搅拌棒吸附萃取-气相色谱-质谱联用测定海水中邻苯二甲酸酯

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为了测定海水中痕量邻苯二甲酸酯,构建并优化了搅拌棒吸附萃取-气相色谱-质谱联用方法.选取邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸丁基苄基酯、邻苯二甲酸二(2-乙基己基)酯和邻苯二甲酸二辛酯这6种邻苯二甲酸酯作为研究对象,优化了萃取时间和解析时间等5种因素,通过回收率和相对标准偏差等对SBSE-GC-MS方法进行验证.结果表明,最佳萃取时间为2 h,最佳甲醇添加量为10%,最佳氯化钠添加量为5%,最佳解析时间为50 min,最佳解析溶剂为甲醇∶乙腈=4∶1(体积比).6种邻苯二甲酸酯的峰面积和质量浓度线性对应关系良好,相关性系数均大于0.997,检出限在0.25~174.42 ng·L-1之间,不同质量浓度的回收率均在56.97%~124.22%之间,相对标准偏差在0.41%~14.39%之间.在建立方法的基础上,测定了胶州湾主要河流入海口的样品,结果表明所有采样点均检出邻苯二甲酸酯,邻苯二甲酸二乙酯检出率为100%,质量浓度较大的污染物为邻苯二甲酸二丁酯、邻苯二甲酸丁基苄基酯、邻苯二甲酸二(2-乙基己基)酯和邻苯二甲酸二辛酯. In order to determine the trace amount of phthalate in seawater, a stir bar adsorption-desorption-gas chromatography-mass spectrometry (GC-MS) method was established and optimized.Drythyl phthalate, diethyl phthalate, Dibutyl formate, butyl benzyl phthalate, di (2-ethylhexyl) phthalate and dioctyl phthalate were selected as the research objects to optimize The extraction time and the analysis time were used to verify the SBSE-GC-MS method through the recovery rate and relative standard deviation.The results showed that the best extraction time was 2 h and the best methanol addition was 10% The optimum amount of sodium chloride is 5%, the optimal time is 50 min, and the optimal solvent is methanol: acetonitrile = 4:1 (volume ratio). The peak area and mass concentration of 6 kinds of phthalates are linear The correlation coefficients were all good, the correlation coefficient was greater than 0.997, the detection limit was between 0.25 ~ 174.42 ng · L-1, the recoveries of different mass concentrations were between 56.97% ~ 124.22%, the relative standard deviations were 0.41% ~ 14.39 % On the basis of the established method, the determination of the Jiaozhou Bay main rivers into the sea samples, the results show that all sampling points were detected adjacent Phthalate, diethyl phthalate detection rate of 100%, the mass concentration of pollutants such as dibutyl phthalate, butyl benzyl phthalate, phthalic acid Di (2-ethylhexyl) phthalate and dioctyl phthalate.
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