Takeshita R, Takabatake E, Minagawa K, Takizawa Y
J Chromatogr. 1977 Mar 21;133(2):303-10. doi: 10.1016/s0021-9673(00)83487-1.
A method was investigated in which all of the phthalate esters in biological samples were determined as phthalic acid by gas-liquid chromatography. The method is based on the separation of phthalate esters from the sample with n-hexane, saponification of the esters with an alkaline ethanolic solution to give phthalic acid, purification of the acid by extraction with diethyl ether and column chromatography using silica gel, and conversion of the acid into bis(2,2,2-trifluoroethyl) phthalate with a 2,2,2-trifluoroethanol solution containing boron trifluoride. The derivative obtained is highly sensitive to an electron-capture detector, giving a sensitivity of 0.1 pg. Biological samples fortified with di(2-ethylhexyl) phthalate at levels of 5-100 ppb were analyzed, with recoveries of 70-100%.
研究了一种通过气液色谱法将生物样品中的所有邻苯二甲酸酯测定为邻苯二甲酸的方法。该方法基于以下步骤：用正己烷从样品中分离邻苯二甲酸酯，用碱性乙醇溶液皂化酯以生成邻苯二甲酸，通过用乙醚萃取和使用硅胶的柱色谱法纯化酸，并用含三氟化硼的2,2,2-三氟乙醇溶液将酸转化为邻苯二甲酸双（2,2,2-三氟乙基）酯。所得衍生物对电子捕获检测器高度敏感，灵敏度为0.1 pg。分析了添加了浓度为5-100 ppb的邻苯二甲酸二（2-乙基己基）酯的生物样品，回收率为70-100%。
