摘要
建立抑制型电导离子色谱法同时分离检测植物酵素中F^(-), Cl^(-), NO_(2)^(-), Br^(-), NO_(3)^(-), SO_(4)^(2-)和PO_(4)^(3-)这7种无机阴离子含量的测定方法。酵素液经离心提取后,先后用C18固相萃取小柱和弱阳离子固相萃取小柱分离净化,以EGCⅢ氢氧化钾自动电解发生器进行梯度洗脱, IonPac AS19离子色谱柱分离,外标法定量。结果表明, 7种阴离子在0~10mg/L范围内呈良好线性关系,相关系数r≥0.999 1,检出限为0.015~0.056 mg/L,定量限为0.15~0.18 mg/L,在1, 2和5mg/L高、中、低3个梯度下各无机阴离子加标回收率分别在90.3%~96.8%, 94.6%~96.9%和97.8%~105.7%之间,各阴离子精密度(n=6, S_(RSD))分别在2.1%~5.1%, 0.7%~3.0%和1.1%~3.2%之间,整体小于5.1%。该方法结果灵敏度高、重现性好,前处理高效简便,适用于酵素中常规无机阴离子的检测。
A method for the simultaneous separation and determination of 7 kinds of inorganic anions in plant enzymes,F^(-), Cl^(-), NO_(2)^(-), Br^(-), NO_(3)^(-), SO_(4)^(2-) and PO_(4)^(3-) was established by suppressed conductance ion chromatography.Plant Jiaosu sample was separated and purified by Cis solid phase extraction column and weak cationic solid phase extraction column.Gradient elution was performed by EGCII potassium hydroxide automatic electrolytic generator,and separated by IonPac AS19 ion chromatographic column.The content of seven inorganic anions was determined by inhibition conductivity detector.The results showed that seven kinds of inorganic anions could be separated very well.The linear relationship between the seven anions was good in the range of 0-10 mg/L,and the linear correlation efficient of this method was≥0.9991.The recoveries of each inorganic anion under the 1,2 and 5 mg/L three gradients were 90.3%-96.8%,94.6%-96.9%and 97.8%-105.7%,and the precision(n=6, S_(RSD))of each inorganic anion was 2.1%-5.1%,0.7%-3.0%and 1.1%-3.2%,which was less than 5.1%.This method had the advantages of accuracy,sensitivity and high efficiency,which was suitable and reliable for the rapid determination of seven inorganic anions in plant Jiaosu.
作者
邓湘波
欧阳吉德
曹滂
贺伟
DENG Xiangbo;OUYANG Jide;CAO Pang;HE Wei(Chenzhou Center for Food and Drug Control,Chenzhou 423000)
出处
《食品工业》
CAS
2023年第9期243-246,共4页
The Food Industry
基金
湖南省自然科学基金青年项目(2019JJ50446)
湖南省市场监督管理局科技计划(2021KJJH85)。
关键词
离子色谱仪
阴离子
固相萃取
植物酵素
ion chromatography
inorganic anions
solid phase extraction purification
plant Jiaosu
