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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2 mol/L盐酸超声提取30 min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、东莨菪碱与(-)-莨菪碱在0.1~0.5 mg/ml质量浓度范围内呈良好的线性关系,相关系数(r2)为0.998 1~0.999 5,在0.2~0.4 mg/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 To establish a method for the simultaneous determination of racemic anisodamine, scopolamine and (-) scopolamine by gas chromatography-mass spectrometry. Methods Mandala was extracted with 2 mol / L hydrochloric acid for 30 min and then filtered. The filtrate was adjusted to pH≈9 with concentrated aqueous ammonia and extracted three times with chloroform. Results There was a good linear relationship between metronidazole, scopolamine and (-) - scopolamine in the concentration range of 0.1-0.5 mg / ml. The correlation coefficient (r2) was 0.998 1-0.999 5. ml. The recoveries were 76.7% -119.0% with RSDs of 0.8% -7.3%. The detection limits were 0.1-1.0 μg / kg. Conclusion The method is simple, rapid and reliable, and can meet the detection and analysis of racimustine, scopolamine and (-) - scopolamine in Datura stramonium.