反相高效液相色谱法测定造纸废水及其污灌土壤中的四氯愈创木酚  

Determination of Tetrachloroguaiacol in Papermaking Wastewater and Polluted Soil by Reversed Phase High Performance Liquid Chromatography

作　　者：陈天明[1,2] 殷春涛[2,3] 丁成[2] 张雁秋[1] 

机构地区：[1]中国矿业大学环境与测绘学院,江苏徐州221116 [2]盐城工学院环境科学与工程学院,江苏盐城224051 [3]安徽理工大学地球与环境学院,安徽淮南232001

出　　处：《纸和造纸》2014年第2期68-71,共4页Paper and Paper Making

基　　金：国家自然科学基金资助项目(21277115)

摘　　要：建立以二氯甲烷萃取浓缩，测定造纸废水及其污灌土壤中痕量四氯愈创木酚含量的反相高效液相色谱法，，待测样品经二氯甲烷萃取、旋转蒸发仪浓缩后，以甲醇定容，待测。高效液相色谱采用EclipseXDB—C18柱，以乙腈-磷酸缓冲溶液（pH3．0，体积比80：20）为流动相，流速1mL·min^-1，检测波长220nm。在优化的色谱条件下，四氯愈创木酚的线性范围1～100mg·L^-1，回归方程y=7303x＋3064．9，R2=0．9997；废水溶液加标回收率72．02％～84．63％，标准偏差（SD）0．019-0．15，变异系数2-26％～12．67％；土壤中加标回收率100．74％～106．23％，标准偏差（SD）0．016-0．036，变异系数1．52％～3．42％。该方法操作简便、准确、重现性好，可作为造纸废水和土壤中的四氯愈创木酚的含量测定方法。A new method was developed and validated for analysis of tetrachloroguaiacol in papermaking wastewater and polluted soil. Tetrachloroguaiacol in the wastewater and polluted soil was extracted by methylene chloride and determined by reversed- phase high-performance （RP-HPLC）. The samples was extracted by methylene chloride, evaporated by rotary evaporator nearly dry and dissolved in methanol in constant volume for further analysis. HPLC was used to determine tetrachloroguaiacol with Eclipse XDB-C18 column, UV detector at 220 nm, and acetonitrile-phosphoric acid aqueous solution （pH=3.0） as the mobile phase. The linear equation of tetrachloroguaiacol y=7303x＋3064.9, related coefficient R2=0.9997. The recovery rate in the wastewater was 72.02%~84.63% with SD 0.016~0.036, the recovery rate in soils was 100.74%~106.23%, and SD was 0.016~0.036. The method was rapid, sensitive and easy operation, and was suitable for the determination of tetrachloroguaiacol in papermaking wastewater samples and soil.

关 键 词：四氯愈创木酚 高效液相色谱 造纸废水 土壤 

分 类 号：O657.72[理学—分析化学] X830[理学—化学]