高压消解-石墨炉原子吸收光谱法测定八角和桂皮中镉、铅含量
Determination of Cadmium and Lead in Star Anise and Cinnamon by GF-AAS Combined with High-Pressure Digestion
摘 要
八角或桂皮样品经硝酸-过氧化氢(5+3)混合液高压密闭消解后,以20 g·L-1磷酸氢二铵作基体改进剂,采用石墨炉原子吸收光谱法测定其中镉和铅的含量.镉和铅的灰化温度分别为400 ℃,600 ℃;镉和铅的原子化温度分别为1 800 ℃,2 100 ℃.镉和铅的线性范围分别为10,50 μg·L-1以内,检出限(3s/k)分别为0.42,0.98 μg·L-1.加标回收率在96.0%~103%之间,测定值的相对标准偏差(n=6)在0.24%~1.7%之间.
八角
桂皮
镉
铅
GF-AAS
Star anise
Cinnamon
Cadmium
Lead
Abstract
Samples of star anise or cinnamon were digested with a mixture of HNO3 and H2O2(5+3) with high-pressure digestion,then cadmium and lead were measured by GFAAS with 20 g·L-1 (NH4)2HPO4 as matrix modifier. The ashing temperatures for cadmium and lead were 400 ℃ and 600 ℃,respectively;the atomization temperatures for cadmium and lead were 1 800 ℃ and 2 100 ℃,respectively. Linearity ranges for cadmium and lead were within 10 and 50 μg·L-1,respectively,with detection limits (3s/k) of 0.42,0.98 μg·L-1,respectively. Values of recovery measured by standard addition method were in the range of 96.0%-103%,with RSD′s (n=6) of 0.24%-1.7%.
中图分类号 O657.31 DOI 10.11973/lhjy-hx201506030
所属栏目 工作简报
基金项目 国家公益性行业科研专项(200810998);云南省应用基础研究计划自筹项目(2013FZ121)
收稿日期 2014/5/16
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备注冯绍平(1984-),男,云南大理人,讲师,硕士,主要从事样品中痕量重金属的分析.
引用该论文: FENG Shao-ping,LIU Wei,HUANG Zhao-long,LI Zi-jing,JIANG Yan. Determination of Cadmium and Lead in Star Anise and Cinnamon by GF-AAS Combined with High-Pressure Digestion[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(6): 855～858
冯绍平,刘卫,黄兆龙,李自静,姜艳. 高压消解-石墨炉原子吸收光谱法测定八角和桂皮中镉、铅含量[J]. 理化检验－化学分册, 2015, 51(6): 855～858
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【3】KARIMA B,NATIVIDAD R M,BADREDINE S,et al. Characterization of trace metals in vegetables by graphite furnace atomic absorption spectrometry after closed vessel microwave digestion[J]. Food Chemistry,2009,116(2):590-594．
【4】任婷,赵丽娇,曹珺,等.高分辨连续光源石墨炉原子吸收光谱法测定食品中铅、镉和铬含量[J].光谱学与光谱分析,2012,32(9):2566-2571．
【5】MICHAEL M,FIONA R,HELEN H. The determination of total germanium in real food samples including Chinese herbal remedies using graphite furnace atomic absorption spectroscopy[J]. Food Chemistry,2006,97(3):411-417．
【6】FABIANA A L,DANIELLE G,ADRIANA P O,et al. Development of a method to determine Ni and Cd in biodiesel by graphite furnace atomic absorption spectrometry[J]. Fuel,2011,90(1):142-146．
【7】魏益华,张金艳,涂田华,等.微波消解样品-电感耦合等离子体质谱法测定青菜中砷、镉、铬和铅[J].理化检验-化学分册,2011,47(11):1320-1322．
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【9】秦公伟,曹小勇,王晶,等.不同年生西洋参中铅、镉含量分析[J].食品科学,2009,30(10):182-184．
【10】梁淑轩,孙汉文.石墨炉原子吸收光谱法分析药用植物中微量营养元素的含量[J].光谱学与光谱分析,2002,22(5):847-849．
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