高效液相色谱法测定微囊藻毒素-LR的方法改进  

Improvement on Microcystin-LR Detection by High Performance Liquid Chromatography

作　　者：张明[1] 李伟英[1,2] 刘颖[1] 傅荣杰[3] 董秉直[1] 

机构地区：[1]同济大学环境科学与工程学院,上海200092 [2]同济大学环境科学与工程学院长江水环境教育部重点实验室,上海200092 [3]安捷伦科技有限公司上海分公司,上海200001

出　　处：《中国给水排水》2008年第22期78-81,共4页China Water & Wastewater

基　　金：国家"十一五"科技支撑计划重点项目(2006BAJ08B02);崇明研发基地水环境研究实验室建设专项(06dz22109)

摘　　要：对国标（GB／T20466-2006）高效液相色谱（HPLC）法检测水中微囊藻毒素-LR（MC-LR）的方法进行了改进，改进如下：C18柱活化前分别用CH2Cl2和CO（CH3）2清洗固相萃取抽吸管路和C18柱填料；样品富集流速取3～5mL／min；洗脱液（CH3OH）用量取3mL；洗脱液流速≤1 mL／min。通过对固相萃取（SPE）操作步骤和色谱条件进行改进，可使高效液相色谱法对MC-LR的最低检测限达10ng／L，固相萃取对不同浓度MC-LR样品的回收率均高于95％，重现性试验标准偏差〈0．02ng／L。The method of detecting MC-LR by HPLC in the national standard （ GB/T 20466 - 2006） was improved. The improvement is as follows： washing the collection tube and C18 cartridge by CH2Cl2 and CO（ CH3 ）2 before pre-wetting the disk respectively; the velocity of sample enrichment is between 3 mL/min and 5 mL/min; the eluent volume is 3 mL CH3OH; the velocity of eluent is controlled at less than 1 mL/min. After the improvement of operation procedures of SPE and chromatogram conditions, the LOD of the method can reach 10 ng/L, the SPE recoveries for different concentrations of MC- LR are more than 95 %, and the standard deviation of the repeated test is less than 0.02 ng/L.

关 键 词：饮用水 微囊藻毒素 检测 

分 类 号：TU991.2[建筑科学—市政工程]