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使用超临界流体萃取和高效液相色谱法测定人类粪便样本中的胆汁酸。

Determination of bile acids in human faecal samples using supercritical fluid extraction and high-performance liquid chromatography.

作者信息

Chaudhury S, Chaplin M F

机构信息

Food Research Centre, South Bank University, London, UK.

出版信息

J Chromatogr B Biomed Sci Appl. 1999 Apr 16;726(1-2):71-8. doi: 10.1016/s0378-4347(98)00585-4.

DOI:10.1016/s0378-4347(98)00585-4
PMID:10348172
Abstract

A supercritical fluid extraction (SFE) method for the extraction of bile acids from faeces is described. HPLC with pulsed amperometric detection was used to examine and confirm the recovery of bile acids. The analytes were extracted within a period of 75 min using supercritical carbon dioxide at a pressure of 34.5 MPa and a temperature of 90 degrees C. In developing this method the following parameters were investigated: temperature, pressure, and extraction time. Two alternative methods of sample preparation were also investigated with a view to reducing the overall analysis time. The method was validated for the major primary and secondary bile acids found in faeces. It was found that the overall mean +/- SD recoveries were 102.1+/-7.92%, 111.6+/-9.91%, 112.1+/-9.92% and 113.7+/-9.92% for dry samples and 108.5+/-15.77%, 110.0+/-7.22%, 115.9+/-11.11% and 106.6+/-9.16% for wet samples with respect to cholic, deoxycholic, chenodeoxycholic and lithocholic acid. The SFE is an alternative to the traditional methods available. The extraction is relatively easy to conduct and does not utilise as much glassware, solvents or time.

摘要

本文描述了一种从粪便中提取胆汁酸的超临界流体萃取(SFE)方法。采用高效液相色谱-脉冲安培检测法对胆汁酸的回收率进行检测和确认。使用超临界二氧化碳在34.5MPa压力和90℃温度下,在75分钟内完成分析物的萃取。在开发该方法时,研究了以下参数:温度、压力和萃取时间。还研究了两种样品制备的替代方法,以减少总体分析时间。该方法针对粪便中主要的初级和次级胆汁酸进行了验证。结果发现,对于干样品,相对于胆酸、脱氧胆酸、鹅去氧胆酸和石胆酸,总体平均回收率±标准差分别为102.1±7.92%、111.6±9.91%、112.1±9.92%和113.7±9.92%;对于湿样品,回收率分别为108.5±15.77%、110.0±7.22%、115.9±11.11%和106.6±9.16%。超临界流体萃取是现有传统方法的一种替代方法。该萃取操作相对容易,且不需要使用大量玻璃器皿、溶剂或时间。

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