摘要
本文旨在建立一种基于高效液相色谱法同时测定环境水样中硫脲与二氧化硫脲含量的方法。对色谱条件进行了优化,流动相为1 mL·min^(-1)的乙腈-水(体积比5∶95),二极管阵列检测器进行变波长测定,硫脲与二氧化硫脲检测波长分别为237.3与271.1 nm。采用外标法进行定量,硫脲在浓度范围为0~5.0 mg·L^(-1)、二氧化硫脲在浓度范围0~50.0 mg·L^(-1)建立了标准曲线,其线性关系良好,线性相关系数高于0.999。采用本方法对采集的地表水和自来水进行分离测定,硫脲和二氧化硫脲的检测限分别为0.01和0.1 mg·L^(-1),定量限分别为0.03和0.33 mg·L^(-1)。加标水样品中硫脲与二氧化硫脲的回收率均超过94.9%,各平行样品的RSD在0.2%~1.2%之间,表明该方法结果准确、稳定可靠,能够满足环境水样的测定需求。
This work aims to develop a method based on high performance liquid chromatography(HPLC)for determination of thiourea and thiourea dioxide simultaneously in environmental water sample.The chromatographic conditions are optimized,and mobile phase is 1 mL·min^(-1) of acetonitrile-pure water solution(5∶95,V/V).Diode array detector is used and the wave length varies with time,and the detection wave lengths of thiourea and thiourea dioxide are set at 237.3 and 271.1 nm,respectively.The external standard method is used for quantitative analysis,and the standard curves have been established for thiourea(0~5.0 mg·L^(-1))and thiourea dioxide(0~50.0 mg·L^(-1)),exhibiting good linearity with correlation coefficients over 0.999.The collected surface water and tap water samples are centrifuged,and the supernatants are injected into a HPLC system for analysis.Detection limits of thiourea and thiourea are 0.01 and 0.1 mg·L^(-1),and limits of quantification are 0.03 and 0.33 mg·L^(-1),respectively.The recoveries of water samples spiked with thiourea and thiourea dioxide are all over 94.9%with RSD ranging from 0.2%to 1.2%,indicating accuracy,stability,and reliability of the method,which will meet the requirement of environmental water analysis.
作者
张媛媛
汤宽厚
张新宇
刘军深
张升晓
ZHANG Yuanyuan;TANG Kuanhou;ZHANG Xinyu;LIU Junshen;ZHANG Shengxiao(Ecological Environment Monitoring Center of Shandong Province,Yantai 264000,China;Environmental Monitoring Center of Yantai,Yantai 264003,China;School of Chemistry and Materials Science,Ludong University,Yantai 264039,China)
出处
《鲁东大学学报（自然科学版）》
2024年第3期248-252,共5页
Journal of Ludong University:Natural Science Edition
基金
烟台市科技创新发展计划战略研究类项目(2023ZLYJ118)
烟台市科技创新发展计划校地融合项目(2022XDRH009)。
关键词
硫脲
二氧化硫脲
高效液相色谱法
环境水样
thiourea
thiourea dioxide
high performance liquid chromatography
environmental water sample
