比卡魯胺的質(zhì)量標(biāo)準(zhǔn)

制藥工程論文編號(hào):ZY025    論文字?jǐn)?shù):10729,頁(yè)數(shù):25

目錄
中文摘要 I
英文摘要 II
目錄 III
1． 緒 論 1
 1．1  選題的目的及意義 1
 1．2  選題的背景 1
 1．3  國(guó)內(nèi)外文獻(xiàn)綜述 1
 1．4  主要研究?jī)?nèi)容 2
2． 實(shí)驗(yàn)部分 3
 2．1  實(shí)驗(yàn)儀器與試劑 3
 2．2  實(shí)驗(yàn)步驟 3
3． 結(jié)果與討論 8
 3．1  性狀結(jié)果 8
 3．2  鑒別結(jié)果 8
 3．3  檢查結(jié)果 10
 3．4  含量測(cè)定結(jié)果 14
4． 總結(jié)和展望 17
 4．1  總結(jié) 17
 4．2  展望 19
致  謝 20
參考文獻(xiàn) 21

摘 要：本論文建立比卡魯胺的質(zhì)量標(biāo)準(zhǔn)。通過(guò)實(shí)驗(yàn)我們確定的含量測(cè)定方法如下：Alltima柱子（150×4.6mm，5μ，Alltech），流動(dòng)相為乙腈-水（47：53），流速是1.0mL/min，檢測(cè)波長(zhǎng)為270nm，進(jìn)樣體積為20μL。此法簡(jiǎn)便、準(zhǔn)確、具專屬性和良好的重現(xiàn)性，可用于該藥物的質(zhì)量控制。在有關(guān)物質(zhì)檢測(cè)項(xiàng)下的破壞性實(shí)驗(yàn)中，本品經(jīng)過(guò)酸、堿、氧化、熱降解及光照破壞后，產(chǎn)生的雜質(zhì)峰能與主峰分離，說(shuō)明該色譜系統(tǒng)能有效分離檢測(cè)降解產(chǎn)物。在有機(jī)溶劑殘留量測(cè)定項(xiàng)下，利用氣相色譜頂空進(jìn)樣法檢查乙醇、三氯乙烷、乙醚、二氯甲烷、四氫呋喃、甲苯、氯仿、乙酸乙酯、石油醚、二甲基甲酰胺和二甲基乙酰胺的殘留量，DMF為溶劑，進(jìn)樣瓶在80℃下平衡30min，HP-5（0.32mm×30m×0.22μm）毛細(xì)管柱，進(jìn)樣口溫度200℃，F(xiàn)ID檢測(cè)器溫度200℃，柱溫50℃。我們依據(jù)中國(guó)藥典各項(xiàng)標(biāo)準(zhǔn)進(jìn)行分析，最終以藥典的形式寫(xiě)出各項(xiàng)目規(guī)范。
關(guān)鍵詞：比卡魯胺；質(zhì)量標(biāo)準(zhǔn)；雜質(zhì)檢查；含量測(cè)定

Abstract：In this article we established the quality control standard of Bicalutamide. The methods of content determination which we have adopted were as follows: Alltima column（150×4.6mm，5μ，Alltech）,and the mobile phase consisted of a mixture of acetonitrile and water buffer solution (47:53) pumped at a flow rate of 1.0mL/min. The detection wavelength was 270nm. The methods of content determination was simple，specific and accurate. It can be used for the quality control of Bicalutamide. In destroying experiments of related substance measure item, the samples were destroyed by acid, alkali, oxidation, heating and illumination. The related substance can be separated from Bicalutamide, which showed this chromatographic system being effective. In organic residual solvents measure item, we used headspace GC chromatography to examine ethanol, trichloroethane, aether, dichloromethane, tetrahydrofuran, toluene, chloroform, ethyl acetate, petroleun ether, DMF and DMAC residue in Bicalutamide. DMF was used as solution. Sample had been equilibrated at 80℃ for 30min. HP-5（0.32mm×30m×0.22μm）capillary column was used. The temperature of injector, FID and column were 200℃., 200℃.and 50℃ respectively. We have done other experiments according to Chinese Pharmacopoeia. Finally, we have written quality standard of Bicalutamide in Chinese Pharmacopoeia’s formats.
Keywords：Bicalutamide; Quality standard; Test of impurities；Quality control