State Key Laboratory of Quality Research in Chinese Medicine (University of Macau), Macao.
J Pharm Biomed Anal. 2012 Jul;66:170-5. doi: 10.1016/j.jpba.2012.03.041. Epub 2012 Mar 28.
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.
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。