国际药学研究杂志
國際藥學研究雜誌
국제약학연구잡지
INTERNATIONAL JOURNAL OF PHARMACEUTICAL RESEARCH
2015年
3期
398-403
,共6页
白俊鹏%尚振苹%蒋晓文%马宏达%赵庆春
白俊鵬%尚振蘋%蔣曉文%馬宏達%趙慶春
백준붕%상진평%장효문%마굉체%조경춘
骨碎补%高效液相指纹图谱%含量测定
骨碎補%高效液相指紋圖譜%含量測定
골쇄보%고효액상지문도보%함량측정
Rhizoma Drynariae%high-performance liquid chromatography fingerprint%quantitative analysis
目的:建立骨碎补的指纹图谱方法,并测定其主要成分的含量。为快速评价骨碎补药材的质量,科学评价及完善骨碎补的质量控制提供可靠方法。方法采用如下液相条件进行指纹图谱分析:Zirchrom C18(4.6 mm×200 mm,5μm),甲醇-磷酸水溶液(pH3.6)为流动相梯度洗脱,流速1.0 ml/min,检测波长283 nm,柱温30℃;并对指纹图谱进行相似度和聚类分析。采用如下液相条件进行含量测定:Kromasil C18(250 mm×4.6 mm,5μm),甲醇-磷酸水溶液(pH3.6)为流动相梯度洗脱,流速1.0 ml/min,检测波长283 nm,柱温30℃。结果建立了16个不同产地骨碎补药材的HPLC指纹图谱,标定了12个共有峰,指认了其中6个主要色谱峰,峰面积归一化法计算6个主要色谱峰面积之和占所有色谱峰总面积>70%。通过相似度分析和聚类分析一致发现16批药材质量可分为3类,说明市售骨碎补药材质量参差不齐。初步建立了骨碎补质量控制方法,采用外标法对16批骨碎补中4个主要成分(E)-4-O-β-D-吡喃葡萄糖基香豆酸、咖啡酸-4-O-β-D-吡喃葡萄糖苷,5,7,3′,5′-四羟基二氢黄酮-7-O-β-D-吡喃葡萄糖苷和柚皮苷进行了含量测定。4个主要成分表现良好的线性范围(r>0.9995)和回收率(97.9%~103.7%)。结论该方法特征性及专属性强,为科学评价及完善骨碎补的质量控制提供可靠方法。
目的:建立骨碎補的指紋圖譜方法,併測定其主要成分的含量。為快速評價骨碎補藥材的質量,科學評價及完善骨碎補的質量控製提供可靠方法。方法採用如下液相條件進行指紋圖譜分析:Zirchrom C18(4.6 mm×200 mm,5μm),甲醇-燐痠水溶液(pH3.6)為流動相梯度洗脫,流速1.0 ml/min,檢測波長283 nm,柱溫30℃;併對指紋圖譜進行相似度和聚類分析。採用如下液相條件進行含量測定:Kromasil C18(250 mm×4.6 mm,5μm),甲醇-燐痠水溶液(pH3.6)為流動相梯度洗脫,流速1.0 ml/min,檢測波長283 nm,柱溫30℃。結果建立瞭16箇不同產地骨碎補藥材的HPLC指紋圖譜,標定瞭12箇共有峰,指認瞭其中6箇主要色譜峰,峰麵積歸一化法計算6箇主要色譜峰麵積之和佔所有色譜峰總麵積>70%。通過相似度分析和聚類分析一緻髮現16批藥材質量可分為3類,說明市售骨碎補藥材質量參差不齊。初步建立瞭骨碎補質量控製方法,採用外標法對16批骨碎補中4箇主要成分(E)-4-O-β-D-吡喃葡萄糖基香豆痠、咖啡痠-4-O-β-D-吡喃葡萄糖苷,5,7,3′,5′-四羥基二氫黃酮-7-O-β-D-吡喃葡萄糖苷和柚皮苷進行瞭含量測定。4箇主要成分錶現良好的線性範圍(r>0.9995)和迴收率(97.9%~103.7%)。結論該方法特徵性及專屬性彊,為科學評價及完善骨碎補的質量控製提供可靠方法。
목적:건립골쇄보적지문도보방법,병측정기주요성분적함량。위쾌속평개골쇄보약재적질량,과학평개급완선골쇄보적질량공제제공가고방법。방법채용여하액상조건진행지문도보분석:Zirchrom C18(4.6 mm×200 mm,5μm),갑순-린산수용액(pH3.6)위류동상제도세탈,류속1.0 ml/min,검측파장283 nm,주온30℃;병대지문도보진행상사도화취류분석。채용여하액상조건진행함량측정:Kromasil C18(250 mm×4.6 mm,5μm),갑순-린산수용액(pH3.6)위류동상제도세탈,류속1.0 ml/min,검측파장283 nm,주온30℃。결과건립료16개불동산지골쇄보약재적HPLC지문도보,표정료12개공유봉,지인료기중6개주요색보봉,봉면적귀일화법계산6개주요색보봉면적지화점소유색보봉총면적>70%。통과상사도분석화취류분석일치발현16비약재질량가분위3류,설명시수골쇄보약재질량삼차불제。초보건립료골쇄보질량공제방법,채용외표법대16비골쇄보중4개주요성분(E)-4-O-β-D-필남포도당기향두산、가배산-4-O-β-D-필남포도당감,5,7,3′,5′-사간기이경황동-7-O-β-D-필남포도당감화유피감진행료함량측정。4개주요성분표현량호적선성범위(r>0.9995)화회수솔(97.9%~103.7%)。결론해방법특정성급전속성강,위과학평개급완선골쇄보적질량공제제공가고방법。
Objective To investigate fingerprint analysis and quantification of Rhizoma Drynaria. Methods HPLC fingerprints were carried out at 30℃on a Zirchrom C18 column (4.6 mm×200 mm, 5μm). The mobile phase was methanol (A) and phosphoric acid aqueous solution (pH3.6, B). Gradient programmer was performed in linear gradient. The chromatogram was monitored at a wavelength of 283 nm throughout the experiment and the chromatographic peaks were obtained, ranging from 200 nm to 400 nm. The injection volume was 10μl. Then quantitative analyses were carried out at 30℃on a Kromasil C18 column (250 mm×4.6 mm,5μm). Results In fingerprint analysis, plant materials from 16 regions were analyzed under the optimized HPLC conditions and 12 peaks were selected as characteristic peaks. Compared with the reference standards, 6 major chromatographic peaks were characterized and identified, with sum of peaks area over 70% according to area normalization method. Additionally, the similarity analysis and HCA analysis were performed and the results got mutual authentication. In quantitative analysis, the four compounds showed good regression(r>0.9995) within test ranges and the recovery of the method was in the range of 97.9%-103.7%. Conclusion The results revealed that the method of reference chromatographic fingerprints combined with multiple compounds determination could be used as an efficient strategy for systematic quality evaluation of Rhizoma Drynariae.