Kim Won Il, Zhao Bing Tian, Zhang Hai Yan, Lee Je Hyun, Son Jong Keun, Woo Mi Hee
College of Pharmacy, Catholic University of Daegu, Gyeongsan, 712-702, Korea.
Arch Pharm Res. 2014;37(9):1139-47. doi: 10.1007/s12272-013-0295-z. Epub 2013 Dec 6.
Two rapid and simple HPLC methods with UV detector to determine three main compounds (magnoflorine, spinosin and 6'''-feruloyl spinosin) and evaporative light scattering detector (ELSD) to determine jujuboside A were developed for the chemical analyses of Zizyphi Semen. Magnoflorine, spinosin, and 6'''-feruloyl spinosin were separated with an YMC J'sphere ODS-H80 column (250 mm × 4.6 mm, 4 μm) by the gradient elution followed by the isocratic elution using methanol with 0.1 % formic acid and water with 0.1 % formic acid as the mobile phase. The flow rate was 1.0 mL/min. Jujuboside A was separated by HPLC-ELSD with YoungJinBioChrom Aegispak C18-L column (250 mm × 4.6 mm, 5 μm) column in a gradient elution using methanol with 0.1 % formic acid (A) and water with 0.1 % formic acid as the mobile phase. These two methods were fully validated with respect to linearity, precision, accuracy, stability, and robustness. These HPLC methods were applied successfully to quantify four compounds in a Zizyphi Semen extract. The HPLC analytical methods were validated for pattern recognition analysis by repeated analysis of 91 seed samples corresponding to 48 Zizyphus jujuba var. spinosa (J01-J48) and 43 Zizyphus mauritiana (M01-M43). The results indicate that these methods are suitable for a quality evaluation of Zizyphi Semen.
建立了两种快速简便的高效液相色谱法用于酸枣仁的化学分析，一种采用紫外检测器测定三种主要化合物（木兰碱、斯皮诺素和6'''-阿魏酰斯皮诺素），另一种采用蒸发光散射检测器（ELSD）测定酸枣仁皂苷A。木兰碱、斯皮诺素和6'''-阿魏酰斯皮诺素采用YMC J'sphere ODS-H80柱（250 mm×4.6 mm，4μm），以甲醇-0.1%甲酸和水-0.1%甲酸为流动相，先梯度洗脱后等度洗脱进行分离，流速为1.0 mL/min。酸枣仁皂苷A采用HPLC-ELSD，以YoungJinBioChrom Aegispak C18-L柱（250 mm×4.6 mm，5μm），以甲醇-0.1%甲酸（A）和水-0.1%甲酸为流动相进行梯度洗脱分离。这两种方法在线性、精密度、准确度、稳定性和耐用性方面均得到充分验证。这些高效液相色谱法成功应用于酸枣仁提取物中四种化合物的定量分析。通过对91份种子样品（对应48个酸枣变种酸枣（J01-J48）和43个毛叶枣（M01-M43））的重复分析，对高效液相色谱分析方法进行了模式识别分析验证。结果表明，这些方法适用于酸枣仁的质量评价。
