超临界流体萃取法对有机锡化合物的选择性萃取

Selective Extraction of Organotin from Biological Sample by Supercritical Fluid Extraction

研究了用超临界流体萃取法直接从脂肪基质的固体样品（大豆粉）中选择性地萃取有机锡化合物的方法。模拟试样萃取结果表明：用较低压力和较高温度的超临界态ＣＯ２作流动相时，有机锡达到最大萃取率，而脂肪类物质仅被少量萃取，从而消除了脂肪类物质对超临界流体色谱法测定有机锡的干扰。

The preliminary separation and concentration of organotin compounds from the matrix of biological samples is necessary, due to the very low content of organotin and the fat included in samples will largely interfere the analysis of organotins. In this work, supercritical fluid extraction (SFE) for the preliminary separation and concentration of organotin has been studied. Pure CO 2 was used as mobile phase. The extractives can be used to supercritical fluid chromatographic (SFC) analysis of organotins. The model sample was prepared by adding diphenyltin (DPT) to soya powder. The effects of the pressure and temperature on SFE were investigated. A small amount of fat was also extracted together with organotins. Extract was injected into SFC system, in which a Kapcell Pak ODS column was used for separation of organotin and fat. The effect of pressure on the extraction percentage of DPT and fat was investigated at 40℃. At lower pressure(1015MPa),a maximum extraction efficiency(63%)was attained for DPT, while the fat is extracted only 283%. The increase in temperature is advantageous for the selective extraction of DPT. However, the extraction efficiency of DPT decreased as the extraction temperature was increased. When a lower pressure (10MPa) and a higher temperature(50℃) were used, the organotin(DPT) was extracted up to a maximum(59.9%) within 30min, while fat was extracted only 4.9%.