固相萃取-高效液相色谱法测定水中呋喃丹  

HPLC Determination of Carbofuran in Water with Pre-enrichment by SPE

作　　者：王晓楠[1] 烟卫[1] 刘昱[1] 

机构地区：[1]国家海洋局天津海水淡化与综合利用研究所,天津300192

出　　处：《理化检验（化学分册）》2011年第4期430-432,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：中央级公益性科研院所基本科研业务费专项资金项目(K-JBYWF-2009-T203);2010年中央级公益性科研院所基本科研业务费专项资金项目(K-JBYWF 2010-G17)

摘　　要：取200mL水样,流经C_(18)固相萃取(SPE)小柱富集呋喃丹。用5.0mL四氢呋喃从SPE柱上洗脱呋喃丹,收集洗脱液,在35℃吹氩蒸干。用1.0mL甲醇溶解残渣,所得溶液供高效液相色谱分析。用Eclipse XDB C_(18)色谱柱及由甲醇-水(1+1)混合溶液作流动相进行分离,并以285nm作激发波长,320nm作发射波长对呋喃丹作荧光检测。测得呋喃丹的质量浓度在5.0×10^(-4)～5.0mg·L^(-1)范围内与相应的峰面积值呈线性关系,检出限(3S/N)为0.02μg·L^(-1)。以水样为基体加入3个浓度水平(1.0,50.0,200.0μg·L^(-1))标准溶液对方法作回收及精密度试验,测得回收率在94.0%～99.6%之间,相对标准偏差(n=7)在1.2%～4.2%之间。Two hundred mL of water sample were taken and passed through C18SPE column to enrich trace amount of carbofuran on the column.Five mL of tetrahydrofuran were used to elute carbofuran from the column, and the eluate was evaporated to dryness by Ar blowing at 35℃.The residue was taken up with 1.0 mL of methanol which was used for HPLC analysis.The Eclipse XDB C_（18）chromatographic column and the mobile phase of mixture of methanol and water（1＋1）were used for separation.Fluorescence detection atλexof 285 nm andλemof 320 nm was adopted in the determination.Linear relationship between values of peak area and mass concentration of carbofuran was obtained in the range of 5×10^-4-5.0 mg·L^-1.with detection limit（3S/N）of 0.02μg·L^-1. Recovery and precision were tested on water samples by standard addition method at 3 concentration levels of 1.0, 50.0,200.0μg·L^-1,giving results of recovery in the range of 94.0%-99.6%and RSD＇s（n=7）in the range of 1.2%-4.2%.

关 键 词：高效液相色谱法 固相萃取 荧光检测 呋喃丹 水样 

分 类 号：O652.63[理学—分析化学]