Tang Dao-quan, Li Zheng, Jiang Xiang-lan, Li Yin-jie, Du Qian, Yang Dong-zhi
Department of Pharmaceutical Analysis, Xuzhou Medical College, Xuzhou, Jiangsu, China; Key Laboratory of New Drug and Clinical Application, Xuzhou Medical College, Xuzhou, Jiangsu, China.
J Sep Sci. 2014 Aug;37(16):2131-7. doi: 10.1002/jssc.201400362. Epub 2014 Jun 27.
A rapid and sensitive ultra high performance liquid chromatography method with diode array detection was developed for the fingerprint analysis and simultaneous determination of seven active compounds in Xiaoyanlidan (XYLD) tablets. The chromatographic separations were obtained on an Agilent Eclipse plus C18 column (50 × 2.1 mm id, 1.8 μm) using gradient elution with water/formic acid (1%) and acetonitrile at a flow rate of 0.4 mL/min. Within 63 min, 36 peaks could be selected as the common peaks for fingerprint analysis to evaluate the similarities among several samples of XYLD tablets collected from different manufacturers. In quantitative analysis, seven compounds showed good regression (R > 0.9990) within test ranges and the recovery of the method was within the range of 95.9-104.3%. The method was successfully applied to the simultaneous determination of seven compounds in six batches of XYLD tablets. These results demonstrate that the combination of chromatographic fingerprint analysis and simultaneous multi-ingredient quantification using the ultra high performance liquid chromatography method with diode array detection offers a rapid, efficient, and reliable approach for quality evaluation of XYLD tablets.
建立了一种采用二极管阵列检测的快速灵敏的超高效液相色谱法，用于消炎利胆片（XYLD）指纹图谱分析及同时测定其中7种活性成分。采用Agilent Eclipse plus C18色谱柱（50×2.1 mm内径，1.8μm），以水/甲酸（1%）和乙腈为流动相进行梯度洗脱，流速为0.4 mL/min，实现色谱分离。在63分钟内，可选择36个峰作为指纹图谱分析的共有峰，以评价从不同厂家收集的多个消炎利胆片样品之间的相似度。在定量分析中，7种化合物在测试范围内呈现良好的线性关系（R＞0.9990），方法回收率在95.9% - 104.3%范围内。该方法成功应用于6批消炎利胆片中7种化合物的同时测定。这些结果表明，采用二极管阵列检测的超高效液相色谱法结合色谱指纹图谱分析和同时多成分定量，为消炎利胆片的质量评价提供了一种快速、高效且可靠的方法。
