对2020年版《中华人民共和国药典》中艾叶所含桉油精、龙脑2种成分测定方法的改进

On the improvement of determination method of eucalyptol and borneol in Aetemisia argyi in Chinese Pharmacopoeia(2020 edition)

目的改进2020年版《中华人民共和国药典》中艾叶所含桉油精、龙脑2种成分的气相色谱条件,解决原方法分析时间长且不能使龙脑完全分离的问题。方法将气相色谱条件改进为初始温度100℃,以每分钟5℃升至150℃,再以每分钟10℃升至250℃,保持1 min;气体流量由原来的每分钟0.6 m L改为每分钟1.0 m L,其他分析条件不变。结果桉油精、龙脑线性回归方程分别为Y=926497X-32.265(r=0.9999),Y=992324X-329.080(r=0.9999),分别在2.00768~451.72800,0.97408~219.16980μg范围内呈良好的线性关系,平均加样回收率分别为96.0%,97.2%,RSD分别为1.561%,1.610%,检测限分别为0.4015,0.1948μg/m L,二者均在21 min内基线达到分离。结论本方法可使艾叶中龙脑完全分离,解决了原方法使龙脑分离不完全、含量计算有误差的问题,且显著缩短了桉油精、龙脑出峰时间,检测结果可靠、稳定、重现性好,可用于艾叶药材的质量控制。

Objective To improve the gas chromatographic conditions of the two components of eucalyptol and borneol under the"Assay"item in the 2020 edition of the Chinese Pharmacopoeia,and solve the problem of the long analysis time of the original method and the inability to separate the borneol completely.Methods Optimize the gas chromatographic conditions in the original method to an initial temperature of 100℃,first increase to 150℃at a rate of 5℃per minute,then increase to 250℃at a rate of 10℃per minute,and hold for 1 minute;the gas flow rate changes from the original per minute 0.6 m L to 1.0 m L,and other analysis conditions remain unchanged.Results The linear regression equations of eucalyptol and borneol were Y=926497X-32.265(r=0.9999)and Y=992324X-329.080(r=0.9999),respectively.The linear relationship is good in the ranges of 2.00768 to 451.72800μg and0.97408 to 219.16980μg,respectively.The average recoveries were 96.0%and 97.2%,with RSDs of 1.561%and1.610%,respectively.The detection limits were 0.4015 and 0.1948μg/m L.Both of them reached baseline separation within 21 min.Conclusion This method can separate borneol completely from Artemisia argyi,solve the problem that the tested borneol component cannot be separated accurately from other components in the original method,and shortens the peak time of eucalyptol and borneol significantly.The test results are reliable,stable and reproducible,and can be used for the quality control of Artemisia argyi.