目的建立测定4种盐酸莫西沙星杂质A、B、C、D对照品含量的定量核磁共振氢谱法(quantitative proton nuclear magnetic resonance,qHNMR)。方法采用核磁共振波谱仪采集4种盐酸莫西沙星杂质对照品的一维定量氢谱(^(1)H-NMR),以1,3,5-三甲...目的建立测定4种盐酸莫西沙星杂质A、B、C、D对照品含量的定量核磁共振氢谱法(quantitative proton nuclear magnetic resonance,qHNMR)。方法采用核磁共振波谱仪采集4种盐酸莫西沙星杂质对照品的一维定量氢谱(^(1)H-NMR),以1,3,5-三甲氧基苯作为内标物,氘代二甲亚砜(DMSO-d6)或氘代氯仿(CDCl_(3))作为溶剂,脉冲程序为noesyigld1d,扫描次数(NS)为32次,弛豫延迟时间(D1)为30 s,测试温度为25℃,对4种盐酸莫西沙星杂质对照品进行定量研究。结果4种盐酸莫西沙星杂质对照品定量峰和1,3,5-三甲氧基苯定量峰信号在核磁共振氢谱上分离度良好,在线性范围内线性关系良好(r^(2)>0.9994),进样精密度和重复性良好。qHNMR法测定含量结果与质量平衡法测定含量结果基本一致。结论建立的qHNMR法准确可靠、简便快速,为该类杂质含量测定提供了新的方法,也可作为该类化学对照品采用质量平衡法定值结果的验证方法。展开更多
目的:建立一种测定6B,10A,17F,19A,19F及20型肺炎链球菌荚膜多糖含量的定量核磁共振氢谱(1H-NMR)法。方法:以二甲基砜为内标物采用Bruker Avance-600型核磁共振波谱仪,设置检测条件,建立定量1H-NMR法用于供试品溶液的测定。结果:获得各...目的:建立一种测定6B,10A,17F,19A,19F及20型肺炎链球菌荚膜多糖含量的定量核磁共振氢谱(1H-NMR)法。方法:以二甲基砜为内标物采用Bruker Avance-600型核磁共振波谱仪,设置检测条件,建立定量1H-NMR法用于供试品溶液的测定。结果:获得各型多糖的1H-NMR谱图,确定用于定量的特征峰。通过比较各型多糖特征峰的峰面积与内标物特征峰的峰面积,计算得到6B,10A,17F,19A,19F及20型肺炎链球菌荚膜多糖含量依次为92.57%,88.56%,84.95%,82.92%,83.98%和85.80%,计算各组数据的相对标准偏差(relative standard deviation,RSD)值依次为0.29%,0.47%,0.48%,0.13%,0.38%和0.22%。结论:本研究建立的测定肺炎链球菌荚膜多糖含量的定量1H-NMR法,从样品制备到采样参数设置以及数据处理,操作简单,可行性高,重复性好,更能够满足检定工作的需求,可作为肺炎球菌荚膜多糖质量控制的一种合理、有效的技术手段。展开更多
建立基于定量核磁共振氢谱(quantitative proton nuclear magnetic resonance,qHNMR)的神曲中葡萄糖含量的测定方法,对市售神曲中葡萄糖的含量进行分析,并探究神曲加工炮制过程中葡萄糖含量的变化规律。以重水为溶剂,2,2,2,3-d4-3-(三...建立基于定量核磁共振氢谱(quantitative proton nuclear magnetic resonance,qHNMR)的神曲中葡萄糖含量的测定方法,对市售神曲中葡萄糖的含量进行分析,并探究神曲加工炮制过程中葡萄糖含量的变化规律。以重水为溶剂,2,2,2,3-d4-3-(三甲基硅基)丙酸钠盐为内标,以化学位移δ4.65、5.24处葡萄糖端基质子双峰信号作为定量峰,对神曲中葡萄糖含量进行定量。经方法学评价,葡萄糖在0.10~6.44 mg·mL-1呈现良好的线性关系,精密度、稳定性、重复性和加样回收率试验的RSD均小于2.3%。市售神曲中葡萄糖含量波动明显,推测与神曲的发酵天数、麸面比及炮制方式等有关。神曲中葡萄糖含量随发酵天数增加呈先增加后降低的趋势;全麦麸或全面粉发酵的神曲中葡萄糖含量明显低于麦麸和面粉混合发酵的神曲;麸炒神曲较生神曲葡萄糖含量略有降低,而焦神曲中葡萄糖含量显著降低。该实验建立的qHNMR方法简单快捷,准确度高,为神曲中葡萄糖含量测定提供了新的方法。此外,该研究阐明了神曲加工炮制过程中葡萄糖的量变规律,对判断神曲发酵程度具有指示意义,为揭示神曲的发酵机制,完善神曲的质量控制方法提供了科学依据。展开更多
Cynanchum paniculatum(Bunge) Kitagawa is usually used as an herbal medicine for treating many diseases. Paeonol is the main active component, and its content is the key indicator for quality control of C. paniculatum....Cynanchum paniculatum(Bunge) Kitagawa is usually used as an herbal medicine for treating many diseases. Paeonol is the main active component, and its content is the key indicator for quality control of C. paniculatum. In the present study, we developed a rapid, accurate and precise method for quantitation of paeonol in C. paniculatum using 1 H NMR spectra. The deuterated solvent of methanol-d4 enabled satisfactory separation of the signals to be integrated in 1 H NMR spectrum. H-6(δ 7.78) of 1 H NMR spectrum of C. paniculatum was selected as the feature signal for quantitation, and trimesic acid(TMA) was selected as an internal standard. Validation of the quantitative method was performed in terms of linearity, specificity, repeatability and stability. This is the first time to report quantitative 1 H NMR(qHNMR) applied to determine the content of paeonol in C. paniculatum and showed a wider linearity range than the reported quantitation of paeonol in others. The simple extraction of paeonol from C. paniculatum was rapid and will prompt the application of the developed method. This work implied that qHNMR represented a feasible alternative to HPLC-based methods for quantitation of paeonol in C. paniculatum, and it was suitable for the quality control of C. paniculatum.展开更多
利用六西格玛设计(design for six Sigma,DFSS)方法,通过定量核磁共振碳谱(quantitative carbon nuclear magnetic resonance spectroscopy,^(13)C qNMR)对由11种已知烃类化合物组成的模型油品进行了芳香碳摩尔百分比[C(ar)%,简称芳碳率...利用六西格玛设计(design for six Sigma,DFSS)方法,通过定量核磁共振碳谱(quantitative carbon nuclear magnetic resonance spectroscopy,^(13)C qNMR)对由11种已知烃类化合物组成的模型油品进行了芳香碳摩尔百分比[C(ar)%,简称芳碳率]测定的系统研究,建立了C(ar)%与样品浓度Conc.、弛豫试剂浓度[Cr(acac)_3]和循环延迟D13个参数之间的数学模型,据此模型得到了优化的参数设置:Conc.为180mg/mL,[Cr(acac)_3]为12 mg/mL,D1为10.5 s.按此设置进行了8组验证实验,其结果重现性较好,相对标准偏差(relative standard deviation,RSD)为0.61%;准确性较高,达到99.0%~100.6%.该方法也可用于其它分析测试方法的系统研究,且实验结果对现行油品芳碳率测定标准中相关参数,如[Cr(acac)_3]和D1的设置能够提出补充性建议.展开更多
文摘目的:建立一种测定6B,10A,17F,19A,19F及20型肺炎链球菌荚膜多糖含量的定量核磁共振氢谱(1H-NMR)法。方法:以二甲基砜为内标物采用Bruker Avance-600型核磁共振波谱仪,设置检测条件,建立定量1H-NMR法用于供试品溶液的测定。结果:获得各型多糖的1H-NMR谱图,确定用于定量的特征峰。通过比较各型多糖特征峰的峰面积与内标物特征峰的峰面积,计算得到6B,10A,17F,19A,19F及20型肺炎链球菌荚膜多糖含量依次为92.57%,88.56%,84.95%,82.92%,83.98%和85.80%,计算各组数据的相对标准偏差(relative standard deviation,RSD)值依次为0.29%,0.47%,0.48%,0.13%,0.38%和0.22%。结论:本研究建立的测定肺炎链球菌荚膜多糖含量的定量1H-NMR法,从样品制备到采样参数设置以及数据处理,操作简单,可行性高,重复性好,更能够满足检定工作的需求,可作为肺炎球菌荚膜多糖质量控制的一种合理、有效的技术手段。
基金Science and Technology Project of Yunnan Provincial Department of Science and Technology(Grant No.2018FD081)Yunnan Local Colleges Applied Basic Research Projects[Grant Nos.2019FH001-(109),2017FH001-092,2017FH001-094 and 2018FH001-019]Youth Research Foundation of Qujing Normal University in 2019(Grant No.2019QN004)。
文摘Cynanchum paniculatum(Bunge) Kitagawa is usually used as an herbal medicine for treating many diseases. Paeonol is the main active component, and its content is the key indicator for quality control of C. paniculatum. In the present study, we developed a rapid, accurate and precise method for quantitation of paeonol in C. paniculatum using 1 H NMR spectra. The deuterated solvent of methanol-d4 enabled satisfactory separation of the signals to be integrated in 1 H NMR spectrum. H-6(δ 7.78) of 1 H NMR spectrum of C. paniculatum was selected as the feature signal for quantitation, and trimesic acid(TMA) was selected as an internal standard. Validation of the quantitative method was performed in terms of linearity, specificity, repeatability and stability. This is the first time to report quantitative 1 H NMR(qHNMR) applied to determine the content of paeonol in C. paniculatum and showed a wider linearity range than the reported quantitation of paeonol in others. The simple extraction of paeonol from C. paniculatum was rapid and will prompt the application of the developed method. This work implied that qHNMR represented a feasible alternative to HPLC-based methods for quantitation of paeonol in C. paniculatum, and it was suitable for the quality control of C. paniculatum.
文摘利用六西格玛设计(design for six Sigma,DFSS)方法,通过定量核磁共振碳谱(quantitative carbon nuclear magnetic resonance spectroscopy,^(13)C qNMR)对由11种已知烃类化合物组成的模型油品进行了芳香碳摩尔百分比[C(ar)%,简称芳碳率]测定的系统研究,建立了C(ar)%与样品浓度Conc.、弛豫试剂浓度[Cr(acac)_3]和循环延迟D13个参数之间的数学模型,据此模型得到了优化的参数设置:Conc.为180mg/mL,[Cr(acac)_3]为12 mg/mL,D1为10.5 s.按此设置进行了8组验证实验,其结果重现性较好,相对标准偏差(relative standard deviation,RSD)为0.61%;准确性较高,达到99.0%~100.6%.该方法也可用于其它分析测试方法的系统研究,且实验结果对现行油品芳碳率测定标准中相关参数,如[Cr(acac)_3]和D1的设置能够提出补充性建议.
文摘采用定量核磁共振法(qNMR)测定甲磺酸伊马替尼原料质量分数。采用Bruker AVANCEⅢ600 MHz核磁共振波谱仪测定核磁共振氢谱,对甲磺酸伊马替尼原料进行质量分数测定,并与高效液相色谱法测定结果相比较。当m(甲磺酸伊马替尼)∶m(马来酸)为0.92~5.77时与定量峰面积比线性关系良好,精密度、重复性和稳定性的相对标准偏差(Relative standard deviation,简称RSD)分别为0.93%,1.6%,1.08%。qNMR法测得甲磺酸伊马替尼原料质量分数为98.6%,与高效液相色谱法的测定结果(98.2%)基本一致。建立的qNMR方法操作简单、准确,可用于甲磺酸伊马替尼质量分数测定。
