipose tissue by cold vapour atomic fluorescence spectrometry.

作者信息

Levine K E, Fernando R A, Lang M, Essader A, Handy R W, Collins B J

机构信息

Research Triangle Institute, 3040 Cornwallis Road, P.O. Box 12194, Research Triangle Park, NC 27709-2194, USA.

出版信息

J Autom Methods Manag Chem. 2000;22(4):103-8. doi: 10.1155/S1463924600000146.

Abstract

A method for the determination of total mercury in rat adipose tissue by cold vapour atomic fluorescence spectrometry (CVAFS) has been developed. Adipose samples were initially subjected to a lyophilization procedure in order to facilitate the homogenization and accurate weighing of small tissue aliquots (approximately 50 mg). A closed vessel microwave digestion procedure using a mixture of sulphuric and nitric acids was used to liberate mercury from the adipose matrix. All mercury species were quantitatively oxidized to Hg(II) by a potassium bromate/bromide oxidation, then reduced to Hg(0) vapour by stannous chloride prior to fluorescence detection. The CVAFS exhibited a linear range of 10 pg Hg/ml to 120 pg Hg/ml. The method detection limit in solution was 2 pg Hg/ml, or 1 ng Hg/g adipose tissue, based on a nominal 50 mg sample and a final volume of 25 ml. A reference material from the National Research Council of Canada (DOLT-2, trace metals in dogfish liver) was prepared in quadruplicate in order to assess the accuracy and precision of the method. Mercury in this material was recovered at 2.22 +/- 0.08 microg/g, which is 104% of the certified level (2.14 +/- 0.10 microg/g).

摘要

已开发出一种通过冷蒸气原子荧光光谱法(CVAFS)测定大鼠脂肪组织中总汞的方法。脂肪样品首先进行冻干处理,以便于对小份组织(约50毫克)进行匀浆和精确称重。使用硫酸和硝酸的混合物进行密闭容器微波消解程序,以从脂肪基质中释放汞。所有汞物种通过溴酸钾/溴化物氧化定量氧化为Hg(II),然后在荧光检测之前用氯化亚锡还原为Hg(0)蒸气。CVAFS的线性范围为10 pg Hg/ml至120 pg Hg/ml。基于标称50毫克样品和最终体积25毫升,该方法在溶液中的检测限为2 pg Hg/ml,或1 ng Hg/g脂肪组织。为评估该方法的准确性和精密度,对加拿大国家研究委员会的一种参考物质(DOLT - 2,角鲨鱼肝中的痕量金属)进行了四次制备。该物质中的汞回收率为2.22 +/- 0.08微克/克,为认证水平(2.14 +/- 0.10微克/克)的104%。

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