HPLC-RID同时测定艾纳香叶中左旋樟脑、左旋龙脑及异龙脑含量

Simultaneous determination of camphor, borneol, and isoborneol in Blumea balsamifera leaf by HPLC-RID

目的:建立HPLC-RID同时测定艾纳香叶中左旋樟脑、左旋龙脑及异龙脑含量的方法。方法:采用甲醇加热提取,酸性氧化铝柱层析处理,测定7种不同干燥方法对艾纳香叶中左旋樟脑、左旋龙脑及异龙脑含量的影响;HPLC色谱条件:依利特C_(18)柱(150mm×4.6mm,5μm),流动相:65%-0.4%磷酸甲醇溶液,流速:1.0m L/min,柱温:40℃,示差检测器。结果:左旋樟脑、左旋龙脑及异龙脑分别在0.102-1.535、0.103-1.554、0.107-1.607mg/m L内呈良好的线性关系,回归方程分别为Y=79 284X+4 796.6(r=0.9993)、Y=79 415X+2756.0(r=0.9991)、Y=77 727X+2 635.7(r=0.9990),平均加样回收率(n=6)分别为101.06%(RSD=1.42%)、98.14%(RSD=0.78%)、95.28%(RSD=1.21%);酸性氧化铝柱层析法前处理能有效的去除杂质对测定的干扰;不同干燥方法左旋龙脑含量由高至低为室内阴干>30℃烘干>冷冻干燥>室外晒干>微波干燥>50℃烘干>70℃烘干。结论:采用酸性氧化铝柱层析前处理,HPLC-RID同时测定左旋樟脑、左旋龙脑及异龙脑含量的方法准确、快捷、可靠,为艾纳香等样品质量控制提供另一种测定方法;不同干燥方法中室内阴干样左旋龙脑含量较高。

Objective: To establish a HPLC-RID method for simultaneous determination of camphor, borneol, and isoborneol contents in leaf of Blumea balsamifera. Methods: Blumea balsamifera leaf was extracted with methanol by heating under reflux, extract was separated and purified by acidic alumina column, and the effects of different dry processing methods on contents of camphor, borneol, and isoborneol in leaf of Blumea balsamifera were detected. The HPLC chromatographic conditions included Hypersil C_(18) column(150mm×4.6mm, 5μm), 65%methanol-0.4%phosphoric acid solution at the flow rate 1.0m L/min of the mobile phase, the column temperature was controlled at 40℃ and refractive index detector(RID) was used. Results: The linear ranges of camphor, borneol, and isoborneol were 0.102-1.535, 0.103-1.554, 0.107-1.607mg/m L, respectively. The regression equations are Y=79 284X+4 796.6(r=0.9993), Y=79 415X+2 756.0(r=0.9991), Y=77 727X+2 635.7(r=0.9990). The average recovery rate(n=6) of camphor, borneol, and isoborneol were 101.06%(RSD=1.42%), 98.14%(RSD=0.78%) and 95.28%(RSD=1.21%). Acidic alumina column can effectively eliminate the interference of impurities on the determination. The content of borneol as indoor shade-dried>30℃ dried>freeze-dried>sun-dried>microwave-dried>50℃ dried>70℃ dried. Conclusion: The HPLC-RID method is precise, reproducible and stable, which can be applied in the quality control of Blumea balsamifera leaf. The content of borneol in the indoor shade-dried method is the highest.