Sun Yan-Mei, Wu Hai-Long, Wang Jian-Yao, Liu Zhi, Zhai Min, Yu Ru-Qin
State Key Laboratory of Chemo/Biosensing and Chemometrics, College of Chemistry and Chemical Engineering, Hunan University, Changsha 410082, China.
State Key Laboratory of Chemo/Biosensing and Chemometrics, College of Chemistry and Chemical Engineering, Hunan University, Changsha 410082, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Jul 1;962:59-67. doi: 10.1016/j.jchromb.2014.05.027. Epub 2014 May 24.
A fast analytical strategy of second-order calibration method based on the alternating trilinear decomposition algorithm (ATLD)-assisted high performance liquid chromatography coupled with a diode array detector (HPLC-DAD) was established for the simultaneous determination of eight flavonoids (rutin, quercetin, luteolin, kaempferol, isorhamnetin, apigenin, galangin and chrysin) in propolis capsules samples. The chromatographic separation was implemented on a Wondasil™ C18 column (250mm×4.6mm, 5μm) within 13min with a binary mobile phase composed of water with 1% formic acid and methanol at a flow rate of 1.0mLmin(-1) after flavonoids were only extracted with methanol by ultrasound extraction for 15min. The baseline problem was overcome by considering background drift as additional compositions or factors as well as the target analytes, and ATLD was employed to handle the overlapping peaks from analytes of interest or from analytes and co-eluting matrix compounds. The linearity was good with the correlation coefficients no less than 0.9947; the limit of detections (LODs) within the range of 3.39-33.05ngmL(-1) were low enough; the accuracy was confirmed by the recoveries ranged from 91.9% to 110.2% and the root-mean-square-error of predictions (RMSEPs) less than 1.1μg/mL. The results indicated that the chromatographic method with the aid of ATLD is efficient, sensitive and cost-effective and can realize the resolution and accurate quantification of flavonoids even in the presence of interferences, thus providing an alternative method for accurate quantification of analytes especially when the complete separation is not easily accomplished. The method was successfully applied to propolis capsules samples and the satisfactory results were obtained.
建立了一种基于交替三线性分解算法(ATLD)辅助的高效液相色谱-二极管阵列检测器(HPLC-DAD)的二阶校正快速分析策略,用于同时测定蜂胶胶囊样品中的8种黄酮类化合物(芦丁、槲皮素、木犀草素、山柰酚、异鼠李素、芹菜素、高良姜素和白杨素)。黄酮类化合物经甲醇超声提取15分钟后,在Wondasil™ C18柱(250mm×4.6mm,5μm)上进行色谱分离,13分钟内完成,流动相为含1%甲酸的水和甲醇组成的二元流动相,流速为1.0mLmin(-1)。通过将背景漂移视为额外的成分或因素以及目标分析物来克服基线问题,并采用ATLD处理目标分析物或分析物与共洗脱基质化合物的重叠峰。线性良好,相关系数不低于0.9947;检测限(LOD)在3.39-33.05ngmL(-1)范围内足够低;回收率在91.9%至110.2%之间,预测均方根误差(RMSEP)小于1.1μg/mL,证实了准确性。结果表明,借助ATLD的色谱方法高效、灵敏且经济高效,即使在存在干扰的情况下也能实现黄酮类化合物的分离和准确定量,从而为分析物的准确定量提供了一种替代方法,尤其是在不易实现完全分离的情况下。该方法成功应用于蜂胶胶囊样品,获得了满意的结果。