固相萃取法测定水中短链氯化石蜡  

Solid-phase Extraction for Analysis of Short-chain Chlorinated Paraffins in Water Samples

作　　者：王迎军 王亚韡[1,2] 江桂斌 WANG Ying-Jun;WANG Ya-Wei＊;JIANG Gui-Bin(State Key Laboratory of Environmental Chemistry and Ecotoxicology,Research Center for Eco-Environmental Sciences,Chinese Academy of Sciences,Beijing 100085,China;University of Chinese Academy of Sciences,Beijing 100049,China)

机构地区：[1]中国科学院生态环境研究中心环境化学与生态毒理国家重点实验室,北京100085 [2]中国科学院大学,北京100049

出　　处：《分析化学》2018年第7期1102-1108,共7页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(Nos.21625702;21621064);国家重点基础研究发展计划项目(No.2015CB453100)资助~~

摘　　要：建立了固相萃取法结合气相色谱-低分辨率电子捕获负化学源质谱(GC/ECNI-MS)测定水样中短链氯化石蜡(SCCPs)的方法。选取了4种不同填料的商品化固相萃取柱,对淋洗溶剂、洗脱溶剂、洗脱溶剂体积等实验参数进行了优化。经过优化的实验条件为:Agilent Bond Elut-C_(18)固相萃取柱分别用3 mL正己烷、3 mL甲醇、3 mL Milli-Q纯水预淋洗并活化,上样后,用3 mL 10%(V/V)甲醇淋洗,3 mL正己烷-二氯甲烷(1∶1,V/V)洗脱。本方法的检出限和定量限分别为18 ng/L和60 ng/L。1μg/L加标水平下回收率为90%~130%,相对标准偏差低于±10%。采用本方法对北京20个水体样品中的短链氯化石蜡水平进行了测定,浓度范围为<LOD^682 ng/L,在检测到SCCPs的18个样品中SCCPs的均值为216 ng/L。A method for short-chain chlorinated paraffins （SCCPs） analysis in water samples based on solid-phase extraction （ SPE） was developed using gas chromatography coupled with electron capture negativechemical ionization mass spectrometry （GC-ENCI-MS）. SPE parameters including the sorbent, elution solventand elution volume were optimized. Agilent Bond Elut-C18 was precleaned with 3 mL of hexane, 3 mL ofmethanol and conditioned with 3 mL of H2O before use. After enriched by the cartridge, the sample waswashed by 3 mL of methanol （10%, V / V） and eluted by 3 mL of mixture of hexane and dichloromethane（1 颐 1, V / V）. The results showed that the limits of detection （ LOD） of SCCPs were 18 ng / L, and thecorresponding limits of quantitation of SCCPs were 60 ng / L. Recovery experiment showed that, for the watersamples spiked with 1 μg / L, the recoveries were in the range of 90% - 135% and the relative standarddeviations were less than±10%. Finally, the SCCPs in 20 surficial water samples collected in Beijing wereanalyzed using the method proposed here. The range of the concentrations of SCCPs was 〈LOD to 682 ng / Lwith a mean concentration of 216 ng / L.

关 键 词：短链氯化石蜡 固相萃取 水样分析 

分 类 号：O658.2[理学—分析化学] X832[理学—化学]