在线固相萃取-高效液相色谱法测定水中的苯脲化合物  

Determination of trace level phenylurea compounds in environmental and drinking waters by high performance liquid chromatography coupled with on-line solid phase extraction

作　　者：滕曼[1] 黄雄风[2] 

机构地区：[1]中国环境监测总站国家环境保护环境监测质量控制重点实验室,北京100012 [2]复旦大学环境科学与工程系,上海200433

出　　处：《环境化学》2014年第9期1581-1586,共6页Environmental Chemistry

摘　　要：通过在线固相萃取-高效液相色谱法快速、准确测定了EPA532方法规定的水中9种痕量苯脲化合物类杀虫剂.通过双梯度高效液相色谱系统中的上样泵,采用大体积自动进样方式,将2.5 mL水样中的被测物富集在萃取柱上;而后通过阀切换将萃取柱切换至分析流路中,进行分离、测定.上样泵的流动相为纯水和甲醇,分析泵的流动相为20 mmol·L-1甲酸铵水溶液和乙腈,流速分别为1.0 mL·min-1和0.6 mL·min-1,检测波长为245 nm,整个分析时间为20 min.方法在0.5—100μg·L-1范围线性关系良好,9种杀虫剂的线性相关系数R2≥0.9927,检出限≤0.093μg·L-1,7次平行测定保留时间RSD≤0.08%,峰面积RSD≤2.57%.该方法前处理简单,快速,重现性好,可用于环境水体和饮用水中痕量杀虫剂、除草剂等污染物的测定.An on-line solid phase extraction（ SPE） system was used for the simple and sensitive determination of nine phenylurea compounds regulated in EPA method 532 in water. A dual-gradient HPLC system provided an efficient platform to fulfill the on-line SPE and separation,and the system operated under automatic control of chromatography data system software. The analytes in 2. 5 mL of water sample were trapped on a SPE cartridge using large injection mode; and then were transferred to the analytical column using valve-switching technique for determination. The mobile phase used for on-line SPE was water-methanol at 1. 0 mL·min-1flow rate,and that used for separation was20 mmol·L-1of NH4COOH-acetonitrile at 0. 6 mL·min-1flow rate; UV detection wavelength was245 nm. The complete analysis only requires 20 min. The relative standard deviation（ RSD） of nine phenylurea compounds were all less than 0. 08% for retention time,and less than 2. 57% for peak area（ n = 7）. Good linearity was obtained from 0. 5 to 100 μg·L-1with the correlation coefficients of above 0. 9927 for all the nine compounds; and the method detection limits（ MDL）were all less than 0. 093 μg·L-1for the nine phenylurea compounds.

关 键 词：苯脲化合物 在线固相萃取 双高效液相色谱系统 水分析 

分 类 号：X832[环境科学与工程—环境工程] O657.72[理学—分析化学]