Kim H J, Conca K R
U.S. Army Natick Research, Development and Engineering Center, Food Engineering Directorate, Natick, MA 01760.
J Assoc Off Anal Chem. 1990 Jul-Aug;73(4):561-4.
A rapid liquid chromatographic (LC) method was developed for a sensitive determination of nitrite in cured meats, using ion-exclusion chromatographic separation and electrochemical detection (IEC-EC). The current AOAC colorimetric method requires 2 h shaking in a steam bath to eliminate interference from reducing compounds such as ascorbic acid. In the present method, nitrite was analyzed in the presence of ascorbic acid without interference, and the extraction time was reduced to 1 min. The extracted nitrite was determined by ion chromatography using anion-exclusion/HS column and amperometric detector equipped with platinum or glassy carbon electrode operating at +1.0 V vs Ag/AgCl reference electrode. The detection limit was 1 ppb as NO2-. The recoveries of 50 ppm nitrite added to frankfurter and meat stick were 103 and 99.6%, respectively, with relative standard deviations less than 4%. The high speed, sensitivity, and selectivity make the new method a useful alternative to the AOAC colorimetric method.
建立了一种快速液相色谱(LC)方法,用于灵敏测定腌肉中的亚硝酸盐,该方法采用离子排斥色谱分离和电化学检测(IEC-EC)。现行的美国官方分析化学师协会(AOAC)比色法需要在蒸汽浴中振荡2小时,以消除诸如抗坏血酸等还原性化合物的干扰。在本方法中,亚硝酸盐在抗坏血酸存在的情况下进行分析且不受干扰,萃取时间缩短至1分钟。采用阴离子排斥/高容量柱和配备铂或玻碳电极的安培检测器(相对于Ag/AgCl参比电极在+1.0 V下操作)通过离子色谱法测定萃取的亚硝酸盐。检测限为1 ppb(以NO2-计)。添加到法兰克福香肠和肉条中的50 ppm亚硝酸盐的回收率分别为103%和99.6%,相对标准偏差小于4%。该新方法的高速、灵敏和选择性使其成为AOAC比色法的一种有用替代方法。