高效液相色谱测定环境水样中的硫脲与二氧化硫脲
Determination of Thiourea and Thiourea Dioxide in Environmental Water Sample by High Performance Liquid Chromatography
张媛媛 1汤宽厚 2张新宇 3刘军深 3张升晓3
作者信息
- 1. 山东省生态环境监测中心,山东 烟台 264000
- 2. 烟台市环境监控中心,山东 烟台 264003
- 3. 鲁东大学 化学与材料科学学院,山东 烟台 264039
- 折叠
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.
Abstract
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 chromato-graphic 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 thi-ourea 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 quantifi-cation are 0.03 and 0.33 mg·L-1,respectively.The recoveries of water samples spiked with thiourea and thi-ourea 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.
关键词
硫脲/二氧化硫脲/高效液相色谱法/环境水样Key words
thiourea/thiourea dioxide/high performance liquid chromatography/environmental water sample引用本文复制引用
基金项目
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)
出版年
2024
NETL
NSTL
万方数据