气相色谱法同时测定不同厂家大活络丸中异龙脑龙脑和丁香酚的含量

Simultaneous determination of isoborneol,borneol and eugenol in Da Huoluo pills by gas chromatogrephy

目的建立同时测定大活络丸中异龙脑、龙脑和丁香酚含量的毛细管气相色谱法,并对不同厂家和不同批次的大活络丸进行质量控制。方法采用HP-5毛细管柱(30 m×0.32 mm,0.25μm),升温程序为70℃保持5 min,以5℃/min升温至150℃,再以20℃/min升温至280℃,保持5 min,进样分流比为5∶1;进样口温度为200℃;FID检测器温度为300℃;载气为高纯氮气,流速为2.0 mL/min;进样量为1μL。结果异龙脑、龙脑和丁香酚在同一色谱条件下可完全分离,分别在1.565~78.230μg/mL,1.660~83.010μg/mL,1.570~78.500μg/mL范围内具有良好的线性关系,平均加样回收率分别为99.22%、99.83%、101.79%,相对标准偏差(RSD)分别为1.02%、0.98%、1.14%。结论该方法为大活络丸中冰片和丁香的质量控制提供了参考依据。

Objective To establish a gas chromatography(GC)method to simultaneously determine the contents of isoborneol,borneol and eugenol in Da Huoluo pills.Methods The separation was achieved on HP-5 column(30 m×0.32 mm,0.25μm).The column temperature was programmed from 70℃(holding 5 min)to 150℃at 5℃/min,then to 280℃at 20℃/min(holding 5 min).The inlet temperature was 200℃.The FID detection temperature was 300℃.Highly pure nitrogen was used as the carrier gas(2.0 mL/min);the injection volume was 1μL.Results Isoborneol,borneol and eugenol had been separated well under the same chromatographic condition.Good linearities of isoborneol,borneol and eugenol were obtained within the ranges of 1.565-78.230μg/mL,1.660-83.010μg/mL and 1.570-78.500μg/mL,respectively.The average recoveries were 99.22%,99.83%and 101.79%,and the RSDs were 1.02%,0.98%and 1.14%,respectively.Conclusion The method is a supplement to the quality control of Da Huoluo pills.