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投稿时间:2024-01-18 修订日期:2024-01-26
投稿时间:2024-01-18 修订日期:2024-01-26
中文摘要: 为践行食品检测工作“环保”的理念,本文以菠菜粉质控样品为研究对象,通过考察硝酸浓度、微波消解温度、赶酸以及其它检测条件对总汞测定的影响,建立稀酸微波消解-氢化物发生原子荧光光谱测定蔬菜中总汞的方法,并对该法进行评价,应用其对九江市售蔬菜汞含量进行测定。结果表明:最佳消解液组成为20%硝酸5 mL+过氧化氢1.0 mL,微波消解最高温度为160 ℃,载流为5% HNO3,负高压280 V,KBH4浓度0.5%。新建立的方法检出限为0.00011 mg/kg,汞在0~2.0 μg/L浓度范围线性关系良好,加标回收率为96.0%~106.0%,RSD为2.5%~5.5%。该方法操作简便,大幅度减少了前处理过程硝酸使用量,无需赶酸,精密度、重现性好,灵敏度、准确度高,推广应用前景广阔。
中文关键词: 稀酸微波消解 蔬菜 总汞 氢化物发生原子荧光光谱法
Abstract:For practicing the concept of “greening” in the food inspection, a microwave-assisted digestion method using diluted nitric acid - hydride generation atomic fluorescence spectrometry was established to determine total mercury content in vegetables. The effects of nitric acid concentration, digesting temperature, acid-driving and other conditions on the determination were investigated by taking Spinach powder as standard reference material. And then, this method was evaluated and applied to determine vegetables sold in Jiujiang. Results indicated that the optimal digestion solution consist of 5 mL of 20% nitric acid and 1.0 mL of hydrogen peroxide, and a maximum microwave digestion temperature of 160 ℃, a carrier current of 5% HNO3, a negative high voltage of 280 V, and a KBH4 concentration of 0.5% were selected. The limit of detection was 0.00011 mg/kg, the linear range of mercury was good at 0~2.0 μg/L, the correlation coefficient (R2) was 0.9997, the recovery ranged from 96.0% to 106.0%, and the relative standard deviation (RSD) was from 2.5% to 5.5%. The method is easy, can reduce the amount of nitric acid used in the pre-treatment steps significantly, free of acid driving, repeatable, and suitable for popularization and application.
keywords: microwave-assisted digestion using diluted nitric acid vegetables total mercury hydride generation atomic fluorescence spectrometry
文章编号: 中图分类号: 文献标志码:
基金项目:江西省市场监督管理局科技项目(GSJK202212); 九江市指导性科技计划(S2023ZDYFN800)
作者 | 单位 | |
张晓荣 | 永修县检验检测中心 | 753699202@qq.com |
傅志丰* | 九江市检验检测认证中心 | dsqlh112@163.com |
引用文本:
张晓荣,傅志丰.稀酸微波消解-氢化物发生原子荧光光谱法测定蔬菜中总汞[J].中国无机分析化学,2024,14(11):1485-1491.
ZHANG Xiaorong,FU Zhifeng.Determination of Total mercury in Vegetables by Hydride Generation Atomic Fluorescence Spectrometry with Diluted Nitric Acid -Microwave-assisted Digestion[J].Chinese Journal of Inorganic Analytical Chemistry,2024,14(11):1485-1491.
张晓荣,傅志丰.稀酸微波消解-氢化物发生原子荧光光谱法测定蔬菜中总汞[J].中国无机分析化学,2024,14(11):1485-1491.
ZHANG Xiaorong,FU Zhifeng.Determination of Total mercury in Vegetables by Hydride Generation Atomic Fluorescence Spectrometry with Diluted Nitric Acid -Microwave-assisted Digestion[J].Chinese Journal of Inorganic Analytical Chemistry,2024,14(11):1485-1491.