二极管阵列检测-流动注射分光光度法同时测定食品中铁铜钴

目的在于建立同时测定食品中铁、铜、钴三种微量元素的新方法。以2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚(5-Br-PADAP)为显色剂，Triton X-100为增敏剂，采用流动注射-CCD二极管阵列检测-分光光度分析法同时对其进行测定。优化了实验参数，并用偏最小二乘法计算程序解析重叠光谱。结果显示，铁、铜和钴的线性范围分别为0.2～10 μg·mL-1,0.1～5.0 μg·mL-1,0.01～1.0 μg·mL-1,检出限分别为：0.2，0.1，0.01 μg·mL-1,进样频率为45样·h-1。所建方法用于茶叶、芝麻、小米等食品测定时，样品加标回收率分别为铁89.4%～102.3%、铜92.2%～108.0%、钴93.2%～110.8%，相对标准偏差为1.1%～12.1%。对国家一级标准参考物质茶叶和桃叶进行测定(ｎ＝8)，结果在其给出的保证值范围之内。

Simultaneous Determination of Iron,Copper and Cobalt in Food Samples by Diode Array Detection-Flow Injection Analysis Using Partial Least Squares Calibration Model

A flow injection-CCD-diode array detection spectrophotometric method using partial least squares (PLS) algorithm for the simultaneous determination of iron, copper and cobalt in food samples has been established. The method was based on the chromogenic reaction between metallic ions and 5-Br-PADAP in the presence of acetic acid-acetic sodium buffer solution (pH 5) containing 30 g x L(-1) ascorbic acid and 2% (phi) Triton X-100. The overlapped spectra of these complexes were collected by CCD diode array detector and the multi-wavelength absorbance data were processed using partial least squares algorithm. The reaction conditions and analytical parameters of FIA were investigated. The food samples can be analyzed without any separation after digestion, and the sampling rate was 45 x h(-1). The linear ranges of Fe2+, Cu+ and Co2+ were 0.2-10.0 microg x mL(-1), 0.1-5.0 microg x mL(-1), and 0.01-1.0 microg x mL(-1) and the detection limits were 0.2, 0.1 and 0.01 microg x mL(-1), respectively. The average recoveries of spiked samples were 89.4%-110.8% for the three elements. The relative standard deviation (RSD) of samples was in the range of 1.1%-12.1%. Comparing the proposed method with ICP-AES, the relative error was below 12.1%. Above all, this method is simple, quick, sensitive, selective, and easy to be apply and generalize.