CCD-二极管阵列检测流动注射分光光度法分析食品中的钼

Spectrophotometric Determination of Molybdenum in Food by CCD Diode Array Detection-FlowInjection Analysis

应用本室组装的流动注射-二极管阵列检测装置,并利用钼与2,3,7-三羟基-9-水杨基荧光酮-6(salicylflurone,SAF)-溴化十六烷基三甲胺(CTMAB)的显色反应,建立了测定钼的流动注射-CCD二极管阵列分光光度法.优化了显色反应条件和流动注射分析参数,本法在0.08～3μg/mL范围内线性良好,检出限为0.08μg/mL.样品加标回收率为84%～93%,相对标准偏差为4.1%.用该法对牛肝标准参考物质进行测定,测得值与保证值比较,两者差值在给出的不确定值范围内(t=1.687,P＞0.05).与ICP-AES比较,两法的测定结果之间无显著性差异(t=0.682,P＞0.5).采样速率为60次/h.本法简便快速,灵敏准确,食品样品硝化后,即可直接测定食品中钼的含量.

Asensitive spectrophotometric method for the determination of molybdenum(Mo)was developed us-ing flowinjection-CCD(charge coupled detector)diode array detection.It is based on the chromogenic reac-tion between metal ions and salicylflurone in the presence of cetyltrimethyl ammonium bromide(CTMAB).The reaction conditions and the analytical parameters of flowinjection analysis were studied.The correlation coefficient of the calibration curve is0.999and the linear range was from0.08to3.0μg/mL with a detec-tion limit of0.08μg/mL.The recoveries of spiked samples were84%-93%,and the RSD4.1%.The developed method was applied to the determination of molybdenum(Mo)in certified reference material of cat-tle liver.The differences between the determined and certified values were within the given uncertain value ranges(t=1.687,P>0.05).The method has also been used to determine Mo in mung bean,kelp and pork liver and the results obtained were in good agreement with those obtained by ICP-AES.The sampling rate is60samples/h -1 .