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[超临界流体萃取法从生物样品中选择性萃取有机锡]

[Selective extraction of organotin from biological sample by supercritical fluid extraction].

作者信息

Ding M, Chen P, Luo G, Koizumi H, Suzuki Y

机构信息

Department of Chemistry, Tsinghua University, Beijing, 100084.

出版信息

Se Pu. 1997 Nov;15(6):527-9.

Abstract

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 CO2 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 degrees C. At lower pressure (10-15 MPa), 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 (10 MPa) and a higher temperature (50 degrees C) were used, the organotin (DPT) was extracted up to a maximum (59.9%) within 30 min, while fat was extracted only 4.9%.

摘要

由于生物样品基质中有机锡化合物的含量极低,且样品中所含的脂肪会极大地干扰有机锡的分析,因此有必要对生物样品基质中的有机锡化合物进行初步分离和浓缩。在本研究中,对用于有机锡初步分离和浓缩的超临界流体萃取(SFE)进行了研究。使用纯二氧化碳作为流动相。萃取物可用于有机锡的超临界流体色谱(SFC)分析。通过向大豆粉中添加二苯基锡(DPT)制备模型样品。研究了压力和温度对SFE的影响。少量脂肪也与有机锡一起被萃取出来。将萃取物注入SFC系统,其中使用Kapcell Pak ODS柱分离有机锡和脂肪。在40℃下研究了压力对DPT和脂肪萃取率的影响。在较低压力(10 - 15MPa)下,DPT的萃取效率达到最大值(63%),而脂肪的萃取率仅为28.3%。温度升高有利于DPT的选择性萃取。然而,随着萃取温度升高,DPT的萃取效率下降。当使用较低压力(10MPa)和较高温度(50℃)时,在30分钟内有机锡(DPT)的萃取率最高可达59.9%,而脂肪的萃取率仅为4.9%。

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