超声辅助提取-固相萃取净化-高效液相色谱法测定灰渣和污泥中11种双酚类及烷基酚类化合物  

Determination of 11 bisphenols and alkylphenols in ash and sludge by high performance liquid chromatography with ultrasonic assisted extraction and solid phase extraction purification

作　　者：朱佩玉 陈海秀 高晨 ZHU Peiyu;CHEN Haixiu;GAO Chen(Jiangsu Kangda Testing Technology Co.,Ltd.,Suzhou 215000,China)

机构地区：[1]江苏康达检测技术股份有限公司,江苏苏州215000

出　　处：《化学分析计量》2022年第3期41-47,共7页Chemical Analysis And Meterage

摘　　要：建立同时测定灰渣和污泥中11种双酚类及烷基酚类化合物(双酚F、双酚A、4-叔丁基苯酚、4-丁基苯酚、4-戊基苯酚、4-己基苯酚、4-叔辛基苯酚、4-庚基苯酚、壬基酚、4-辛基苯酚和4-壬基苯酚)的超声辅助提取-固相萃取净化-高效液相色谱法。以二氯甲烷-丙酮(体积比为1∶1)为提取溶剂,提取时间为20 min,提取温度为30℃,提取液经C18固相萃取柱净化后采用高效液相色谱紫外检测器进行定量分析,检测波长为225 nm。11种双酚类及烷基酚类化合物的质量浓度在0.1~2.0 mg/L范围内与色谱峰面积具有良好的线性关系,相关系数均大于0.999,方法检出限为4.3~8.4μg/kg,定量限为17.2~33.6μg/kg。低、高两种加标浓度水平时的回收率为70.6%~93.4%,测定结果的相对标准偏差为3.9%~8.3%(n=6)。该方法满足灰渣和污泥中双酚类及烷基酚类化合物的检测要求。A high performance liquid chromatography method with ultrasound assisted extraction and solid phase extraction purification was established for the simultaneous determination of 11 bisphenols and alkylphenols(bisphenol F,bisphenol A,4-t-butylphenol,4-n-butylphenol,4-n-pentylphenol,4-n-hexylphenol,4-t-octylphenol,4-n-heptylphenol,nonylphenol,4-n-octylphenol and 4-n-nonylphenol)in ash and sludge.Dichloromethane-acetone(volume ratio was 1∶1)was selected as the extraction solvent.The extraction time was 20 min,and the extraction temperature was 30℃.The extract was purified by C18 solid phase extraction column and then passed through a high performance liquid chromatography with ultraviolet detector for quantitative analysis,the detection wavelength was 225 nm.The mass concentrations of 11 bisphenols and alkylphenols had a good linear relationship with the chromatographic peak area in the range of 0.1-2.0 mg/L,the correlation coefficients were all more than 0.999,the detection limits were 4.3-8.4μg/kg,and the quantitation limits were 17.2-33.6μg/kg.The recoveries at low and high spiked concentration levels were 70.6%-93.4%,and the relative standard deviations of the determination results were 3.9%-8.3%(n=6).The method can meet the detection requirements of bisphenols and alkylphenols in ash and sludge.

关 键 词：双酚类化合物 烷基酚类化合物 超声提取 固相萃取 灰渣 污泥 

分 类 号：O657.7[理学—分析化学]