气相色谱法同时测定龙脑樟鲜叶中右旋龙脑、樟脑及乙酸龙脑酯的含量

Simultaneous Determination of the Contents of d-Borneol,Camphor and Bornyl Acetate in the Leaves of Cinnamomum camphora chvar.Borneol by GC

建立了气相色谱法同时测定龙脑樟鲜叶中右旋龙脑、樟脑及乙酸龙脑酯含量的方法。采用水蒸气蒸馏法提取龙脑樟鲜叶中的天然冰片,硅胶柱层析法精制天然冰片粗品,GC法测定其中右旋龙脑、樟脑及乙酸龙脑酯的含量。色谱条件:色谱柱为DB-5MS(30.00 m×250.00μm×0.25μm),进样量1μL,柱温从90℃开始程序升温,流速1 mL/min,进样口温度280℃。右旋龙脑、樟脑及乙酸龙脑酯的回归方程分别为y=3.4462x-7.4057(r=0.9998);y=3.4881x-0.0026(r=0.9999);y=2.8657x-0.0914(r=1.0000),表明三者分别在99.14~991.37μg/mL、1.92~19.18μg/mL及2.01~20.01μg/mL范围内线性关系良好。三者的平均回收率分别为100.86%、98.36%和101.66%,相对标准偏差(RSD)分别为1.94%、2.88%和2.18%。从龙脑樟鲜叶中提取纯化后的天然冰片中右旋龙脑质量分数均在98.45%以上,樟脑及乙酸龙脑酯质量分数较低,不含异龙脑,说明龙脑樟鲜叶质量较佳。该法操作简便、准确、精密度高、分离度好,分析时间短,可为龙脑樟药材的质量控制提供参考。

To establish a GC method for simultaneous determination of the contents of d-borneol,camphor and bornyl acetate in the leaves of Cinnamomum camphora chvar.Borneol,the crude product of the leaves of Cinnamomum camphora chvar.Borneol was obtained by steam distillation and purified by column chromatography,in which,the contents of d-borneol,camphor and bornyl acetate were determined by GC assay.Chromatographic conditions were as follows:chromatographic column was silica capillary column(30.00 m×250.00μm×0.25μm),initial temperature was 90℃,carrier gas was high purity(≥99.999%)helium,flow rate was 1 mL/min,injection volume was 1μL,and inlet temperature was 280℃.The respective regression equations of d-borneol,camphor and bornyl acetate were as follows:y=3.4462x-7.4057(r=0.9998);y=3.4881x-0.0026(r=0.9999);y=2.8657x-0.0914(r=1.0000).They showed a good linear relationship in the range of 99.14μg/mL to 991.37μg/mL,1.92μg/mL to 19.18μg/mL,2.01μg/mL to 20.01μg/mL,respectively.The respective average recovery were 100.86%,98.36%and 101.66%,with RSDs of 1.94%,2.88%and 2.18%respectively.After extraction and purification,the mass percentage content of d-borneol was all over 98.45%,the content of camphor and bornyl acetate were low,excluding isoborneol.The established GC method could be used for quality control of Cinnamomum camphora chvar.Borneol,which is simple,accurate,sensitive,precise and rapid.