分散固相萃取法萃取再生水中DBP与DEHP

为定量分析再生水中邻苯二甲酸二丁酯(DBP)和邻苯二甲酸二(2-乙基己基)酯(DEHP)痕量环境激素,考察了分散固相萃取(DSPE)预处理方法的萃取条件,并用于实际再生水样的预处理分析。结果表明,当萃取剂(HC-C18)用量为0.20 g、洗脱剂为6 mL乙酸乙酯、萃取时间为20 min、摇床振荡速度为200 r·min-1、萃取温度为50 ℃时,DBP与DEHP回收率分别为96.91%和101.82%。2种物质在0.50~50.00 μg·L-1范围内线性良好,相关系数(R2)分别为0.998 6和0.998 8,检出限分别是0.05和0.008 μg·L-1,加标回收率平均为96.58%和97.23%,相对标准偏差分别为3.37%~8.29%和4.91%~5.74%。该方法无需过滤水样,能够减少目标物在过滤过程中的损失,预处理时间短,且不会造成萃取小柱堵塞,适用于水质变化大、悬浮物含量高的再生水分析。采用DSPE-GC-MS方法对再生水中DBP、DEHP检测分析,方法的准确度和精密度满足痕量物质分析要求。

Extraction of DBP and DEHP in reclaimed water by dispersive-solid phase extraction

In order to make quantitative analyses of dibutyl phthalate (DBP) and di-2-ethylhexyl phthalate (DEHP) which are environmental hormones in reclaimed water, the extraction conditions in the pretreatment process of dispersive-solid phase extraction (DSPE) were investigated, and finally the pretreatment method was used for the analysis of real reclaimed water. The results showed that when the extractant (HC-C18) dosage of 0.20 g,eluent of 6 mL ethyl acetate, extraction time of 20 min, shaking speed of 200 r· min-1 and the extraction temperature of 50 ℃, the recoveries of DBP and DEHP were 96.91% and 101.82%,respectively. The calibration curves were linear in the range of 0.50 to 50.00 μg·L-1, and the correlation coefficients were 0.998 6 and 0.998 8,respectively, the detection limits were 0.05 and 0.008 μg·L-1, the recoveries of standard addition averaged at 96.58% and 97.23% and the RSDs of DBP and DEHP were 3.37% to 8.29% and 4.91% to 5.74% separately. Without the need of filtering water,this method can reduce the loss of the target compounds in the filtering process, shorten the pretreatment time, and can not cause extraction column blockage, it is suitable for the analysis of reclaimed water which has changeable water quality and high content of suspended substance. Ultimately, the accuracy and precision met the requirement of trace analysis by using DSPE-GC-MS for DBP and DEHP detection.