本文選題：核磁共振波譜法　切入點(diǎn)：b型流感嗜血桿菌多糖　出處：《中國(guó)生物制品學(xué)雜志》2014年08期

【摘要】：目的建立核磁共振波譜(nuclear magnetic resonance,NMR)法測(cè)定b型流感嗜血桿菌(Haemophilus influenzae type b,Hib)莢膜多糖中核糖含量的方法。方法利用NMR技術(shù)中的氫核磁共振波譜(1H-NMR)的定量功能,對(duì)不同濃度的D-核糖進(jìn)行定量分析,驗(yàn)證該方法的精密度及準(zhǔn)確度,并與傳統(tǒng)化學(xué)方法進(jìn)行比較。結(jié)果 NMR法定量結(jié)果相對(duì)標(biāo)準(zhǔn)偏差(RSD)均小于1.0%,相對(duì)誤差除最低濃度20 mmol/L為7.4%外,其余濃度均在1%~3%之間,不同濃度的樣品回收率在97.2%~107%之間;化學(xué)法定量結(jié)果 RSD在0.6%~7.9%之間,相對(duì)誤差在3%~6.5%之間,不同濃度樣品回收率在93.5%~105.3%之間;兩種方法檢測(cè)的3批Hib莢膜多糖中核糖含量無(wú)明顯差別,均在《中國(guó)藥典》三部(2010版)規(guī)定的320~410 mg/g之間。結(jié)論 1H-NMR定量方法取樣少,可直接定量,該方法精密度高、準(zhǔn)確度高、重現(xiàn)性好,且不破壞多糖結(jié)構(gòu),可應(yīng)用于細(xì)菌莢膜多糖質(zhì)量控制的核糖定量。
[Abstract]:Objective to establish a method for the determination of ribose in Haemophilus influenzae type bhib capsule polysaccharides by nuclear magnetic resonance spectroscopy (NMR).Methods using the quantitative function of 1H-NMRs in NMR, quantitative analysis of different concentrations of D-ribose was carried out. The precision and accuracy of the method were verified and compared with the traditional chemical method.Results the relative standard deviation (RSD) of NMR was less than 1.0. The relative error was between 1.0% and 7.4%, except the lowest concentration of 20 mmol/L was 7.4%. The recoveries of samples of different concentrations were between 97.2% and 10.7%, and the relative errors were between 0.6% and 7.9% by chemical method.The relative error was between 6.5% and 93.5%, and the recoveries of samples with different concentrations were between 93.5% and 105.3%. There was no significant difference in the contents of ribose in the three batches of Hib capsule polysaccharides detected by the two methods, both of which were in the range of 320,410 mg/g as stipulated in the Chinese Pharmacopoeia, three parts of Chinese Pharmacopoeia and three parts of Chinese Pharmacopoeia.Conclusion 1H-NMR quantitative method can be used in the quality control of bacterial capsule polysaccharides because of its high precision, high accuracy, good reproducibility and no damage to the structure of polysaccharides.
【作者單位】： 昆明醫(yī)科大學(xué);中國(guó)醫(yī)學(xué)科學(xué)院北京協(xié)和醫(yī)學(xué)院醫(yī)學(xué)生物學(xué)研究所;
【基金】：國(guó)家國(guó)際科技合作項(xiàng)目(2010DFB32890) Bill & Melinda Gates foundation(OPP1049425)
【分類(lèi)號(hào)】：R378;O657.61

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