基于混合固定相色谱柱的SPE-HPLC法检测环境水体中三嗪类除草剂  

SPE-HPLC analysis of triazine herbicides in environmental waters using mixed stationary phase

作　　者：王硕蕾[1] 王宛[2] 范中南[1] 孙宝利[1] 黄金丽[1] 董一威[1] 陕红[1] 汪群杰[1] 

机构地区：[1]中国农业科学院农业环境与可持续发展研究所,北京100081 [2]天津博纳艾杰尔科技有限公司,天津300457

出　　处：《分析试验室》2011年第7期98-102,共5页Chinese Journal of Analysis Laboratory

摘　　要：利用混合固定相色谱柱(Optim ix SCX/C8)分析了8种三嗪类化合物,在0.01 mol/L乙酸钠缓冲溶液(pH4.2)-CH3CN(75:25,V/V)等度洗脱的流动相条件下,实现了利用液相色谱方法分离同分异构体敌草净和西草净,并对比了相同色谱条件下8种目标物在C8色谱柱上的分离效果;比较了PEP和C18固相萃取柱在处理大体积水样时对目标物的吸附性能,最终选用PEP柱净化富集,建立了8种三嗪类化合物的SPE-HPLC分析方法。结果显示,8种三嗪类化合物在0.5～50 mg/L范围内线性良好,相关系数优于0.9992;在1～50μg/L范围内,方法的平均加标回收率在79.2%～103.1%之间,RSD为2.2%～7.3%;检出限(LOD)及定量限(LOQ)分别为0.08～0.24μg/L和0.2～0.8μg/L。可用于环境水样中多种三嗪类除草剂残留的检测。A method of SPE-HPLC for the separation of eight triazine herbicides is described in this paper.A pair of isomers（Desmetryn and Simetryn） which could hardly be resolved by conventional reversed-phase were originally separated with good resolution.The separation was performed on a novel mixed stationary phase Optimix SCX/C8（250 mm × 4.6 mm,i.d.5 μm） using a mixture of 0.01 mol/L sodium acetate buffer（pH 4.2）-CH3CN（75： 25,V/V） as the mobile phase.A comparison with a conventional reversed-phase column for the separation of the 8 triazines was also conducted.The method for solid phase extraction was studied for details.Two SPE cartridges were compared in adsorption performance when handling large amounts of water samples.The PEP cartridge was selected for further analysis.The proposed method was validated with respect to linearity,limits of detection and repeatabilities,and satisfactory results were obtained.The linear ranges for 8 triazines were 0.5~50 mg/L with correlation coefficients above 0.9992.In the range of 1~50 μg/L,the average recoveries in spiked water samples ranged from 79.2% to 103.1% with RSDs（%） between 2.2% and 7.3%.The LODs and LOQs of the method were 0.08~0.24 μg/L and 0.2~0.8 μg/L,respectively.The method for quality control purposes can be applied to the simultaneous determination of multi-residues of triazine herbicides in surface water as well as sauce water for drinking use.

关 键 词：固相萃取 高效液相色谱 三嗪类除草剂 混合固定相色谱柱 

分 类 号：O657.7[理学—分析化学]