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[使用偏最小二乘校准模型通过二极管阵列检测-流动注射分析同时测定食品样品中的铁、铜和钴]

[Simultaneous determination of iron, copper and cobalt in food samples by diode array detection-flow injection analysis using partial least squares calibration model].

作者信息

Mi Jian-Ping, Li Yuan-Qian, Zou Xiao-Li, Zheng Bo, Yang Jing-Guo

机构信息

Department of Sanitary Technology, West China School of Public Health, Sichuan University, Chengdu 610041, China.

出版信息

Guang Pu Xue Yu Guang Pu Fen Xi. 2007 Jun;27(6):1188-91.

Abstract

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.

摘要

建立了一种采用偏最小二乘法(PLS)算法的流动注射-电荷耦合器件-二极管阵列检测分光光度法,用于同时测定食品样品中的铁、铜和钴。该方法基于金属离子与5-溴-邻苯二胺偶氮吡啶(5-Br-PADAP)在含有30 g·L⁻¹抗坏血酸和2%(体积分数) Triton X-100的乙酸-乙酸钠缓冲溶液(pH 5)存在下的显色反应。通过电荷耦合器件二极管阵列检测器收集这些配合物的重叠光谱,并使用偏最小二乘法算法处理多波长吸光度数据。研究了流动注射分析(FIA)的反应条件和分析参数。食品样品消化后无需任何分离即可进行分析,进样速率为45次·h⁻¹。Fe²⁺、Cu⁺和Co²⁺的线性范围分别为0.2 - 10.0 μg·mL⁻¹、0.1 - 5.0 μg·mL⁻¹和0.01 - 1.0 μg·mL⁻¹,检测限分别为0.2、0.1和0.01 μg·mL⁻¹。三种元素加标样品的平均回收率为89.4% - 110.8%。样品的相对标准偏差(RSD)在1.1% - 12.1%范围内。将该方法与电感耦合等离子体发射光谱法(ICP-AES)比较,相对误差低于12.1%。总之,该方法简单、快速、灵敏、选择性好,易于应用和推广。

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