毛细管气相色谱法测定多廿醇片中5种主要成分的含量

GC determination of five main ingredients in policosanol tablets

目的:建立毛细管气相色谱法直接测定多廿醇片中5种主要成分(二十四烷醇、二十六烷醇、二十七烷醇、二十八烷醇和三十烷醇)的含量。方法:采用 Agilent 4890D 气相色谱仪,氢火焰离子检测器,DB-5HT(30 m×0.25 mm,0.1μm)毛细管色谱柱。初始温度120℃保持5 min,然后以20℃·min^(-1)速度升至270℃保持1 min,再以5℃·min^(-1)升温至310℃保持5min。用正二十烷醇作内标物定量,进样量1μL(分流比6:1)。结果:多廿醇在4.8～432.0μg·mL^(-1)考察范围内,各组分峰面积与内标峰面积的比值与其对应的浓度呈良好的线性关系,r 值均大于等于0.9996,最低检出限为3μg·mL^(-1)。方法回收率在96.8%～101.2%之间,RSD 在0.29%～3.7%。结论:本法操作简单、准确,重复性、稳定性好,结果准确可靠,是一种可行的多廿醇含量测定方法。

Objective：To establish a method for the determination of five main ingredients （tetracosanol, hexacosanol,heptacosanol, oetaeosanol and triaeontanol） in policosanol tablets by GC with capillary column. Method：The gas chromatography was Agilent 4890D with a hydrogen flame ionization detector, and the separation was performed on a DB -5HT column （30m×0.25mm,0.1μm）. The temperature program was as following：the initial column temperature was kept at 120 ℃ for 5 min, then increased to 270 ℃ at the rate of 20 ℃ ·min^ -1 and maintained for 1 min,finally the temperature to 310 ℃ at the rate of 5 ℃·min^-1 for 5 min. The cicosanol was used as an internal standard （IS）. 1 μL sample （with split ratio of 6：1 ） was injection into GC. Results：The calibration curves were yielded by the ratios of the five ingredient＇ s peak area to IS peak area according to their concentrations, respectively ; and a good linear relationship was observed from 4. 8 - 432.0 μg·mL^-1 （ r ≥0. 9996 ）, and the limit detection （LOD） was 3μg·mL^-1. The recoveries for five ingredient were 96. 80% - 101.2% , and relative standard deviations were 0.29% -3.68%. Condusion： The method is simple, accurate, reproducible and stable; it can be used as a routine method for determination of policosanol.