摘要
本文以标准物质和自然污染样品为研究对象,对影响稻米中无机砷测定的关键影响因素进行系统研究。通过研究,揭示粒径对于稻米中无机砷测定的重要影响;通过对不同前处理方法的考察,优选出高效快速的微波辅助提取方式,并借助可精准控温的单模微波消解技术,考察温度以及微波提取升温程序对提取效率的影响,确保各砷形态之间不发生转变的前提下提高粗粒径样品无机砷的提取效率;同时,针对液相-原子荧光光谱法在常用色谱条件下砷形态分离度较差,AsV检测灵敏度较低的问题,对分离流速和流动相组成进行调整,建立微波辅助提取-液相色谱-原子荧光光谱法对稻米样品中的无机砷进行精准快速测定。该方法可实现30 min内对40目样品中的无机砷进行高效提取,10 min对无机砷的有效分离和测试,同时提高无机砷的检测灵敏度和精准性,尤其适合批量大米样品无机砷的测定。
In this paper, certified reference materials and natural pollution samples were taken as research objects to study systematically the key factors for determination of inorganic arsenic (iAs) in rice. The effect of the particle size on the determination of inorganic arsenic in rice was revealed. The microwave assisted extraction method was selected and the single mode microwave digestion technology was used to accurately study the effect of temperature and heating program on the extraction efficiency. At the same time, according to the poor separation of arsenic and the low sensitivity of AsV, the flow velocity and the composition of the flow phase were adjusted. The method of determining the inorganic arsenic in rice by microwave-assisted extraction coupled liquid chromatography-atomic fluorescence spectrometry was established. The method can achieve high efficiency extraction of inorganic arsenic in 30 min for 40 mesh samples, meanwhile, the separate and test of iAs can be accomplished in 10 min, and the sensitivity and precision of the detection of inorganic arsenic were improved. It is suitable for rapid and accurate determination of iAs in batch samples.
作者
周明慧
陈曦
张洁琼
伍燕湘
王松雪
Zhou Minghui;Chen Xi Zhang;Jieqiong;Wu Yanxiang;Wang Songxue(Academy of National Food and Strategic Reserves Administration,Beijing 100037)
出处
《中国粮油学报》
EI
CAS
CSCD
北大核心
2019年第9期112-117,共6页
Journal of the Chinese Cereals and Oils Association
基金
国家重点研发计划(2017YFC1601300)
中央级公益性科研院所基本业务费课题(ZX1703)
关键词
无机砷
大米
粒径
温度
关键影响因素
Inorganic arsenic
rice
particle size
temperature
key factors
