液液萃取-气相色谱-质谱联用法同时测定曼陀罗中的消旋山莨菪碱、东莨菪碱与(-)-莨菪碱

Determination of raceanisodamine,scopolamine and (-)-hyoscyamine in datura by LLE-GC-MS

目的建立一种气相色谱-质谱联用法同时测定消旋山莨菪碱、东莨菪碱与（-）-莨菪碱的方法。方法曼陀罗经2mol／L盐酸超声提取30min后过滤，滤液用浓氨水调节pH≈9后用三氯甲烷提取3次，挥干定容后上机测定。结果消旋山莨菪碱、东茛菪碱与（一）一莨菪碱在0．1～0．5mg／ml质量浓度范围内呈良好的线性关系，相关系数（r^2）为0．9981～0．9995，在0．2～0．4mg／ml两个浓度水平的加标回收率为76．7％～119．0％，RSD为0．8％～7．3％，检出限为0．1～1．0μg／kg。结论本方法简单、快速、可靠，能够满足曼陀罗中消旋山莨菪碱、东莨菪碱与（-）-莨菪碱的检测分析。

Objective A method for determination of raceanisodamine, scopolamine and （-）-hyoscyamine by LLE-GC- MS was established. Methods Datura was filtered after ultrasonic extraction with 2 mol/L hydrochloric acid for 30 rain. The filtrate was extracted three times with chloroform after adjusting pH to 9 with concentrated aqueous ammonia. The extract was evaporated to dryness and diluted to constant volume before determination. Results There was a good linearity between the peak area and the concentration of raceanisodamine, scopolamine and （-） -hyoscyamine within the range of 0. 1- 0.5 mg/ml, the correlation coefficients were 0. 998 1-0. 999 5, the recoveries of spiked samples at 0.2 mg/ml and 0. 4 mg/ml to flowers and leaves of datura were ranged from 76.7% to 119.0% , RSDs were ranged from 0.8% to 7.3% , and the detection limits were ranged from 0. 1 to 1.0 μg/kg. Conclusion The method was simple, rapid and reliable. It could be applied to determine raceanisodamine, scopolamine and （-）-hyoscyamine in datura.