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使用超声提取和毛细管柱气相色谱-电子捕获检测并采用内标校准法测定沉积物中的多氯联苯。

Determination of polychlorinated biphenyls in sediments, using sonication extraction and capillary column gas chromatography-electron capture detection with internal standard calibration.

作者信息

Dunnivant F M, Elzerman A W

机构信息

Environmental Systems Engineering, Clemson University, SC 29634-0919.

出版信息

J Assoc Off Anal Chem. 1988 May-Jun;71(3):551-6.

PMID:3134332
Abstract

A sonication technique is presented for the extraction of polychlorinated biphenyls (PCBs) from sediments. In addition, a quantitation scheme is described which allows peak-specific and, in many cases, congener-specific determination of PCBs. PCBs are quantitated by capillary column gas chromatography-electron capture detection, with internal standard calibration. Results utilizing sonication extraction were compared with those obtained by Soxhlet and steam distillation extractions of 3 U.S. Environmental Protection Agency (EPA) quality control sediment samples and 3 lake sediments known to be contaminated with PCBs. Environmental lake sediments were extracted wet, with no drying prior to extraction. Recoveries by each technique varied depending on the sediment sample being extracted and degree of chlorination of PCB congeners. With proper selection of extraction solvent, the sonication technique can recover amounts of PCBs equivalent to and sometimes greater than recoveries by the Soxhlet or steam distillation techniques. A 24-h quiescent period in the extraction solvent between 2 sonications improved extraction efficiency for 2 freeze-dried sediments but did not affect results obtained for 3 environmentally contaminated sediments that were extracted without drying. Replacement of Soxhlet extraction with the sonication technique results in reduced sample preparation time, decreased volumes of solvents and sample, and substitution of common laboratory glassware in place of fragile, expensive Soxhlet glassware. Sonication extraction can also improve precision compared with Soxhlet extraction.

摘要

本文介绍了一种从沉积物中提取多氯联苯(PCBs)的超声处理技术。此外,还描述了一种定量方案,该方案能够对PCBs进行峰特异性以及在许多情况下的同系物特异性测定。PCBs通过毛细管柱气相色谱 - 电子捕获检测进行定量,并采用内标校准。将超声提取的结果与通过索氏提取法和蒸汽蒸馏法对3个美国环境保护局(EPA)质量控制沉积物样品以及3个已知被PCBs污染的湖泊沉积物进行提取所获得的结果进行了比较。对环境湖泊沉积物进行湿法提取,提取前不进行干燥处理。每种技术的回收率因所提取的沉积物样品以及PCB同系物的氯化程度而异。通过适当选择提取溶剂,超声处理技术能够回收与索氏提取法或蒸汽蒸馏法相当甚至有时更高含量的PCBs。在两次超声处理之间,在提取溶剂中静置24小时可提高对2种冻干沉积物的提取效率,但对3种未经干燥处理的受环境污染沉积物的提取结果没有影响。用超声处理技术取代索氏提取法可缩短样品制备时间,减少溶剂和样品的用量,并能用普通实验室玻璃器皿替代易碎、昂贵的索氏玻璃器皿。与索氏提取法相比,超声提取还可提高精密度。

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