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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Eclipse XDB-C18柱,以乙腈-磷酸缓冲溶液(pH 3.0,体积比80:20)为流动相,流速1 mL·min-1,检测波长220 nm。在优化的色谱条件下,四氯愈创木酚的线性范围1~100 mg·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 RP-HPLC method was developed for the determination of trace tetrachlorophenol in papermaking effluent and its effluent soil by dichloromethane extraction and concentration. The sample to be tested is extracted with methylene chloride, concentrated by rotary evaporator, fixed with methanol and tested. High performance liquid chromatography with Eclipse XDB-C18 column with acetonitrile-phosphate buffer solution (pH 3.0, volume ratio of 80:20) as the mobile phase, flow rate of 1 mL · min-1, detection wavelength of 220 nm. Under the optimal chromatographic conditions, the linear range of TCQC was 1 ~ 100 mg · L-1, the regression equation was y = 7303x + 3064.9, R2 = 0.9997. The recoveries of spiked wastewater were 72.02% ~ 84.63% The standard deviations (SD) ranged from 0.016 to 0.036, and the coefficients of variation ranged from 1.52% to 3.42%. The method is simple, accurate, reproducible and can be used as a method for the determination of tetrachloroguanitol in papermaking wastewater and soil.