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作 者:王新科 段雯利 Wang Xinke;Duan Wenli(Drug Inspection,Monitoring and Evaluation Center in Yangling Demonstration Area,Shaanxi Yangling 712100,China)
机构地区:[1]杨凌示范区药品检验监测评价中心,陕西杨陵712100
出 处:《中国药师》2020年第12期2499-2501,共3页China Pharmacist
摘 要:目的:采用HPLC法检测鼻咽清毒颗粒中苍术苷和羧基苍术苷两味毒性成分的限量。方法:采用Waters XTERRA C18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.35%磷酸二氢钠溶液(含0.15%四丁基氢氧化铵,磷酸调pH至3.5)(35∶65),检测波长203 nm,流速1.0 ml·min-1,柱温30℃,进样量10μl。结果:苍术苷和羧基苍术苷分别在0.0610~2.443,0.0232~0.929μg·ml-1浓度范围内与峰面积呈良好的线性关系(r分别为0.9998和0.9999);平均回收率分别为99.71%和99.04%,RSD分别为0.59%和0.74%(n=9)。结论:该方法简便、重复性好、回收率高、结果可靠,可用于鼻咽清毒颗粒中毒性成分苍术苷和羧基苍术苷的限量检查。Objective: To establish an HPLC method for the determination of toxic components atractyloside and carboxyatractyloside in Biyan Qingdu granules. Methods: The determination was performed on a Waters XTERRA C18( 250 mm×4.6 mm,5 μm) column with the mobile phase consisting of acetonitrile-0.35% sodium dihydrogen phosphate solution( containing 0.15% tetrabutylammonium hydroxide,adjusting pH to 3.5 with phosphoric acid)( 35 ∶ 65) at the flow rate of 1.0 ml·min-1. The detection wavelength was set at 203 nm. The column temperature was set at 30 ℃ and the injection volume was 10 μl. Results: The linear range of atractyloside and carboxyatractyloside was 0.061 0-2.443( r = 0.999 8) and 0.023 2-0.929 μg·ml-1( r= 0.999 9),respectively;the average recovery was 99.71% and 99.04%,and the RSD was 0.59% and 0.74%( n = 9),respectively. Conclusion: The method is simple and reproducible with high recovery and reliable results. It can be used for the limit detection of atractyloside and carboxyatractyloside in Biyan Qingdu granules.
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