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采用高效液相色谱-二极管阵列检测器同时测定佛手果实中香豆素类、黄酮类和柠檬苦素类成分的含量。

Simultaneous quantification of coumarins, flavonoids and limonoids in Fructus Citri Sarcodactylis by high performance liquid chromatography coupled with diode array detector.

机构信息

State Key Laboratory of Quality Research in Chinese Medicine (University of Macau), Macao.

出版信息

J Pharm Biomed Anal. 2012 Jul;66:170-5. doi: 10.1016/j.jpba.2012.03.041. Epub 2012 Mar 28.

Abstract

A high performance liquid chromatography coupled with diode array detector (HPLC-DAD) method was developed for simultaneous quantification of eleven major bioactive components including six coumarins, three flavonoids and two limonoids in Fructus Citri Sarcodactylis. The analysis was performed on a Cosmosil 5 C(18)-MS-II column (4.6 mm × 250 mm, 5 μm) with water-acetonitrile gradient elution. The method was validated in terms of linearity, sensitivity, precision, stability and accuracy. It was found that the calibration curves for all analytes showed good linearity (R(2)>0.9993) within the test ranges. The overall limit of detection (LOD) and limit of quantification (LOQ) were less than 3.0 and 10.2 ng. The relative standard deviations (RSDs) for intra- and inter-day repeatability were not more than 4.99% and 4.92%, respectively. The sample was stable for at least 48 h. The spike recoveries of eleven components were 95.1-104.9%. The established method was successfully applied to determine eleven components in three samples from different locations. The results showed that the newly developed HPLC-DAD method was linear, sensitive, precise and accurate, and could be used for quality control of Fructus Citri Sarcodactylis.

摘要

建立了一种高效液相色谱-二极管阵列检测(HPLC-DAD)法,用于同时定量测定佛手果实中的 11 种主要生物活性成分,包括 6 种香豆素、3 种黄酮类化合物和 2 种柠檬苦素。分析在 Cosmosil 5 C(18)-MS-II 柱(4.6mm×250mm,5μm)上进行,采用水-乙腈梯度洗脱。该方法在线性、灵敏度、精密度、稳定性和准确性方面进行了验证。结果表明,所有分析物的校准曲线均呈良好的线性(R(2)>0.9993),在测试范围内。总体检测限(LOD)和定量限(LOQ)均小于 3.0 和 10.2ng。日内和日间重复性的相对标准偏差(RSD)分别不超过 4.99%和 4.92%。样品在至少 48 小时内稳定。11 种成分的加标回收率为 95.1-104.9%。所建立的方法成功地应用于来自不同产地的 3 个样品中 11 种成分的测定。结果表明,新建立的 HPLC-DAD 方法线性良好、灵敏、准确、精确,可用于佛手果实的质量控制。

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