气相色谱内标法测定两种黄芪属疯草中苦马豆素含量

Determination of Swainsonine in Astragalus locoweed by internal standard gas chromatography

【目的】建立一种苦马豆素（Swainsonine,SW）的微量定量检测方法。【方法】以甲基--αD-吡喃甘露糖苷（me-Gal,纯度99%）为内标,在柱温200℃、进样口温度300℃、氢火焰离子化检测器（FID）温度280℃、高纯氮气载气压力200 kPa条件下,对苦马豆素进行气相色谱分析,以SW进样质量浓度对SW和me-Gal峰面积的比值进行回归分析,得回归方程,并进行单点校正因子测定和加样回收试验。【结果】单点校正因子为1.067 8,在0.047～6mg/mL SW进样质量浓度对SW和me-Gal峰面积比值的线性关系良好。加样平均回收率为107.33%,变异黄芪地上部分SW含量为（39.2±0.16）mg/kg,茎直黄芪地上部分SW含量为（43.6±0.13）mg/kg。【结论】气相色谱内标法准确、重现性好,可作为苦马豆素的微量定量检测方法。

[Objective] The study established a method for determination of Swainsonine. [Method] Swainsonine in Astragalus locoweed was determinated by mainternal standard gas chromatography with me-Gal as internal standard under the oven temperature 200 ℃, injection temperature 300 ℃, detector （FID） temperature 280 ℃ and flow rate of carrier gas 200 kPa. [Result] The analysis results of single-calibration-ratio was 1. 067 8 and good linear relationship was obtained in the range of 0. 047 to 6 mg/mL. The recovery percentage was 107.33%. The SW contents of A. variabilis and A. strictus were （39.2±0.16） mg/kg and （43.6±0.13） mg/kg respectively. [Conclusion] The internal standard method had high accuracy and good repertability and could be a determination method of Swainsinine.