气相色谱-质谱法测定沉积物中的烷基酚和双酚A  

Determination of alkylphenols and bisphenol A in sediment by gas chromatography-mass spectrometry

作　　者：汪素芳 曹莹[1] 董淮晋 冯学良 高存富 魏占亮 WANG Sufang;CAO Ying;DONG Huaijin;FENG Xueliang;GAO Cunfu;WEI Zhanliang(The Environment Analysis and Testing Laboratory,Chinese Research Academy of Environmental Sciences,Beijing,100012,China)

机构地区：[1]中国环境科学研究院环境检测与实验中心,北京100012

出　　处：《环境化学》2024年第3期1064-1068,共5页Environmental Chemistry

基　　金：国家重点研发计划(2020YFC1807703)资助。

摘　　要：本文以内分泌干扰物烷基酚和双酚A为研究对象,使用加速溶剂萃取-硅胶柱净化-气相色谱质谱联用仪,建立了同时测定沉积物中8种痕量APs和BPA的检测方法.沉积物样品经冷冻干燥后,用丙酮-二氯甲烷(V/V=1/2)为萃取溶剂,在100℃下进行加速溶剂萃取.萃取液浓缩后使用硅胶柱净化,经气相色谱分离、质谱检测,根据保留时间、质谱碎片及其丰度定性,内标法定量.结果显示,待测物在10—2000μg·L^(-1)范围内线性关系良好,相关系数大于0.9994,检出限在0.6—1.9μg·kg^(-1)之间.目标物在200、500μg·L^(-1)标准溶液中相对标准偏差(n=7)为1.9%—5.4%,加标样品回收率为85.7%—99.5%.用本方法检测天津某河流的沉积物样品,4-丁基苯酚、4-叔辛基苯酚、4-壬基酚、双酚A被检出,实际样品中APs和BPA的加标回收率为84.5%—97.4%.实验表明,使用该方法检测沉积物中的APs和BPA,操作简便,灵敏度高,准确性和重现性良好,可满足沉积物中痕量APs和BPA的检测需要.A method was developed for the simultaneous determination of 8 trace APs and BPA in sediments by accelerated solvent extraction,silica gel column purification and gas chromatographymass spectrometry.After freeze-drying,the samples were extracted with acetone-dichloromethane(V/V=1/2)as the extraction solvent under 100℃.The extracts were purified by silica gel column,separated by gas chromatography and detected by mass spectrometry,qualitatively determined according to retention time,mass spectrum and abundance of fragments,and quantified by internal standard methods.The results showed that the target compounds showed a good linear relationship in the range of 10—2000μg·L^(-1),and the correlation coefficients were greater than 0.9994,and the limits of detections(LODs)were between 0.6 and 1.9μg·kg^(-1).The relative standard deviations(RSDs,n=7)of the compounds in 200μg·L^(-1) and 500μg·L^(-1) standard solutions were in the range of 1.9%—5.4%,and the spiked recoveries were in the range of 85.7%—99.5%.And the method was applied to the detection of sediment samples from a river in Tianjin.And 4-butylphenol,4-tertoctylphenol,4-nonylphenol and bisphenol A were detected.In addition,the spiked recoveries of APs and BPA in the actual samples were in the range of in the range of 84.5%-97.4%.The results show that this method was simple,high in sensitivity and recoveries,good in accuracy and reproducible,and could meet the requirements of trace APs and BPA detection in sediment samples.

关 键 词：气相色谱-质谱法 烷基酚类化合物 双酚A 沉积物 

分 类 号：X832[环境科学与工程—环境工程] O657.63[理学—分析化学]