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作 者:吕朝耕 杨健[1] 康传志 杨婉珍[1,2] 周利[1,3] 李振皓 郭兰萍
机构地区:[1]中国中医科学院中药资源中心道地药材国家重点实验室培育基地,北京100700 [2]首都医科大学中医药学院,北京100069 [3]广东药科大学中药学院,广东广州510006 [4]浙江寿仙谷医药股份有限公司,浙江武义321200
出 处:《中药材》2017年第6期1360-1363,共4页Journal of Chinese Medicinal Materials
基 金:国家自然科学基金(81130070;81072989);国家科技支撑计划项目(2012BAI29B02;2012BAI28B002)
摘 要:目的:建立UPLC-MS/MS法同时测定铁皮石斛中9个有机酸类成分的含量。方法:采用ACQUITY UPLC BEH C_(18)色谱柱(100 mm×2.1 mm,1.8μm);以0.1%甲酸溶液(A)-0.1%甲酸乙腈(B)为流动相,梯度洗脱;流速0.6 mL/min;柱温40℃。采用电喷雾离子源,负离子检测方式,得到相应的提取离子流图,以峰面积进行定量。结果:9个有机酸类成分具有良好的线性关系,r值均大于0.998,方法精密度、重复性和稳定性的RSD值均小于3%,加样回收率在95.61%~102.66%,RSD值均小于3.5%。不同产地铁皮石斛中有机酸类成分在组成和含量上存在较大差异。结论:该研究建立的方法操作简便、准确、重复性好,可用于铁皮石斛药材中有机酸类成分的定量测定,测定结果可为该药材质量标准的完善提供依据。Objective:To establish an UPLC-MS/MS method for the simultaneous determination of nine organic acids in Dendrobium officinale.Methods:The determination was carried out by an ACQUITY UPLC BEH C1s (100 mm × 2.1 mm,1.8 μm)with a gradient elution system using 0.1% formic acid(A)-acetonitrile(with 0.1% formic acid) (B)as mobile phase,the flow rate was 0.6 mL/ min,the column temperature was 40 ℃.MS instrument was equipped with ESI-Ion source,gaining the extracted ion chromatograms.Results:The nine components had good linearity (r 〉 0.998),and the precision,repeatability,stability and accuracy of the established method were well-validated and proved to be satisfactory,with the RSD 〈 3 %.The recoveries were 95.61% ~ 102.66%,with the RSD 〈 3.5%.There were great differences in composition and content of organic acids in Dendrobium officinale from different habitats.Conclusion:The established method is proved to be rapid,accurate and sensitive for the determination of organic acids in Dendrobium officinale.Moreover,the quantitative results may be useful for the improvement of quality control of this herbal medicine.
关 键 词:有机酸 超高效液相色谱-三重四级杆串联质谱 铁皮石斛 质量评价
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