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建立一种亚临界流体萃取和 GC-MS 验证方法,用于海洋样品中的多氯联苯(PCBs)。

Development of a subcritical fluid extraction and GC-MS validation method for polychlorinated biphenyls (PCBs) in marine samples.

机构信息

Department of Food Science and Engineering, Ocean University of China, Qingdao, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Apr 1;923-924:37-42. doi: 10.1016/j.jchromb.2013.01.033. Epub 2013 Feb 8.

DOI:10.1016/j.jchromb.2013.01.033
PMID:23455072
Abstract

This paper describes a new procedure for extracting polychlorinated biphenyls (PCBs) from marine samples using subcritical 1,1,1,2-tetrafluoroethane (R134a). The extraction procedure was optimized at temperatures varying from 20 to 70°C and pressures ranging from 3 to 15 MPa. The volume of the co-solvent was then optimized using 1,1,1,2-tetrafluoroethane (R134a) as the subcritical phase. PCBs were characterized by GC-MS using the optimized conditions of 3 MPa, 30°C, and a co-solvent volume of 6 mL. The average yields of PCBs from subcritical fluid extraction of spiked oyster samples were measured and found to be greater than 90%, with relative standard deviations (RSD) of less than 10%. Detection limits of this method were in the range of 0.045-0.108 ng/g of dry mass. The method was compared to Soxhlet extraction and then applied for monitoring PCBs in oysters from Qingdao, Shandong, China.

摘要

本文描述了一种使用亚临界 1,1,1,2-四氟乙烷(R134a)从海洋样品中提取多氯联苯(PCBs)的新方法。在 20 至 70°C 的温度和 3 至 15 MPa 的压力范围内优化了提取程序。然后使用 1,1,1,2-四氟乙烷(R134a)作为亚临界相优化了共溶剂的体积。使用优化条件(3 MPa、30°C 和共溶剂体积为 6 mL),通过 GC-MS 对 PCBs 进行了表征。从加标牡蛎样品的亚临界流体萃取中测量了 PCBs 的平均收率,发现大于 90%,相对标准偏差(RSD)小于 10%。该方法的检测限在 0.045-0.108 ng/g 干质量范围内。该方法与索氏提取进行了比较,然后应用于监测来自中国山东青岛的牡蛎中的 PCBs。

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