食品科学 ›› 2011, Vol. 32 ›› Issue (22): 196-200.doi: 10.7506/spkx1002-6630-201122040

• 分析检测 • 上一篇    下一篇

石墨炉原子吸收法分析食醋中镉测定条件的响应曲面法优化

刘全德,李 超,宋 慧,唐仕荣,陈尚龙   

  1. 徐州工程学院食品工程学院
  • 出版日期:2011-11-25 发布日期:2011-11-11
  • 基金资助:
    江苏省高校自然科学基金项目(10KJD550004)

Response Surface Methodology for Optimization of Operating Conditions for Cadmium Determination in Table Vinegar by Graphite Furnace Atomic Absorption Spectrometry

LIU Quan-de,LI Chao,SONG Hui,TANG Shi-rong,CHEN Shang-long   

  1. (College of Food Engineering, Xuzhou Institute of Technology, Xuzhou 221008, China)
  • Online:2011-11-25 Published:2011-11-11

摘要: 利用响应曲面法对食醋中镉的测定条件进行优化。在单因素试验基础上,选取磷酸二氢铵质量浓度、灰化温度和原子化温度为自变量、吸光度为响应值,根据Box-Benhnken试验设计原理,采用三因素三水平响应曲面设计对吸光度进行回归分析,模拟得到二次多项式回归方程的预测模型。结果确定最佳测定条件为磷酸二氢铵质量浓度4.24mg/mL、灰化温度1013℃、原子化温度1921℃,在此条件下,测定食醋中镉的质量浓度为0.188μg/mL,与模型预测值基本相符,加标回收率为98.76%,相对标准偏差为2.68%。表明该方法可应用于实际样品测定。

关键词: 石墨炉原子吸收法, 食醋, 镉, 响应曲面法

Abstract: Response surface methodology was employed to optimize three operating conditions for cadmium determination in table vinegar by graphite furnace atomic absorption spectrometry (GFAAS). On the basis of one-factor-at-a-time experiments, absorbance at 228.8 nm of tested samples was modeled against NH4H2PO4 concentration, ashing temperature and atomization temperature using a three-variable three-level Box-Benhnken experimental design combined with multiple regression analysis. The built regression model was analyzed by response surface methodology. It was found that the optimal determination conditions were 4.24 mg/mL NH4H2PO4 concentration, ashing 1013 ℃, and atomization at 1921℃. Under these conditions, the predicted values showed a good agreement with the experimental values. Using the optimized GFAAS method, the content of cadmium in a commercial vinegar sample was determined to be 0.188 μg/mL with a spike recovery of 98.76% and a relative standard deviation of 2.68%.

Key words: graphite furnace atomic absorption spectrometry (GF-AAS), table vinegar, cadmium, response surface methodology (RSM)

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