固相萃取法测定水中短链氯化石蜡

引用本文: 王迎军, 王亚韡, 江桂斌. 固相萃取法测定水中短链氯化石蜡[J]. 分析化学, 2018, 46(7): 1102-1108. doi: 10.11895/j.issn.0253-3820.181008 shu

Citation: WANG Ying-Jun, WANG Ya-Wei, JIANG Gui-Bin. Solid-phase Extraction for Analysis of Short-chain Chlorinated Paraffins in Water Samples[J]. Chinese Journal of Analytical Chemistry, 2018, 46(7): 1102-1108. doi: 10.11895/j.issn.0253-3820.181008 shu

固相萃取法测定水中短链氯化石蜡

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
基金项目:
本文系国家自然科学基金项目（Nos.21625702，21621064）和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-C₁₈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。1 μg/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

关键词:

English

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

1.
State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China;
2.
University of Chinese Academy of Sciences, Beijing 100049, China
Received Date: 03 January 2018
Revised Date: 04 April 2018
Fund Project:
This work was supported by the National Natural Science Foundation of China (Nos. 21625702, 21621064) and the State Key Development Program for Basic Research of China (No. 2015CB453100).

Abstract: 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 negative chemical ionization mass spectrometry (GC-ENCI-MS). SPE parameters including the sorbent, elution solvent and elution volume were optimized. Agilent Bond Elut-C₁₈ was precleaned with 3 mL of hexane, 3 mL of methanol and conditioned with 3 mL of H₂O before use. After enriched by the cartridge, the sample was washed by 3 mL of methanol (10%, V/V) and eluted by 3 mL of mixture of hexane and dichloromethane (1:1, V/V). The results showed that the limits of detection (LOD) of SCCPs were 18 ng/L, and the corresponding limits of quantitation of SCCPs were 60 ng/L. Recovery experiment showed that, for the water samples spiked with 1 μg/L, the recoveries were in the range of 90%-135% and the relative standard deviations were less than ±10%. Finally, the SCCPs in 20 surficial water samples collected in Beijing were analyzed using the method proposed here. The range of the concentrations of SCCPs was

Key words:

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