含钒(III)的格里斯试剂用于柱后衍生化及同时测定婴儿食品中的亚硝酸盐和硝酸盐。
Use of Griess reagent containing vanadium(III) for post-column derivatization and simultaneous determination of nitrite and nitrate in baby food.
作者信息
Casanova John A, Gross Lois K, McMullen Sarah E, Schenck Frank J
机构信息
U.S. Food and Drug Administration, Southeast Regional Laboratory, 60 Eighth St NE, Atlanta, GA 30309, USA.
出版信息
J AOAC Int. 2006 Mar-Apr;89(2):447-51.
An ion chromatographic method with post-column derivatization and spectrophotometric detection is presented for the determination of nitrate and nitrite (NOx) in baby food. NOx residues found naturally or added as preservatives were extracted from baby foods and determined by using ion chromatography with post-column derivatization and spectrophotometric detection. Nitrate was reduced to nitrite online by post-column reduction using vanadium(lll) chloride and heat. Nitrite reacted with Griess reagent to produce a dye that was detected at 525 nm. The use of V(III) and heat to promote the reduction of nitrate to nitrite online is a novel feature of this detection system. The determination of incurred NOx residues in samples by using AOAC Method 993.03 yielded results comparable to those obtained by ion chromatography with spectrophotometric detection. The toxic and carcinogenic metal cadmium used in the AOAC Method to reduce the nitrate to nitrite was avoided. The proposed method provides simultaneous determination of nitrate and nitrite. Average recoveries of nitrate and nitrite residues ranged from 82 to 107% for fortification levels of 25-400 ppm.
本文介绍了一种采用柱后衍生化和分光光度检测的离子色谱法，用于测定婴儿食品中的硝酸盐和亚硝酸盐（NOx）。从婴儿食品中提取天然存在或作为防腐剂添加的NOx残留，并采用柱后衍生化和分光光度检测的离子色谱法进行测定。通过使用氯化钒（III）和加热进行柱后还原，将硝酸盐在线还原为亚硝酸盐。亚硝酸盐与格里斯试剂反应生成一种染料，在525nm处进行检测。使用V（III）和加热促进硝酸盐在线还原为亚硝酸盐是该检测系统的一个新特点。采用AOAC方法993.03测定样品中产生的NOx残留，其结果与采用分光光度检测的离子色谱法获得的结果相当。避免了AOAC方法中用于将硝酸盐还原为亚硝酸盐的有毒致癌金属镉。所提出的方法可同时测定硝酸盐和亚硝酸盐。对于25 - 400ppm的强化水平，硝酸盐和亚硝酸盐残留的平均回收率在82%至107%之间。
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