摘要
目的建立仙灵骨葆胶囊(XLGB)多波长高效液相色谱-紫外真空波-蒸发光散射检测器(HPLC-UVD-ELSD)指纹图谱结合主要代表成分同时定量的方法,对市售制剂进行整体质量控制。方法采用Poroshell 120 EC-C18色谱柱(4. 6 mm×100mm,2. 7μm);检测波长分别为240、270、334 nm; ELSD漂移管温度105℃;载气流速2. 0 L·min-1;建立XLGB多波长HPLCUVD-ELSD指纹图谱,对主要特征峰进行明确化学指认并确定组方中药来源,运用相似度软件对15批市售制剂进行相似度评价,同时在市售制剂批间差异小的前提下测定主要代表成分的含量。结果建立了XLGB多波长HPLC-UVD-ELSD指纹图谱结合6个代表成分同时定量的方法;覆盖该复方6味组方中药的31个主要特征峰得到明确化学指认,并初步确定了26个特征峰的组方中药来源; 15批市售制剂的指纹图谱与对照指纹图谱的相似度值在0. 943~0. 997之间; 6个定量成分线性关系良好(r=0. 999 0~0. 999 6),且平均回收率为98. 5%~104. 9%。结论该方法专属、快速、高效,能全面反映XLGB的整体质量;且贴近实际生产,有望进一步规范、提升成为企业内控标准。
OBJECTIVE To establish the fingerprint of Xianling Gubao Capsules （XLGB） by multi-wavelength HPLC-UVD- ELSD and determine the main representative components simultaneously, in order to provide reference for the overall quality control of XLGB. METHODS The separation was developed on Poroshell 120 EC-Cls column （4. 6 mm × 100 mm, 2. 7 μm） by gradient elution with methanol-water [ both containing 0. 1% （V/V） formic acid] at 240,270 and 334 nm, the temperature of drift tube was maintained at 105℃ and the carrier gas flow rate was 2. 0 L · min-1. An HPLC-UVD-ELSD fingerprint of XLGB was set up, and 15 batches of XLGB were evaluated by similarity assay. Furthermore, the contents of the main representative components were determined on the premise of small disparities between batches. RESULTS The multi-wavelength HPLC-UVD-ELSD fingerprint of XLGB was estab- lished with good separation, and six chemical components were determined simultaneously. Thirty-one main characteristic peaks from six herbs of XLGB were chemically identified and 26 main characteristic peaks were assigned to individual herbs. The similarity of 15 batches of XLGB was about 0. 943 to 0.997. Moreover, good linear relationships were found （ r = 0. 999 0 - 0. 999 6） , and the average recovery rates were 98.5% - 104. 9%. CONCLUSION The method can be used for the overall quality control of XLGB with good specificity and high efficiency and is close to the actual production, which is promising to be further improved to be used as an industry internal control standard.
作者
姚志红
郑远茹
周先强
李梦森
陈子林
戴毅
姚新生
YAO Zhi-hong;ZHENG Yuan-ru;ZHOU Xlan-qiang;LI Meng-sen;CHEN Zi-lin;DAI Yi;YAO Xin-sheng(Institute of Traditional Chinese Medicine ＆ Natural Products,Jinan University,Guangzhou 510632,China;Guangdong Province Key Laboratory of Pharmacodynamic Constituents of TCM and New Drug Research,College of Pharmacy,Jinan University,Guangzhou 510632,China)
出处
《中国药学杂志》
CAS
CSCD
北大核心
2018年第17期1504-1510,共7页
Chinese Pharmaceutical Journal
基金
国家自然科学基金重大国际合作项目资助(81220108028)
十二五重大新药创制专项项目资助(2011ZX9201-201-05)
