本文關(guān)鍵詞： 成分分析 含量測(cè)定 山豆根 生物堿 指紋圖譜　出處：《北京中醫(yī)藥大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：研究目的:山豆根為臨床常用藥,近年來關(guān)于山豆根在臨床使用中出現(xiàn)中毒的現(xiàn)象屢有報(bào)道,原因之一是將毒性大的山豆根與毒性小的北豆根混用,導(dǎo)致患者中毒。而目前關(guān)于山豆根尚缺乏系統(tǒng)性的質(zhì)量標(biāo)準(zhǔn)方面的研究。本研究通過山豆根進(jìn)行指紋圖譜、有效成分含量測(cè)定,并結(jié)合高分辨質(zhì)譜進(jìn)行成分分析,為完善補(bǔ)充現(xiàn)有關(guān)于山豆根的質(zhì)量標(biāo)準(zhǔn)提供參考依據(jù)和思路。研究方法:(1)研究采用UPLC-PDA對(duì)山豆根70%甲醇部位的提取物進(jìn)行指紋圖譜分析,所得cdf格式文件導(dǎo)入到國家藥典委員會(huì)出版的《中藥色譜指紋圖譜相似度評(píng)價(jià)系統(tǒng)A版》軟件進(jìn)行分析,生成山豆根的指紋圖譜共有模式、共有峰以及相似度。并且指定氧化苦參堿作為參照峰,通過計(jì)算其他共有峰的相對(duì)保留時(shí)間和相對(duì)峰面積對(duì)不同產(chǎn)地的山豆根的差異進(jìn)行評(píng)價(jià)。(2)研究通過對(duì)山豆根的提取方法進(jìn)行單因素考察初步確定山豆根的最佳提取條件(包括不同方法、不同溶劑、不同時(shí)間),再通過HPLC-PDA對(duì)樣品進(jìn)行色譜條件考察,實(shí)現(xiàn)對(duì)苦參堿、氧化苦參堿、槐果堿、氧化槐果堿等四種生物堿的分離,最終進(jìn)行定量,最后結(jié)果再采用SAS 8.2統(tǒng)計(jì)分析軟件進(jìn)行聚類分析,將山豆根按產(chǎn)地分為三類,實(shí)現(xiàn)對(duì)不同產(chǎn)地山豆根的差異評(píng)價(jià)。(3)研究通過UPLC-Q-TOF/MS對(duì)道地產(chǎn)區(qū)山豆根進(jìn)行成分而分析,所得數(shù)據(jù)通過Waters公司的配套軟件Unify進(jìn)行智能匹配分析,最終確定山豆根中可能含有的成分。研究結(jié)果:(1)13批山豆根含有27個(gè)共有色譜峰,指認(rèn)了其中2個(gè)分別是苦參堿和氧化苦參堿;不同批次山豆根藥材共有峰相對(duì)保留時(shí)間在3.925%～4.588%之間,而相對(duì)峰面積的RSD較大,且13批山豆根藥材的相似度大部分大于0.9,但其中2批北豆根的相似度則較差。(2)13批山豆根中有12批苦參堿與氧化苦參堿的總含量達(dá)到藥典標(biāo)準(zhǔn)(≥0.7%),有1批含量低于藥典標(biāo)準(zhǔn),且13個(gè)產(chǎn)地按照苦參堿、氧化苦參堿、槐果堿、氧化槐果堿的含量大概可以分為三類。(3)通過Unify軟件智能匹配,并結(jié)合文獻(xiàn)中的特征碎片離子比對(duì),推斷出山豆根中含有的56種成分。研究結(jié)論:(1)本研究中的不同產(chǎn)地的山豆根在化學(xué)成分上相似度良好,該方法精密度、穩(wěn)定性及重復(fù)性較好,特征性及專屬性較強(qiáng),可以為山豆根和北豆根的鑒別提供思路,從而避免因臨床混用導(dǎo)致的藥物中毒事件的發(fā)生。(2)結(jié)果表明,不同產(chǎn)地四種生物堿含量差異顯著,道地產(chǎn)區(qū)有效成分含量相對(duì)較高�？鄥A和氧化苦參堿總量大于1.00%的產(chǎn)地大部分為廣西,與廣西為山豆根的道地產(chǎn)區(qū)這一事實(shí)相符合,且苦參堿與氧苦參堿的含量呈現(xiàn)"此消彼長";聚類分析結(jié)果表明,不同產(chǎn)地對(duì)山豆根生物堿的含量影響較大,不同分組的產(chǎn)地區(qū)分不夠明顯,可能是由于產(chǎn)地?cái)?shù)量有限的原因?qū)е?提示應(yīng)該增加樣本的產(chǎn)地、批次以獲取更為準(zhǔn)確客觀的研究結(jié)果。(3)最終推斷結(jié)果為進(jìn)一步分析山豆根化學(xué)成分提供了參考思路,但是推斷結(jié)果需要進(jìn)一步驗(yàn)證。
[Abstract]:Research purposes: tonkinensis is commonly used in clinical medicine, in recent years on the Rrst in clinical use in poisoning have repeatedly reported that one of the reasons is Shandougen and toxicity big small Beidougen mix, resulting in poisoning. At present, the quality standard of radix sophorae tonkinensis is still a lack of systematic aspects of the study. The study of fingerprint by Shandougen, determination of active ingredients, combined with component analysis of high resolution mass spectrometry, to provide reference and ideas for the improvement of sophoratonkinensis supplement the existing quality standards. Research methods: (1) research by UPLC-PDA of Shandougen 70% methanol extracts were part of the fingerprint analysis, the CDF the format of the file into the A software version > < chromatographic fingerprint evaluation system published by the State Pharmacopoeia Commission analysis, fingerprint generation sophoratonkinensis common mode, there are The peak and similarity. And specify Oxymatrine as the reference peak, through the calculation of other common peak difference of relative retention time and relative peak area of different origin of sophoratonkinensis evaluation. (2) to study the optimum extraction condition was investigated by single factor extraction method of radix sophorae tonkinensis initially identified Shandougen (including the different methods, different solvents, different time), and then investigated by HPLC-PDA chromatographic conditions for samples of matrine, Oxymatrine, sophocarpine, Oxysophocarpine and separation of four kinds of alkaloids, the final quantity, and then the final results using SAS 8.2 statistical analysis software for cluster analysis, the mountain according to the origin of root is divided into three categories, realize the evaluation of differences of different origin Shandougen. (3) through the study of UPLC-Q-TOF/MS on real estate areas of Rrst composition and analysis, the data through the Waters company supporting software Matching analysis of intelligent Unify, and ultimately determine the Rrst may contain ingredients in. Results: (1) the 13 batch of Rrst containing 27 common peaks were identified, of which 2 are respectively of matrine and Oxymatrine; different batches of Shandougen common peak relative retention time in 3.925% ~ 4.588%, while the RSD of the relative peak area is larger, and the 13 batch of similarity Shandougen most of more than 0.9, but the 2 batch of rhizomamenispermi similarity is poor. (2) the total content of the 13 batch of Rrst in 12 batches of matrine and oxymatrine to reach the standard of Chinese Pharmacopoeia (more than 0.7%), 1 group was lower than the standard of Pharmacopoeia, and 13 samples in accordance with matrine, Oxymatrine, sophocarpine, Oxysophocarpine contents can be divided into three categories. (3) by Unify software, intelligent, and combined with the characteristic fragment ions in comparingliterature, infer 56 contain tonkinensis in . conclusions: (1) in the study of different origin Shandougen good similarity in chemical composition, the precision, stability and repeatability, characteristic and specificity is strong, can provide ideas for the identification of Rrst and Beidougen, so as to avoid the drug caused by clinical mix poisoning (2). The results show that the difference of four kinds of alkaloid content in different areas significantly, the content of effective components of real estate areas is relatively high. Matrine and Oxymatrine is greater than 1% of the total area most of the Guangxi, and Guangxi for the fact that the real estate areas of Rrst accord and the content of matrine and oxygen matrine showed a "shift"; cluster analysis showed that the effect of alkaloid content in different areas of Rrst larger, different groups of origin differentiation is not obvious, which may be due to the limited number of places,. Should increase the sample from batch to obtain more accurate and objective results. (3) the final inference results provide a reference for the further analysis of Rrst chemical composition, but the inference results need to be further verified.

【學(xué)位授予單位】：北京中醫(yī)藥大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：R284.1

【參考文獻(xiàn)】

相關(guān)期刊論文 前10條

1 王美玲;張清清;付爽;劉月紅;梁釧鐳;陳娜;丁永勝;王海麗;瞿曉梅;趙保勝;高曉燕;;UPLC-Q-TOF MS~E技術(shù)結(jié)合UNIFI數(shù)據(jù)庫篩查方法快速分析巴戟天化學(xué)成分[J];質(zhì)譜學(xué)報(bào);2017年01期

2 韓馥蔓;王莉鑫;陳影;陳兩綿;馮偉紅;王錦玉;劉德文;游云;仝燕;;HPLC同時(shí)測(cè)定山豆根中7種生物堿及3種黃酮的含量[J];中國中藥雜志;2016年24期

3 李偉;馮育林;黎田兒;吳歡;李艷;鐘國躍;吳蓓;何明珍;;UPLC-Q-TOF/MS技術(shù)結(jié)合診斷離子方法快速分析連錢草中黃酮類化合物[J];質(zhì)譜學(xué)報(bào);2016年06期

4 田婷婷;馬英華;解偉偉;靳怡然;許慧君;張?zhí)m桐;杜英峰;;LC-MS/MS同時(shí)測(cè)定藍(lán)萼香菜中4種二萜類成分及其聚類分析[J];中國中藥雜志;2016年02期

5 孫旭;高媛;吳洋;王莉;劉云云;姚麗敏;陳瑤;;復(fù)方山豆根合劑質(zhì)量標(biāo)準(zhǔn)的研究[J];解放軍藥學(xué)學(xué)報(bào);2015年06期

6 趙慶華;謝元璋;李素君;楊倩;孫蓉;;山豆根水提組分對(duì)咽喉實(shí)熱證小鼠急性毒性實(shí)驗(yàn)研究[J];中國藥物警戒;2015年02期

7 李自紅;魏悅;范毅;朱杰;趙天增;;蘆丁的電噴霧離子阱質(zhì)譜分析[J];分析試驗(yàn)室;2015年02期

8 陸國壽;葉勇;盧文杰;黃周鋒;曾繁強(qiáng);;多葉越南槐中苦參堿與氧化苦參堿的分離鑒定及含量測(cè)定研究[J];廣西醫(yī)學(xué);2014年08期

9 鄒恒偉;;山豆根的研究進(jìn)展與趨向[J];廣西農(nóng)學(xué)報(bào);2014年03期

10 劉芷;賈英;趙旭;張晨寧;吳博;畢開順;;五味子的UPLC指紋圖譜研究[J];中草藥;2014年11期

，

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