柱前衍生-高效液相色谱法检测水中王铜残留的研究
投稿时间:2017-08-02      点此下载全文 HTML
引用本文:庾金良,杜卓时,周名振,吕清科,宋宏宇,等.柱前衍生-高效液相色谱法检测水中王铜残留的研究[J].农药学学报,2017,19(6):765-770.
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作者单位E-mail
庾金良 苏州西山中科药物研究开发有限公司, 江苏 苏州 215000  
杜卓时 密苏里大学哥伦比亚分校 化学工程系, 美国 密苏里州哥伦比亚  
周名振 苏州西山中科药物研究开发有限公司, 江苏 苏州 215000  
吕清科 苏州西山中科药物研究开发有限公司, 江苏 苏州 215000  
宋宏宇 苏州西山中科药物研究开发有限公司, 江苏 苏州 215000 songhongyu@szxszk.com 
中文摘要:建立了一种柱前衍生-高效液相色谱检测水中王铜(碱式氯化铜,copper oxychloride)的方法,并应用于不同水样中王铜残留量的测定。样品在酸性条件下经二乙基二硫代氨基甲酸钠(DDTC-Na)柱前衍生,使用C18反相色谱柱,以甲醇-水为流动相等度洗脱,在305 nm波长下进行检测。结果表明:在0.06~2 mg/L范围内,王铜的质量浓度与对应的峰面积间线性关系良好,方法的检出限(LOD)为0.02 mg/L,定量限(LOQ)为0.06 mg/L;在0.06、0.2和1 mg/L添加水平下,王铜在3种水样中的平均回收率在85%~108%之间,相对标准偏差(RSD)在2.2%~14%之间,3种水样对王铜的检测均不产生干扰。该方法准确、可靠,操作简便,可应用于快速检测水中王铜的残留量。
中文关键词:柱前衍生  高效液相色谱  残留    王铜
 
Determination of copper oxychloride residue in water using high performance liquid chromatography method with pre-column derivatization
Abstract:A new method was developed for the determination of copper oxychloride residue in different water matrix using high performance liquid chromatography with pre-column derivatization. The sample was acidified and then pretreated with pre-column derivatization method using sodium diethyldithiocarbamate before injection. The chromatographic separation was performed on a C18 reversed phase column,using methanol and water as the mobile phase and quantified by UV-vis spectroscopy at the wavelength of 305 nm. The results showed that the calibration curve was linear within the range of 0.06-2 mg/L. The limit of detection (LOD) and limit of quantification (LOQ) of this method were 0.02 mg/L and 0.06 mg/L, respectively. The average recoveries in three different water matrix at three spiked concentration levels of 0.06, 0.2 and 1 mg/L ranged from 85% to 108% with the relative standard deviations (RSD) from 2.2% to 14%. The substances in all different water matrix did not appear to interfere with the determination. This method is simple, accurate and reliable, which is suitable for the rapid determination of copper oxychloride in water.
Key words:pre-column derivatization  high performance liquid chromatography  residues  water  copper oxychloride
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