蒙藥清血八味片質(zhì)量控制方法研究
發(fā)布時(shí)間：2018-08-20 11:40
【摘要】：目的蒙藥清血八味片由寒水石(涼制)、紫草、土木香、人工牛黃、梔子、瞿麥、石膏、甘草等八味藥材組成,為蒙醫(yī)臨床常用驗(yàn)方,在治療血病方面療效顯著。清血八味片的物質(zhì)基礎(chǔ)研究薄弱,現(xiàn)有質(zhì)量標(biāo)準(zhǔn)很不完善,亟需提高質(zhì)量控制水平。本課題擬建立清血八味片的指紋圖譜,對(duì)清血八味片中多指標(biāo)性成分進(jìn)行含量測(cè)定方法研究,定性定量分析清血八味片所含無(wú)機(jī)元素,實(shí)現(xiàn)對(duì)清血八味片多方面的質(zhì)量控制方法研究,從而更加全面的控制產(chǎn)品質(zhì)量。方法1.利用HPLC-PDA技術(shù)建立清血八味片的指紋圖譜,將18批清血八味片樣品色譜圖采用相似度軟件進(jìn)行處理,對(duì)建立的指紋圖譜及其各項(xiàng)技術(shù)參數(shù)進(jìn)行分析。利用各單味藥材譜圖對(duì)清血八味片中共有峰進(jìn)行歸屬,通過(guò)已有對(duì)照品進(jìn)行部分特征峰的指認(rèn)。2.以硝酸加過(guò)氧化氫體系為消解試劑,供試品經(jīng)微波消解后,采用電感耦合等離子體質(zhì)譜(ICP-MS)法測(cè)定清血八味片中 Be、B、Na、Mg、Al、P、K、Ca、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、As、Se、Rb、Sr、Mo、Ag、Cd、Sn、Sb、Cs、Ba、Hg、Tl、Pb共32種無(wú)機(jī)元素的含量,繪制無(wú)機(jī)元素含量分布曲線建立清血八味片無(wú)機(jī)元素指紋譜,用SPSS 19.0軟件對(duì)數(shù)據(jù)進(jìn)行主成分分析并篩選主要特征元素。3.由于寒水石及石膏主成分相同,故對(duì)兩者所含鈣總量進(jìn)行測(cè)定。通過(guò)理化鑒別試驗(yàn)進(jìn)行清血八味片的鈣鹽與硫酸鹽的鑒別反應(yīng);對(duì)清血八味片的樣品處理?xiàng)l件進(jìn)行合理優(yōu)化,并對(duì)測(cè)定方法進(jìn)行考察;將樣品經(jīng)炭化后灰化,采用乙二胺四乙酸二鈉(EDTA-2Na)絡(luò)合滴定法對(duì)清血八味片中鈣成分進(jìn)行含量測(cè)定。4.選擇清血八味片中主要活性成分京尼平龍膽二糖苷、梔子苷、甘草苷、甘草酸、異土木香內(nèi)酯和土木香內(nèi)酯作為指標(biāo)性成分,通過(guò)單因素考察選擇最佳供試品提取方法,并對(duì)色譜檢測(cè)條件進(jìn)行優(yōu)化,利用高效液相色譜法同時(shí)測(cè)定18批樣品中6個(gè)指標(biāo)性成分的含量。結(jié)果1.清血八味片HPLC色譜圖中各成分得到了良好分離,確定了 21個(gè)共有指紋峰,初步闡明了共有峰來(lái)源并定性了部分色譜峰。將18批次樣品色譜圖與生成的對(duì)照指紋圖譜進(jìn)行匹配,平均相似度為0.974,RSD為1.54%,表明18批樣品生成的圖譜的相似度較高,差異較小。所建立的指紋圖譜方法可行性較好。2.ICP-MS法測(cè)定的32種無(wú)機(jī)元素線性關(guān)系良好,相關(guān)系數(shù)r ≥ 0.9995,各元素的檢測(cè)限在 0.001～6.390 μg/L,加樣回收率為 94.36%～105.47%,RSD 為 1.53%～4.56%。通過(guò)無(wú)機(jī)元素含量分布曲線分析建立了清血八味片的無(wú)機(jī)元素指紋譜,不同批次的樣品均有相似的峰形,且不同無(wú)機(jī)元素含量的多寡順序趨于一致。經(jīng)主成分分析篩選出清血八味片主要特征無(wú)機(jī)元素為 Co、As、Ba、Ca、Sb、Ti、Ni、Fe、Cs、Se、P、Al、K。測(cè)定的樣品中檢測(cè)出Pb、Cd、As、Hg、Cu,5種重金屬元素的含量均低于《中國(guó)藥典》2015版的限度要求。3.采用絡(luò)合滴定法測(cè)定清血八味片中鈣含量,樣品最佳處理?xiàng)l件是將樣品在調(diào)壓電爐上炭化1 h至炭化完全后,置于馬弗爐中在700～800℃下灰化6 h。測(cè)定方法的重復(fù)性試驗(yàn)RSD為0.32%,加樣回收率為98.67%～101.25%,RSD為0.97%,均滿足定量分析的要求。4.采用HPLC法測(cè)定清血八味片中京尼平龍膽二糖苷、梔子苷、甘草苷、甘草酸、異土木香內(nèi)酯和土木香內(nèi)酯等被測(cè)組分均達(dá)到基線分離,在一定濃度范圍內(nèi)6種成分的線性關(guān)系良好,相關(guān)系數(shù)r≥0.9998,精密度、重復(fù)性、穩(wěn)定性、加樣回收率等內(nèi)容均符合定量分析要求。18批樣品的6種成分含量較穩(wěn)定,無(wú)顯著性差異。結(jié)論本課題通過(guò)對(duì)蒙藥清血八味片進(jìn)行指紋圖譜、無(wú)機(jī)元素分析、多成分含量測(cè)定的研究,為該產(chǎn)品質(zhì)量標(biāo)準(zhǔn)的提升和產(chǎn)品質(zhì)量的全面控制提供技術(shù)參考,為該蒙成藥的生產(chǎn)加工、市場(chǎng)流通、藥效物質(zhì)基礎(chǔ)研究、臨床應(yīng)用等提供科學(xué)依據(jù)。
[Abstract]:OBJECTIVE Qingxue Bawei tablets are composed of eight kinds of medicinal materials, such as cold water stone, Shikong grass, earthwood fragrance, artificial bezoar, Gardenia jasminoides, Trichosanthes, gypsum and liquorice. It is a common prescription in Mongolian medicine and has remarkable curative effect in treating blood diseases. To establish the fingerprint of Qingxue Bawei Tablets, to study the content determination method of multi-index components in Qingxue Bawei Tablets, to analyze the inorganic elements in Qingxue Bawei Tablets qualitatively and quantitatively, and to study the quality control method of Qingxue Bawei Tablets in many aspects, so as to control the quality of products more comprehensively. Methods 1. Using HPLC-PDA technology. The fingerprint of Qingxuebaobawei tablets was established. The chromatograms of 18 batches of Qingxuebaobawei tablets were processed by similarity software. The fingerprint and its technical parameters were analyzed. Nitric acid plus hydrogen peroxide system was used as digestion reagent. After microwave digestion, the contents of Be, B, Na, Mg, Al, P, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Mo, Ag, Cd, Sn, Sb, Cs, Ba, Hg, Tl and Pb in Qingxue Bawei tablets were determined by inductively coupled plasma mass spectrometry (ICP-MS). To establish the fingerprint spectrum of inorganic elements in Qingxue Bawei Tablets, principal component analysis and screening of main characteristic elements were carried out with SPSS 19.0 software. After carbonization and ashing, the content of calcium in Qingxue Bawei tablets was determined by EDTA-2Na complexometric titration. 4. Geniposide, geniposide, glycyrrhizin were selected as the main active components in Qingxue Bawei tablets. Glycyrrhizic acid, iso-tufa lactone and tufa lactone were used as index components, and the best extraction method was selected by single factor investigation. The chromatographic detection conditions were optimized. The content of 6 index components in 18 batches of samples was determined by high performance liquid chromatography. Results 1. The components in the HPLC chromatogram of Qingxuebaobawei tablets were obtained. Twenty-one common fingerprint peaks were identified by good separation, and the source of common peaks was elucidated preliminarily. The fingerprint of 18 batches of samples were matched with the corresponding fingerprints with an average similarity of 0.974 and RSD of 1.54%. The results showed that the similarity of the fingerprints produced by 18 batches of samples was high and the difference was small. The correlation coefficient R (> 0.9995), the detection limit of each element is 0.001-6.390 ug/L, the recovery is 94.36%-105.47%, RSD is 1.53%-4.56%. The fingerprint spectrum of inorganic elements in Qingxuebaobawei tablets is established by analyzing the content distribution curve of inorganic elements. The main characteristic inorganic elements of Qingxuebai Bawei tablets were Co, As, Ba, Ca, Sb, Ti, Ni, Fe, Cs, Se, P, Al, K. The contents of Pb, Cd, As, Hg, Cu and 5 heavy metal elements were lower than those in the Chinese Pharmacopoeia > 2015. Calcium content in Qingxue Bawei tablets was determined by complexometric titration. The optimum conditions for sample treatment were carbonization for 1 h in a pressure regulating furnace and ashing for 6 h in a muffle furnace at 700-800 C. The repeatability test RSD of the method was 0.32%. The recovery of sample addition was 98.67%-101.25% and RSD was 0.97%. Quantitative analysis of Geniposide, Geniposide, Geniposide, Glycyrrhizin, Glycyrrhizic acid, Isoamylactone and Cinnamolide in Qingxuebai Bawei Tablets were determined by HPLC. The six components were separated at baseline. The linear relationship of the six components was good within a certain concentration range. The correlation coefficient R (>0.9998), precision, repeatability and stability were obtained. The contents of six components in 18 batches of samples were stable, and there was no significant difference between them.Conclusion The research on fingerprint, inorganic element analysis and multi-component content determination of Mongolian medicine Qingxue Bawei tablets can provide a reference for the improvement of product quality standard and the overall control of product quality. Technical reference will provide scientific basis for the production, processing, market circulation, basic research of pharmacodynamic substances and clinical application of the Mongolian patent medicine.
【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)】：R29
本文編號(hào)：2193472
[Abstract]:OBJECTIVE Qingxue Bawei tablets are composed of eight kinds of medicinal materials, such as cold water stone, Shikong grass, earthwood fragrance, artificial bezoar, Gardenia jasminoides, Trichosanthes, gypsum and liquorice. It is a common prescription in Mongolian medicine and has remarkable curative effect in treating blood diseases. To establish the fingerprint of Qingxue Bawei Tablets, to study the content determination method of multi-index components in Qingxue Bawei Tablets, to analyze the inorganic elements in Qingxue Bawei Tablets qualitatively and quantitatively, and to study the quality control method of Qingxue Bawei Tablets in many aspects, so as to control the quality of products more comprehensively. Methods 1. Using HPLC-PDA technology. The fingerprint of Qingxuebaobawei tablets was established. The chromatograms of 18 batches of Qingxuebaobawei tablets were processed by similarity software. The fingerprint and its technical parameters were analyzed. Nitric acid plus hydrogen peroxide system was used as digestion reagent. After microwave digestion, the contents of Be, B, Na, Mg, Al, P, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Mo, Ag, Cd, Sn, Sb, Cs, Ba, Hg, Tl and Pb in Qingxue Bawei tablets were determined by inductively coupled plasma mass spectrometry (ICP-MS). To establish the fingerprint spectrum of inorganic elements in Qingxue Bawei Tablets, principal component analysis and screening of main characteristic elements were carried out with SPSS 19.0 software. After carbonization and ashing, the content of calcium in Qingxue Bawei tablets was determined by EDTA-2Na complexometric titration. 4. Geniposide, geniposide, glycyrrhizin were selected as the main active components in Qingxue Bawei tablets. Glycyrrhizic acid, iso-tufa lactone and tufa lactone were used as index components, and the best extraction method was selected by single factor investigation. The chromatographic detection conditions were optimized. The content of 6 index components in 18 batches of samples was determined by high performance liquid chromatography. Results 1. The components in the HPLC chromatogram of Qingxuebaobawei tablets were obtained. Twenty-one common fingerprint peaks were identified by good separation, and the source of common peaks was elucidated preliminarily. The fingerprint of 18 batches of samples were matched with the corresponding fingerprints with an average similarity of 0.974 and RSD of 1.54%. The results showed that the similarity of the fingerprints produced by 18 batches of samples was high and the difference was small. The correlation coefficient R (> 0.9995), the detection limit of each element is 0.001-6.390 ug/L, the recovery is 94.36%-105.47%, RSD is 1.53%-4.56%. The fingerprint spectrum of inorganic elements in Qingxuebaobawei tablets is established by analyzing the content distribution curve of inorganic elements. The main characteristic inorganic elements of Qingxuebai Bawei tablets were Co, As, Ba, Ca, Sb, Ti, Ni, Fe, Cs, Se, P, Al, K. The contents of Pb, Cd, As, Hg, Cu and 5 heavy metal elements were lower than those in the Chinese Pharmacopoeia > 2015. Calcium content in Qingxue Bawei tablets was determined by complexometric titration. The optimum conditions for sample treatment were carbonization for 1 h in a pressure regulating furnace and ashing for 6 h in a muffle furnace at 700-800 C. The repeatability test RSD of the method was 0.32%. The recovery of sample addition was 98.67%-101.25% and RSD was 0.97%. Quantitative analysis of Geniposide, Geniposide, Geniposide, Glycyrrhizin, Glycyrrhizic acid, Isoamylactone and Cinnamolide in Qingxuebai Bawei Tablets were determined by HPLC. The six components were separated at baseline. The linear relationship of the six components was good within a certain concentration range. The correlation coefficient R (>0.9998), precision, repeatability and stability were obtained. The contents of six components in 18 batches of samples were stable, and there was no significant difference between them.Conclusion The research on fingerprint, inorganic element analysis and multi-component content determination of Mongolian medicine Qingxue Bawei tablets can provide a reference for the improvement of product quality standard and the overall control of product quality. Technical reference will provide scientific basis for the production, processing, market circulation, basic research of pharmacodynamic substances and clinical application of the Mongolian patent medicine.
【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)】：R29
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