超声辅助提取-氢化物原子荧光光谱法测定香辛料中的铅

建立了一种操作简单、快速、高灵敏度、高提取效率的超声辅助提取-氢化物发生-原子荧光光谱法测定香辛料中铅的分析方法。考察了提取液的酸度、超声温度和时间对提取效率的影响,最终确定1.5%的硝酸为提取溶剂,超声时间和温度分别为60 min,40℃。考察了载流酸度、铁氰化钾浓度对铅测定时荧光值和线性系数的影响。实验表明铅含量在0~20μg/L范围内线性关系良好,线性相关系数大于0.999,检出限为2.6μg/kg,相对标准偏差为1.59%~3.52%,加标回收率为98.3%~108.3%,适用于香辛料中铅含量的检测。

Determination of Pb in Spices by Ultrasonic-Assisted Extraction-Hydride Atomic Fluorescence Spectrometry

A simple,rapid,sensitive and efficient method for the determination of Pb in spices by ultrasonic-assisted extraction-hydride generation-atomic fluorescence spectrometry is established.The effects of acidity of extraction solution,ultrasonic temperature and time on the extraction efficiency are investigated.Finally,1.5%nitric acid is selected as the extraction solvent,the ultrasonic time and temperature is 60 min and 40℃respectively.The effects of current-carrying acidity and potassium ferricyanide concentration on the fluorescence value and linear coefficient of Pb.The experimental results show that the linear relationship is good when the Pb content is 0~20μg/L,the linear correlation coefficient is greater than 0.999,the detection limit is 2.6μg/kg,the relative standard deviation is 1.59%~3.52%,and the recovery rate is 98.3%~108.3%,it is suitable for the detection of Pb in spices.