气相色谱分析测定高级烷醇的方法研究

Capillary GC Determination of Policosanols

建立天然高级烷醇混合物含量分析的气相色谱方法。以三氯甲烷为溶剂,二十六烷烃为内标物,采用毛细管色谱柱:SE-30(30m×0.32mm,0.25μm);载气为N2,流量1.7ml/min;分流模式,分流比1:10;空气0.24MPa;氢气0.11MPa;进样口温度300℃;FID检测器,检测温度300℃;柱温为290℃恒温模式;进样量0.2μl。二十六烷醇平均回收率高达98.85%(n=5),RSD为1.02%;在8h内样品和仪器性能稳定性好。该气相色谱检测分析方法重现性好、精密度高,完全可以满足高级烷醇混合物的分析测定。

A new method was established for the determination of mixed policosanols by capillary gas chromatography （GC）. Following extraction with chloroform, chromatographic separation and quantification were achieved on an SE-30 （30 m×0.32 mm, 0.25 μm） capillary column using hexacosane as internal standard and N 2 as carry gas with a flow rate of 1.7 ml/min in shunting model with a shunting ratio of 1：10 under the following conditions： air pressure 0.24 MPa, hydrogen pressure 0.11 MPa, injection port temperature 300℃,detection temperature of FID detector 300 ℃, constant column temperature 290 ℃, and injection volume 0.2 lal. The average spiked recovery of hexacosanol was 98.85% （n = 5）, with a relative standard deviation （RSD） of 1.02%. Within 8 h, both test sample, a mixture of 4 policosanols and instrument performance showed good stability. This method has good repeatability and high precision, and therefore can be used to determinate policosanols.