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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 HPLC fingerprint of TGP Tongxijianling granule (CXG) and to conduct multi-component quantitative analysis to provide a basis for evaluating its quality. Methods The mobile phase consisted of Dilma Luster ODS (250 mm × 4.6 mm, 5 μm) with methanol-0.1% phosphoric acid as mobile phase. The gradient elution was 0-15 min, 20-30% methanol and 15-30 min % Methanol; 30-40 min, 30-60% methanol; 40-55 min, 60% methanol; volume flow rate 1.0 m L / min; detection wavelength 254, 283, 274, 300 nm; The quality evaluation of 10 batches of CXG fingerprints was carried out by the similarity evaluation, and the 6 index components were identified quantitatively. Results A total of 18 common peaks of CXG HPLC fingerprints were identified. Six of the six components were identified as cimnifluralin (No.4), 5-O-methyl-Vaisalain (7 Peppermint (peak 10), hesperidin (peak 15), paeonol (peak 16) and imperatorin (peak 17) were used to fingerprint 10 batches of samples using the similarity software Atlas analysis, the similarity of batches of samples are above 0.9. The linear range of ciclinoid, 5-O-methylvishisainin, pentmentone, hesperidin, paeonol and imperatorin were 0.013-0.505 mg / m L (r = 0.999 8 (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) and 0.006-0.251 mg / m L (r = 0.999 5) and 0.014-0.576 mg / m L (r = 0.999 4). The mass fractions of ciminosine, 5-O-methylvishisainin, pentmentone, hesperidin, paeonol and imperatorin in 10 batches of samples were 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 and 11.152 ~ 11.291 mg / g. Conclusion The established CXG HPLC fingerprinting and quantitative analysis method has high sensitivity and specificity and can be used for the quality control of CXG.