摘要
建立了测定番石榴叶中齐墩果酸和熊果酸的气相色谱-质谱(GC-MS)方法.以双(三甲硅烷)三氟乙酰胺(BSTFA)为衍生化试剂,将齐墩果酸和熊果酸制成三甲基硅烷衍生物后,在DB-5 MS毛细管柱上进行分离.柱升温程序为:柱初温100 ℃,恒温保持2 min, 以10 ℃/min的速度升温至300 ℃,保持14 min.通过与标准样品对照比较保留时间和质谱确认样品中齐墩果酸和熊果酸的色谱峰.以峰面积进行定量测定,齐墩果酸和熊果酸的线性范围分别为4.1～102 μg/mL和4.7～114 μg/mL,回收率分别为77.1%和89.4%,6次平行测定的相对标准偏差分别为3.7%和3.5%.
A gas chromatographic-mass spectrometric method for determining oleanolic and ursolic acid has been developed. Trimethylsilyl derivatives of the acids were prepared with bis（trimethylsilyl）trifluoroacetamide （BSTFA） for gas-chromatographic separation on a DB-5 MS capillary column. The temperature program comprised two phases： initially the temperature was set at 100℃ for 2 min. It was then ramped to 300 ℃ at a rate of 10℃/min and held for 14 min. oleanolic acid and ursolic acid were comfirmed by comparison of both mass spectra and GC retention time with the standards. The quantitative analysis was based on the peak area. Excellent linearity was obtained over the range 4.1-102μg/mL for oleanolic acid and 4.7-114μg/mL for ursolic acid respectively. The recovery of the spiked oleanolic and ursolic acid was 77. 1% and 89. 4% respectively with acceptable RSD.
出处
《分析测试技术与仪器》
CAS
2005年第3期178-181,共4页
Analysis and Testing Technology and Instruments
基金
广东省重大项目(A301020301)
