齿痛消炎灵颗粒HPLC特征指纹图谱研究及多成分定量测定  

HPLC fingerprint and determination of multi-components in Chitong Xiaoyanling Granules

作　　者：徐放[1,2] 李明珠[2] 孙阳[2] 王艳杰[2] 梁颖[2] 吴勃岩[2] 安铁洙[1] 

机构地区：[1]东北林业大学生命科学学院,黑龙江哈尔滨150040 [2]黑龙江中医药大学基础医学院,黑龙江哈尔滨150040

出　　处：《中草药》2017年第18期3748-3753,共6页Chinese Traditional and Herbal Drugs

基　　金：国家自然科学基金面上项目(31272441)

摘　　要：目的建立齿痛消炎灵颗粒(CXG)的HPLC指纹图谱,并进行多成分定量分析,为评价其质量提供依据。方法采用Dikma Luster ODS(250 mm×4.6 mm,5μm)色谱柱,以甲醇-0.1%磷酸水溶液为流动相,梯度洗脱:0~15 min,20%~30%甲醇;15~30 min,30%甲醇;30~40 min,30%~60%甲醇;40~55 min,60%甲醇;体积流量1.0 m L/min;检测波长254、283、274、300 nm;柱温30℃。通过相似度评价对10批次CXG指纹图谱进行质量评价,并对指认的6个指标成分进行定量测定。结果共确定CXG HPLC指纹图谱18个共有峰,通过与混合对照品比较指认其中6个指标成分分别为升麻素苷(4号峰)、5-O-甲基维斯阿米醇苷(7号峰)、胡薄荷酮(10号峰)、橙皮苷(15号峰)、丹皮酚(16号峰)和欧前胡素(17号峰),利用相似度软件对10批样品指纹图谱进行分析,各批样品相似度均在0.9以上。升麻素苷、5-O-甲基维斯阿米醇苷、胡薄荷酮、橙皮苷、丹皮酚和欧前胡素线性范围分别为0.013~0.505 mg/m L(r=0.999 8)、0.052~2.097 mg/m L(r=0.999 2)、0.019~0.772 mg/m L(r=0.998 9)、0.025~1.003 mg/m L(r=0.999 1)、0.006~0.251 mg/m L(r=0.999 5)和0.014~0.576 mg/m L(r=0.999 4)。10批样品中升麻素苷、5-O-甲基维斯阿米醇苷、胡薄荷酮、橙皮苷、丹皮酚和欧前胡素线质量分数分别在7.267~7.333 mg/g、4.260~4.522 mg/g、2.033~2.093 mg/g、12.234~12.771 mg/g、19.023~19.334 mg/g和11.152~11.291 mg/g。结论所建立的CXG HPLC指纹图谱和定量测定分析方法灵敏度高、专属性强,可用于CXG的质量控制。Objective To establish an HPLC fingerprint and to determine six compounds in Chitong Xiaoyanling Granules（CXG） for reference of the effective quality control. Methods The analysis was carried out on an analytical column Dikma Luster ODS（250 mm × 4.6 mm, 5 μm） with gradient elution by methanol（A）-0.1% phosphoric acid solution（B）（0—15 min, 20%—30% A; 15—30 min, 30% A; 30—40 min, 30%—60% A; 40—55 min, 60% A）, at the detection wavelengths of 254, 283, 274, and 300 nm and a flow rate of 1.0 m L/min. The column temperature was 30 ℃. Similarity evaluation software was used to evaluate the fingerprint of 10 batches of CXG, and the six marker components were quantified. Results The common mode of the fingerprint was set up with 18 common peaks, and six of them were identified by comparison with the reference. The similar degrees of 10 batches of samples were over 0.9, they were prim-O-glucosylcimifugin, 4′-O-β-D-glucosyl-5-O-methylvisamminol, pulegone, hesperidin, paeonol, and isoimperatorin. The linear ranges were 0.013—0.505 mg/m L（r = 0.999 8）, 0.052—2.097 mg/m L（r = 0.999 2）, 0.019—0.772 mg/m L（r = 0.998 9）, 0.025—1.003 mg/m L（r = 0.999 1）, 0.006—0.251 mg/m L（r = 0.999 5）, and 0.014—0.576 mg/m L（r = 0.999 4） for primO-glucosylcimifugin, 4′-O-β-D-glucosyl-5-O-methylvisamminol, pulegone, hesperidin, paeonol, and isoimperatorin, respectively. The contents of prim-O-glucosylcimifugin, 4′-O-β-D-glucosyl-5-O-methylvisamminol, pulegone, hesperidin, paeonol, and isoimperatorin were 7.267—7.333, 4.260—4.522, 2.033—2.093, 12.234—12.771, 19.023—19.334, and 11.152—11.291 mg/g in 10 batches of samples, respectively. Conclusion The established method has high sensitivity and specificity, and can be used for the quality control of CXG.

关 键 词：齿痛消炎灵颗粒 HPLC 指纹图谱 相似度分析 升麻素苷 5-O-甲基维斯阿米醇苷 胡薄荷酮 橙皮苷 丹皮酚 欧前胡素 

分 类 号：R286.02[医药卫生—中药学]