核磁共振波谱法测定胆酸甲酯的含量
NMRS Determination of Methyl Ester of Cholic Acid
摘 要
采用核磁共振波谱法测定胆酸甲酯的含量。以顺丁烯二酸为内标,氘代二甲基亚砜和重水为溶剂,测试温度为298 K,脉冲宽度为8 μs,弛豫时间为50 s,扫描次数为16次。δ 6.28为顺丁烯二酸的定量峰,δ 3.79和δ 0.59为胆酸甲酯的定量峰,以两个定量峰试验结果的平均值计算胆酸甲酯的含量。顺丁烯二酸与胆酸甲酯的定量峰不受其他信号干扰,顺丁烯二酸与胆酸甲酯的质量比在0.208~1.03范围内呈线性。胆酸甲酯的绝对含量测定结果为99.4%,测定值的相对标准偏差(n=6)为0.33%。
胆酸甲酯
含量
NMR
Methyl ester of cholic acid
Content
Abstract
NMRS was applied to the determination of methyl ester of cholic acid. Maleic acid was used as the internal standard. Deuterated dimethyl sulfoxide and deutoxide were used as solvents. The testing temperature taken was 298 K, the pulse width was 8 μs, the relaxation time was 50 s, and the number of scanning was 16. The proton signals at δ 3.79 and δ 0.59 for methyl ester of cholic acid, and at δ 6.28 for maleic acid were selected for quantification. The content of methyl ester of cholic acid was obtained by calculating the average of test results of 2 quantitative peaks. Linearity range of mass ratio of maleic acid and methyl ester of cholic acid was found between 0.208-1.03. The content of methyl ester of cholic acid found was 99.4% with RSD (n=6) of 0.33%.
中图分类号 O657.2 DOI 10.11973/lhjy-hx201604004
所属栏目 试验与研究
基金项目 广东省科技计划项目(2012B040307002)
收稿日期 2015/4/10
修改稿日期
网络出版日期
作者单位点击查看
备注叶汝汉(1985-),男,广东江门人,助理研究员,硕 士,研究方向为有机化学分析。
引用该论文: YE Ru-han,ZHANG Yi,CHEN Jiang-han,LIU Ya-ling,CHEN Yong,PAN Wen-long. NMRS Determination of Methyl Ester of Cholic Acid[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(4): 388～391
叶汝汉,张 怡,陈江韩,柳亚玲,陈 泳,潘文龙. 核磁共振波谱法测定胆酸甲酯的含量[J]. 理化检验－化学分册, 2016, 52(4): 388～391
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参考文献
【1】国家药典委员会.中华人民共和国药典二部［M］.北京:中国医药科技出版社, 2010.
【2】HOLZGRABE U, DEUBNER R, SCHOLLMAYER C. Quantitative NMR spectroscopy-applications in drug analysis［J］. J Pharm Biomed Anal, 2005,38(1):806-812.
【3】HOLZGRABE U. Quantitative NMR spectroscopy in pharmaceutical applications［J］. Prog Nucl Magn Reson Spectrosc, 2010,53(1):229-240.
【4】BEYER T, DIEHL B, RANDEL G, et al. Quality assessment of unfractionated heparin using 1H nuclear magnetic resonance spectroscopy［J］. J Pharm Biomed Anal, 2008,48(1):13-19.
【5】胡敏,胡昌勤,刘文英.核磁共振波谱法测定药物基准物质的绝对含量［J］.分析化学, 2004,32(4):451-455.
【6】于小波,沈文斌,相秉仁.定量核磁共振技术及其在药学领域中的应用进展［J］.药学进展, 2010,34(1):17-23.
【7】蒋孟虹,于小波,毛黎顺,等.核磁共振法测定10-O-(N,N-二甲氨基乙基)-银杏内酯B甲磺酸盐标准物质的含量［J］.中国药科大学学报, 2013,44(4):339-342.
【8】王强,汪茂田,张志权.核磁共振法定量测定替米考星含量［J］.分析测试学报, 2003,22(6):101-103.
【9】刘阳,刘朝霞,吴建敏,等.19F核磁共振定量技术测定阿托伐他汀钙含量［J］.北京师范大学学报(自然科学版), 2014,50(3):287-289.
【10】刘阳,周颖,张才煜,等.核磁共振定量法测定脒基吡唑含量［J］.药物分析杂志, 2014,34(6):1087-1090.
【11】ICH Harmonised Tripartite Guideline Q3A(R2). Impurities in new drug substances［EB/OL］. ［2014-12-10］. http://www.ich.org/products/guidelines/quality/article/quality-guidelines.html.
【12】国家食品药品监督管理局药品审评中心.化学药物杂质研究的技术指导原则［EB/OL］. ［2014-12-10］.http://www.cde.org.cn/attachmentout.do?mothed=list&id=161.
【13】ICH Harmonised Tripartite Guideline Q2 (R1). Validation of analytical procedures: text and methodology［EB/OL］. ［2014-12-10］. http://www.ich.org/products/guidelines/quality/article/quality-guidelines.html.
【14】国家食品药品监督管理局药品审评中心.化学药物质量控制分析方法验证技术指导原则［EB/OL］. ［2014-12-10］. http://www.cde.org.cn/zdyz.do?method=largePage&id=2063.
【15】邓志威,李璟,许美凤,等.核磁共振技术在药物分析鉴定中的应用［J］.分析测试学报, 2012,31(9):1081-1088.
【16】GJERSING E, HAPPS R M, SYKES R W, et al. Rapid determination of sugar content in biomass hydrolysates using nuclear magnetic resonance spectroscopy［J］. Biotechnol Bioeng, 2013,110(3):721-728.
【17】OHTSUKI T, SATO K, SUGIMOTO N, et al. Absolute quantitative analysis for sorbic acid in processed foods using proton nuclear magnetic resonance spectroscopy［J］. Anal Chim Acta, 2012,734:54-61.
【18】PAULI G F, GODECKE T D, JAKI B U, et al. Quantitative 1H-NMR development and potential of an analytical method: an update［J］. J Nat Prod, 2012,5:834-851.
【19】RUNDLOF T, MATHIASSON M, BEKIROGLU S, et al. Survey and qualification of internal standards for quantification by 1H NMR spectroscopy［J］. J Pharm Biomed Anal, 2010,52:645-651.
【20】MALZ F, JANCKE H. Validation of quantitative NMR［J］. J Pharm Biomed Anal, 2005,38(5):813-823.
【21】张友杰,刘小鹏.药物核磁共振定量分析参数的研究［J］.波谱学杂志, 2007,24(3):289-295.
【2】HOLZGRABE U, DEUBNER R, SCHOLLMAYER C. Quantitative NMR spectroscopy-applications in drug analysis［J］. J Pharm Biomed Anal, 2005,38(1):806-812.
【3】HOLZGRABE U. Quantitative NMR spectroscopy in pharmaceutical applications［J］. Prog Nucl Magn Reson Spectrosc, 2010,53(1):229-240.
【4】BEYER T, DIEHL B, RANDEL G, et al. Quality assessment of unfractionated heparin using 1H nuclear magnetic resonance spectroscopy［J］. J Pharm Biomed Anal, 2008,48(1):13-19.
【5】胡敏,胡昌勤,刘文英.核磁共振波谱法测定药物基准物质的绝对含量［J］.分析化学, 2004,32(4):451-455.
【6】于小波,沈文斌,相秉仁.定量核磁共振技术及其在药学领域中的应用进展［J］.药学进展, 2010,34(1):17-23.
【7】蒋孟虹,于小波,毛黎顺,等.核磁共振法测定10-O-(N,N-二甲氨基乙基)-银杏内酯B甲磺酸盐标准物质的含量［J］.中国药科大学学报, 2013,44(4):339-342.
【8】王强,汪茂田,张志权.核磁共振法定量测定替米考星含量［J］.分析测试学报, 2003,22(6):101-103.
【9】刘阳,刘朝霞,吴建敏,等.19F核磁共振定量技术测定阿托伐他汀钙含量［J］.北京师范大学学报(自然科学版), 2014,50(3):287-289.
【10】刘阳,周颖,张才煜,等.核磁共振定量法测定脒基吡唑含量［J］.药物分析杂志, 2014,34(6):1087-1090.
【11】ICH Harmonised Tripartite Guideline Q3A(R2). Impurities in new drug substances［EB/OL］. ［2014-12-10］. http://www.ich.org/products/guidelines/quality/article/quality-guidelines.html.
【12】国家食品药品监督管理局药品审评中心.化学药物杂质研究的技术指导原则［EB/OL］. ［2014-12-10］.http://www.cde.org.cn/attachmentout.do?mothed=list&id=161.
【13】ICH Harmonised Tripartite Guideline Q2 (R1). Validation of analytical procedures: text and methodology［EB/OL］. ［2014-12-10］. http://www.ich.org/products/guidelines/quality/article/quality-guidelines.html.
【14】国家食品药品监督管理局药品审评中心.化学药物质量控制分析方法验证技术指导原则［EB/OL］. ［2014-12-10］. http://www.cde.org.cn/zdyz.do?method=largePage&id=2063.
【15】邓志威,李璟,许美凤,等.核磁共振技术在药物分析鉴定中的应用［J］.分析测试学报, 2012,31(9):1081-1088.
【16】GJERSING E, HAPPS R M, SYKES R W, et al. Rapid determination of sugar content in biomass hydrolysates using nuclear magnetic resonance spectroscopy［J］. Biotechnol Bioeng, 2013,110(3):721-728.
【17】OHTSUKI T, SATO K, SUGIMOTO N, et al. Absolute quantitative analysis for sorbic acid in processed foods using proton nuclear magnetic resonance spectroscopy［J］. Anal Chim Acta, 2012,734:54-61.
【18】PAULI G F, GODECKE T D, JAKI B U, et al. Quantitative 1H-NMR development and potential of an analytical method: an update［J］. J Nat Prod, 2012,5:834-851.
【19】RUNDLOF T, MATHIASSON M, BEKIROGLU S, et al. Survey and qualification of internal standards for quantification by 1H NMR spectroscopy［J］. J Pharm Biomed Anal, 2010,52:645-651.
【20】MALZ F, JANCKE H. Validation of quantitative NMR［J］. J Pharm Biomed Anal, 2005,38(5):813-823.
【21】张友杰,刘小鹏.药物核磁共振定量分析参数的研究［J］.波谱学杂志, 2007,24(3):289-295.
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