麦枣怡神颗粒的指纹图谱研究

目的:建立麦枣怡神颗粒的指纹图谱,为其后续开发提供科学依据。方法:以10批麦枣怡神颗粒为样品,采用高效液相色谱(HPLC)法建立指纹图谱。色谱柱为Venusil XBP C18(L);流动相为乙腈-0.2%磷酸(梯度洗脱);流速在7~10 min时为1→0.7mL/min,10~15 min时为0.7→1 mL/min,其余时间为1 mL/min;检测波长分别为284 nm(0~7 min)、330 nm(7~32 min)、360 nm(32~45 min);柱温为25℃;进样量为10μL。采用"中药色谱指纹图谱相似度评价系统"(2004 A版)软件生成指纹图谱并进行相似度评价,然后通过对照药材及对照品对各共有峰进行归属和指认。结果:在方法学考察中,精密度、稳定性(24 h)、重复性均良好[各共有峰的相对峰面积和相对保留时间的RSD均<3%(n=6)]。10批样品的相似度均在0.900以上。共确定了17个共有峰,其中共有峰1、6来自莱菔子,共有峰7、9、14、15、16来自陈皮,共有峰5、10、11、12、13来自甘草,共有峰2来自陈皮、甘草、酸枣仁,共有峰3来自甘草、莱菔子,共有峰8来自大麦、莱菔子,共有峰4、17均来自陈皮、甘草。并指认了其中共有峰1为橙皮苷,共有峰9为芥子碱。结论:该方法建立的麦枣怡神颗粒指纹图谱准确、可靠,可以用于麦枣怡神颗粒的质量控制。

Fingerprint Study of Maizao Yishen Granules

OBJECTIVE:To establish the fingerprint of Maizao yishen granules,and to provide scientific basis for its further development. METHODS:HPLC method was adopted to establish the fingerprint by using 10 batches of Maizao yishen granules sa samples. The determination was performed on Venusil XBP C18(L) column with mobile phase consisted of acetonitrile-0.2%phosphoric acid(gradient elution)at the flow rate of 1→0.7 mL/min at 7-10 min,0.7→1 mL/min at 10-15 min and 1 mL/min at the rest of time. The detection wavelengths were set at 284 nm(0-7 min),330 nm(7-32 min)and 360 nm(32-45 min). The column temperature was 25 ℃,and sample size was 10 μL. The fingerprint of Maizao yishen granules was established,and the similarity evaluation was performed by using"Similarity Evaluation System of TCM Chromatographic Fingerprints"(2004 A edition)software. Then,the common peaks were assigned and identified by comparing reference substance and control medicinal materials. RESULTS:The precision,stability(24 h) and repeatability of the methodological investigation were all good [RSD values of relative retention time and relative peak area of each chromatographic peak were less than 3%(n=6)]. The similarity of10 batches of samples were all above 0.900. Seventeen common peaks were identified,of which common peak 1 and 6 came from Semen Raphani;common peak 7,9,14,15 and 16 from Citrus reticulata;common peak 5,10,11,12 and 13 came from Glycyrrhiza uralensis;common peak 2 came from C. reticulata,G. uralensis and Ziziphus jujuba;peak 3 came from G. uralensis and Semen Raphani;peak 8 came from Hordeum vulgare and Semen Raphani;peak 4 and 17 came from C. reticulata and G.uralensis. Peak 1 was identified as hesperidin and the peak 9 was identified as sinapine. CONCLUSIONS:Established fingerprint of Maizao yishen granules is accurate and reliable,and can be used for quality control of Maizao yishen granules.