定量核磁共振(Quantitative Nuclear Magnetic Resonance,QNMR)法操作简便,不需要自身对照品即可进行含量测定,准确度高,定性与定量可同时进行,在新药开发、药物的对照品研究、质量控制以及代谢组学等药学领域诸多方面具有显著优势.目...定量核磁共振(Quantitative Nuclear Magnetic Resonance,QNMR)法操作简便,不需要自身对照品即可进行含量测定,准确度高,定性与定量可同时进行,在新药开发、药物的对照品研究、质量控制以及代谢组学等药学领域诸多方面具有显著优势.目前美国药典、英国药典、欧洲药典、日本药局方以及中国药典均已将该技术作为法定标准收载于附录中.本文综述了QNMR的原理、方法及近年来在药学领域的应用进展,并对其应用前景进行了展望.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
Objective: To develop a qNMR method for quantitative analysis of triacylglycerols in fruit oil of Hippophae rhamnoides(seabuckthorn, SBT) and analyze commercial samples of SBT oils using GC–MS and FTIR.Methods: SBT f...Objective: To develop a qNMR method for quantitative analysis of triacylglycerols in fruit oil of Hippophae rhamnoides(seabuckthorn, SBT) and analyze commercial samples of SBT oils using GC–MS and FTIR.Methods: SBT fruit oil(IPHRFH) was extracted with hexane and the triglyceride(TAG) was isolated by vacuum liquid chromatography. Six different branded SBT oils purchased from e-commerce suppliers(Amazon) and in-house prepared SBT oil was analyzed by qNMR and fatty acyl composition of TAGs determined by using NMR. In-house oil was also analysed by GC–MS and FTIR spectroscopy.Results: The qNMR results showed that the oil contained 80.3% of triacylglycerol(TAG). The SBT oil TAGs comprised of linolenate 6.6%, palmitoleate/oleate 65.4%, and total saturated fatty acyl chain including palmitate 28% as determined by qNMR. GC–MS analysis revealed that the major acyl functionalities present in the TAG were palmitoleic acid 36.5%, oleic acid 12.9%, palmitic acid 21.2%, and linoleic acid 18%. Of the six commercial samples analyzed, samples from only one supplier(SW) were fruit oil;All others were the seed oils or mix of fruit oil and seed oil. The labels for samples except for the SW did not indicate whether it was fruit oil or seed oil.Conclusion: The results suggest that SBT oil should be analyzed by combination of GC–MS, FTIR and qNMR for factual content of free fatty acid or TAGs, which are chemically different in nature and affect the quality of oil. GC–MS showed the content of omega free fatty acids after hydrolysis, while qNMR and FTIR showed the content of TAGs. The major acyl functionalities found in SBT fruit oil TAGs are palmitoleate/palmitate/oleate, while linoleate and linonelate make up a minor fraction. Furthermore,analysis of commercial samples showed discrepancies between label claims and actual content.展开更多
文摘定量核磁共振(Quantitative Nuclear Magnetic Resonance,QNMR)法操作简便,不需要自身对照品即可进行含量测定,准确度高,定性与定量可同时进行,在新药开发、药物的对照品研究、质量控制以及代谢组学等药学领域诸多方面具有显著优势.目前美国药典、英国药典、欧洲药典、日本药局方以及中国药典均已将该技术作为法定标准收载于附录中.本文综述了QNMR的原理、方法及近年来在药学领域的应用进展,并对其应用前景进行了展望.
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.
基金Department of Biotechnology, Government of India for a research grant (DBT-New Delhi, No. BT/ PR9116/NDB/39/390/2013)。
文摘Objective: To develop a qNMR method for quantitative analysis of triacylglycerols in fruit oil of Hippophae rhamnoides(seabuckthorn, SBT) and analyze commercial samples of SBT oils using GC–MS and FTIR.Methods: SBT fruit oil(IPHRFH) was extracted with hexane and the triglyceride(TAG) was isolated by vacuum liquid chromatography. Six different branded SBT oils purchased from e-commerce suppliers(Amazon) and in-house prepared SBT oil was analyzed by qNMR and fatty acyl composition of TAGs determined by using NMR. In-house oil was also analysed by GC–MS and FTIR spectroscopy.Results: The qNMR results showed that the oil contained 80.3% of triacylglycerol(TAG). The SBT oil TAGs comprised of linolenate 6.6%, palmitoleate/oleate 65.4%, and total saturated fatty acyl chain including palmitate 28% as determined by qNMR. GC–MS analysis revealed that the major acyl functionalities present in the TAG were palmitoleic acid 36.5%, oleic acid 12.9%, palmitic acid 21.2%, and linoleic acid 18%. Of the six commercial samples analyzed, samples from only one supplier(SW) were fruit oil;All others were the seed oils or mix of fruit oil and seed oil. The labels for samples except for the SW did not indicate whether it was fruit oil or seed oil.Conclusion: The results suggest that SBT oil should be analyzed by combination of GC–MS, FTIR and qNMR for factual content of free fatty acid or TAGs, which are chemically different in nature and affect the quality of oil. GC–MS showed the content of omega free fatty acids after hydrolysis, while qNMR and FTIR showed the content of TAGs. The major acyl functionalities found in SBT fruit oil TAGs are palmitoleate/palmitate/oleate, while linoleate and linonelate make up a minor fraction. Furthermore,analysis of commercial samples showed discrepancies between label claims and actual content.
