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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℃、8.4MPa、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、35ng/gdw(干重)。
In order to simultaneously extract and test p-nonylphenol (NP), p-nonylphenol ethoxylate (NP1EO) and p-nonylphenol diethyl ether (NP2EO) Various conditions and conditions for silylation of nonylphenols are optimized. The silanization reaction of these compounds quickly reaches the end of the reaction in a mixture of acetone and acetone-dichloromethane (acetone content ≥ 60%). The optimum extraction conditions of accelerated solvent extraction system were 120 ℃, 8.4MPa, two cycles of extraction; the best extraction solvent was dichloromethane. Compared with Soxhlet extraction and acidified suspension liquid extraction, the extraction rate, reproducibility and accuracy were significantly improved. The average recoveries were between 89.3% and 95.7% with relative standard deviations between 2.3% and 13.4%. The detection limits of nonylphenol, p-nonylphenol monoethoxy and p-nonylphenol diethoxyethanol were 10, 30 and 35ng / gdw (dry weight) respectively.