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目的:建立毛细管气相色谱测定抗感至宝合剂中百秋李醇含量的方法,制定并提高抗感至宝合剂质量标准。方法:样品经石油醚(30~60)℃萃取处理后进行含量测定。色谱条件:HP-5毛细管柱(0.25μm×0.25 mm×30 m);FID检测器,1 177进样口初始温度180℃,保持10 min,以每分钟5℃的速率升温至230℃,保持3 min;进样口温度280℃,检测器温度280℃,分流比37∶1,流速1 mL.min-1,进样量1μL。以正十八烷为内标,理论板数按百秋李醇峰计算不低于50 000。结果:百秋李醇进样量在0.012~0.072μg线性关系良好Y=294X+12.8,(r=0.999 6),平均加样回收率为98.45%,RSD 1.09%。结论:该方法稳定、结果可靠、重复性好,可作为抗感至宝合剂质量控制标准之一。
OBJECTIVE: To establish a method of capillary gas chromatography for the determination of the content of Plectranthrol in Kangzaozhibao Mixture, and to develop and improve the quality standard of Kangzaozhibao Compound. Methods: The samples were extracted with petroleum ether (30 ~ 60) ℃ for determination. Chromatographic conditions: HP-5 capillary column (0.25 μm × 0.25 mm × 30 m); FID detector, 1 177 inlet initial temperature of 180 ° C for 10 min, raising the temperature to 230 ° C at a rate of 5 ° C per minute 3 min; inlet temperature 280 ℃, detector temperature 280 ℃, split ratio 37: 1, flow rate 1 mL.min-1, injection volume 1μL. With n-octadecane as the internal standard, the number of theoretical plates should not be less than 50 000 according to the peak of Plum blossom alcohol. Results: The linear range was 0.012 ~ 0.072μg. The average recovery was 98.45% and the RSD was 1.09%. The average correlation coefficient was 294X + 12.8 (r = 0.999 6). Conclusion: The method is stable, the results are reliable, reproducible, and can be used as one of the quality control standards for Kangnaozhibao Mixture.