加速溶剂提取__(期刊论文)

沉积物中壬基苯酚类雌性激素化合物的加速溶剂提取方法研究

http://www.100md.com 《分析化学》 2006年第5期

加速溶剂提取,,加速溶剂提取，气相色谱质谱联用分析，壬基苯酚，内分泌干扰物质,摘要,关键词,1引言,2实验部分,3结果与讨论,Refer

     摘要

    为了同时提取和检测沉积物中的雌性激素化合物对壬基苯酚(NP)、对壬基苯酚一乙氧醚(NP1EO)和对壬基苯酚二乙氧醚(NP2EO)，对加速溶剂提取体系的各种条件和对壬基苯酚类化合物的硅烷基化反应条件等进行了优化。在丙酮和丙酮二氯甲烷混合液(丙酮含量≥60%)介质中，这些化合物的硅烷基化反应很快达到反应终点。加速溶剂提取体系的最佳提取条件是120℃、8.4 MPa、两次循环提取；最佳提取溶剂是二氯甲烷。与索氏提取和酸化悬浮液液提取比较，明显提高了提取率、重现性和准确性。平均添标回收率在89.3%~95.7%之间，相对标准偏差为2.3%~13.4%。本方法对壬基苯酚、对壬基苯酚一乙氧醚和对壬基苯酚二乙氧醚化合物的检出限分别为10、30、35 ng/g dw (干重)。

    关键词 加速溶剂提取，气相色谱质谱联用分析，壬基苯酚，内分泌干扰物质

    Accelerated Solvent Extraction of Nonylphenolic Estrogen Compounds from Sediment

    Li Donghao*1, Shim Wonjoon2, Oh Jaeryoung2, Fang Yingyu1

    (Analysis and Inspection Center, Yanbian University,Yanji 133002)

    (South Sea Institute, Korea Ocean Research and Development Institute, Korea 656834)

    Abstract In order to simultaneous extraction and determine of pnonylphenol (NP), pnonylphenol monoethoxylate (NP1EO) and pnonylphenol diethoxylate (NP2EO)from sediment samples, the accelerated solvent extraction parameters were optimized in terms of extracting temperature, extracting pressure, extracting cycle and extracting solvent. The phenolic compounds extracted were silyl derivated with bis(trimethylsilyl)trifluoroacetamide (BSTFA) in the acetone or acetonedichloromethane mixture (acetone ≥60%). The best extracting: 120℃, 8.33 MPa (1200 psi), two cycles and dichloromethane. Average extraction recovery of spiked analytes ranged from 89.3 to 95.7% with low RSD of 2.3%-13.4%. Method detection limits for the determination of NP ......

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