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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 the simultaneous determination of levodincarnone, levonorilol and isoborneol in elmentir leaves. Methods: The effects of seven different drying methods on the contents of levodincarnone, levonorubicin and isoborneol were studied by methanol heating and acidic alumina column chromatography. HPLC chromatographic conditions were as follows: Eighteen C 18 ) Column (150 mm × 4.6 mm, 5 μm), mobile phase: 65% -0.4% phosphoric acid in methanol, flow rate: 1.0 mL / min, column temperature: 40 ° C, differential detector. Results: There was a good linear relationship between L-camphor, levonorrhea and isoborneol in 0.102-1.535,0.103-1.554,0.107-1.607mg / m L, the regression equation was Y = 79284X + 4 796.6 (r = (N = 6) were 101.06% (RSD = 1.42%), 98.14 (r = 0.9993), Y = 79 415X + 2756.0 (r = 0.9991) and Y = 77 727X + (RSD = 0.78%) and 95.28% (RSD = 1.21%). The pretreatment with acidic alumina column chromatography can effectively remove the interference of the impurities on the determination. The content of levoborane in different drying methods is from high to low, > 30 ℃ drying> freeze-drying> outdoor drying> microwave drying> 50 ℃ drying> 70 ℃ drying. CONCLUSION: The method of simultaneous determination of levofloxacin, levonorrhea and isoborneol by HPLC-RID with acidic alumina column chromatography is an accurate, rapid and reliable method for the quality control of some samples ; Different methods of drying indoor indolent levoneriodine content is higher.