火焰原子吸收光谱法测定牛奶中不同化学形态的钙

食品科学 ›› 2012, Vol. 33 ›› Issue (22): 278-281.

火焰原子吸收光谱法测定牛奶中不同化学形态的钙

宋慧1,2，陈尚龙1,2，李超1,2，巫永华1,2，王锋1，黄小冬1，陈华云1

1.徐州工程学院食品(生物)工程学院 2.江苏省食品资源开发与质量安全重点建设实验室

收稿日期:2012-06-18 修回日期:2012-10-19 出版日期:2012-11-25 发布日期:2012-11-20
通讯作者: 宋慧 E-mail:4506402@qq.com

Speciation Analysis of Calcium in Milk by Flame Atomic Absorption Spectrophotometry

Received:2012-06-18 Revised:2012-10-19 Online:2012-11-25 Published:2012-11-20

摘要/Abstract

摘要： 建立火焰原子吸收光谱法测定牛奶中不同化学形态钙的方法。研究乙醇体积分数、离心温度、离心力和离心时间对蛋白沉淀效果的影响，确定最佳分离条件，即乙醇体积分数50%、离心温度2℃、离心力6000×g、离心时间6min，建立沉淀剂分离牛奶中元素结合态和非结合态的方法。探讨释放剂硝酸镧的质量浓度对吸光度的影响，确定最佳质量浓度为6.00mg/mL。在此条件下，测定牛奶中总钙的质量浓度为808.6μg/mL，其中结合态钙的质量浓度为641.8μg/mL，占总钙的质量分数为79.4%；非结合态钙的质量浓度为173.0μg/mL，占总钙的质量分数为21.4%。本法的精密度(RSD)小于3.3%，仪器检出限为0.11μg/mL，加标平均回收率为97.0%，RSD为1.7%。该方法准确、稳定，具有较高的实用价值。

关键词: 火焰原子吸收分光光度法, 化学形态, 钙

Abstract: An effective method was developed for speciation analysis of calcium in milk by flame atomic absorption spectrophotometry. The effects of ethanol concentration, centrifuge temperature, centrifugal force and centrifugation time on protein sedimentation were discussed. The best conditions for separating calcium from samples were found to be protein sedimentation with 50% and centrifugation at 2 ℃ and 6000 × g for 6 min. The best La(NO3)3 concentration for releasing bound calcium was 6.00 mg/mL as determined by analyzing the effect on absorbance. Under the optimized conditions, the total calcium concentration of milk was determined to be 808.6 μg/mL and the bound and free calcium concentrations were 641.8 μg/mL and 173.0 μg/mL, which accounted for 79.4% and 21.4% of the total calcium, respectively. The precision (RSD) of the developed method was less than 3.3%, and the limit of detection was 0.11 μg/mL. The average spike recoveries of calcium was 97.0% with a RSD of 1.7%. This method was accurate, stable and applicable.

Key words: flame atomic absorption spectrophotometry (FAAS), speciation analysis, calcium

中图分类号:

O657.31

宋?慧1,2，陈尚龙1,2，李?超1,2，巫永华1,2，王?锋1，黄小冬1，陈华云1. 火焰原子吸收光谱法测定牛奶中不同化学形态的钙[J]. 食品科学, 2012, 33(22): 278-281.

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