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微波消解-石墨炉原子吸收光谱法测定9种中兽药散剂中铅含量
潘娟
0
(上海市兽药饲料检测所)
摘要:
采用微波消解技术处理样品,用石墨炉原子吸收光谱法测定(GFAAS),对消解溶剂和微波条件进行了优化,研究了石墨炉原子吸收法的测定条件。实验表明,以HNO3 HClO4 H2O2(4 0.5 1,V V V)作为微波消解溶剂最佳,在基体改进剂Pd(NO3)2存在下,可有效地消除基体的影响,建立了微波消解—石墨炉原子吸收光谱法测定9种中兽药散剂中铅含量的方法,方法的线性范围为5.00~80.00 ng/mL(r=0.9978);检出限为0.39 ng/mL;添加回收率为87.1%~96.3%,相对标准偏差(RSD)为1.9%~6.9%(n=9),将该法应用于9种中兽药散剂中铅的测定,结果令人满意。
关键词:  石墨炉原子吸收光谱法  微波消解    中兽药散剂
DOI:
投稿时间:2010-10-22修订日期:2010-12-03
基金项目:
Determination of Lead in 9 Veterinary Chinese Materia Medica Powders by Microwave Digestion-Graphite Furnace Atomic Absorption Spectrometry
panjuan
(Shanghai Institute for Veterinary Drug & Feeds Control)
Abstract:
A method using microwave digestion technique for the determination of lead in 9 Veterinary Chinese Materia Medica Powders by the graphite furnace atomic absorption spectrometry (GFAAS) was developed. Through optimum experimental conditions, the matrix modifier used in this work was Pd(NO3)2, digestion solvents HNO3+HClO4+H2O2(4+0.5+1, V+V+V), ashing temperature 700℃, and atomization temperature 2000℃, respectively. Under the above experimental conditions, lead in 9 Veterinary Chinese Materia Medica Powders was determined. The detection limit of lead was 0.39ng/mL, the recoveries were between 87.1% and 96.3% with the relative standard deviation being between 1.9% and 6.9%, and the experimental results were satisfactory.The method was rapid and reliable, and could be applied to the determination of lead in 9 Veterinary Chinese Materia Medica Powders.
Key words:  GFAAS  microwave digestion  lead  veterinary traditional Chinese herb medicine

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