核磁共振定量法测定茶苯海明的含量
|
摘要
目的:建立定量核磁共振波谱法同时测定茶苯海明中苯海拉明和8-氯茶碱的方法。方法:以对苯二酚为内标,氘代甲醇为溶剂,分别采用苯海拉明中的δ2.89的甲基峰与8-氯茶碱中的δ3.47的甲基峰和内标峰的比值计算含量。结果:该方法精密度小于0.6%,线性相关系数(r)均为0.9999,实际测定茶苯海明原料药中的苯海拉明与8-氯茶碱的含量分别为54.04%与45.37%。结论:本文建立的核磁定量法快速、简单、准确,为该品种的含量测定提供了新的方法。
Objective: To establish a quantitative nuclear magnetic resonance spectroscopic(q NMR) method for simultaneous determination of diphenhydramine and 8-chlorotheophylline in dimenhydrinate. Methods: Hydroquinone was used as internal standard and deuterated methanol was used as solvent. The ratios of methyl peak of δ 2.89 in diphenhydramine and the methyl peak of δ 3.47 in 8-chlorotheophylline with internal standard peak were used to calculate the contents respectively. Results: The precision of the method was less than 0.6% and the linear correlation coefficient(r) was 0.9999. The actual content of diphenhydramine and 8-chlorotheophylline in the raw material of dimenhydrinate was 54.04% and 45.37%, respectively. Conclusion:The q NMR method established in this paper is a rapid, simple and accurate method, which provides a new way to determine the content of the dimenhydrinate.
Objective: To establish a quantitative nuclear magnetic resonance spectroscopic(q NMR) method for simultaneous determination of diphenhydramine and 8-chlorotheophylline in dimenhydrinate. Methods: Hydroquinone was used as internal standard and deuterated methanol was used as solvent. The ratios of methyl peak of δ 2.89 in diphenhydramine and the methyl peak of δ 3.47 in 8-chlorotheophylline with internal standard peak were used to calculate the contents respectively. Results: The precision of the method was less than 0.6% and the linear correlation coefficient(r) was 0.9999. The actual content of diphenhydramine and 8-chlorotheophylline in the raw material of dimenhydrinate was 54.04% and 45.37%, respectively. Conclusion:The q NMR method established in this paper is a rapid, simple and accurate method, which provides a new way to determine the content of the dimenhydrinate.
引文
[1]中国药典:二部[S].2015:713-714.
[2]USP 38[S].2015:3134.
[3]EP 8.0[S].2015:2063-2065.
[4]JP 17[S].2016:809.
[5]U.D?GE,K.EGER.A Simple HPLC-UV Method for the Determination of Dimenhydrinate and Related Substances–identification of an Unknown Impurity[J].Pharmazie,2007,(64):174-178.
[6]F.Malz,H.Jancke.Validation of Quantitative NMR[J].J Pharm Biomed Anal,2005,38:813-823.
[7]U.Holzgrabe,R.Denbner,C.Schollmayer,et al.Quantitative NMR Spectroscaopy-applications in Drug Analysis[J].J Pharm Biomed Anal,2005,38:806-812.
[8]禹珊,郭强胜,王会琳,等.定量核磁共振波谱法同时测定中药虎杖中白藜芦醇和虎杖苷的含量[J].分析化学,2015,43(1):69-74.
[9]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.
[10]韦英亮,莫建光,潘艳坤,等.磺胺类标准物质期间核查NMR定量方法研究[J].波谱学杂志,2013,30(3):371-379.
[11]Liu SY,Hu CQ.A Comparative Uncertainty Study of the Calibration of Macrolide Antibiotic Reference Standards Using Quantitative Nuclear Magnetic Resonance and Mass Balance Methods[J].Anal Chim Acta,2007,(602):114-121.
[12]Wu Y,He Y,He W Y,et al.Application of Quantitative1H NMR for the Calibration of Protoberberine Alkaloid Reference Standards[J].J Pharm Biomed Anal,2014,90:92-97.
[13]Stephen A.Wise,Hendrik Emons.Reference Materials for Chemical Analysis[J].Anal Bioanal Chem,2015,407:8557-8569.
[14]Michael A.Nelson,Mary Bedner,Brian E.Lang,et al.Metrological Approaches to Organic Chemical Purity:Primary Reference Materials for Vitamin D Metabolites[J].Anal Bioanal Chem,2015,407:8557-8569.
[15]中国药典:四部[S].2015:52-56.
[16]Pauli G F,Jaki B U,Lankin D C,et al.Quantitative 1H NMR Development and Potential of an Analytical Method:An Update[J].J Nat Prod,2005,68(1):133-149.
[2]USP 38[S].2015:3134.
[3]EP 8.0[S].2015:2063-2065.
[4]JP 17[S].2016:809.
[5]U.D?GE,K.EGER.A Simple HPLC-UV Method for the Determination of Dimenhydrinate and Related Substances–identification of an Unknown Impurity[J].Pharmazie,2007,(64):174-178.
[6]F.Malz,H.Jancke.Validation of Quantitative NMR[J].J Pharm Biomed Anal,2005,38:813-823.
[7]U.Holzgrabe,R.Denbner,C.Schollmayer,et al.Quantitative NMR Spectroscaopy-applications in Drug Analysis[J].J Pharm Biomed Anal,2005,38:806-812.
[8]禹珊,郭强胜,王会琳,等.定量核磁共振波谱法同时测定中药虎杖中白藜芦醇和虎杖苷的含量[J].分析化学,2015,43(1):69-74.
[9]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.
[10]韦英亮,莫建光,潘艳坤,等.磺胺类标准物质期间核查NMR定量方法研究[J].波谱学杂志,2013,30(3):371-379.
[11]Liu SY,Hu CQ.A Comparative Uncertainty Study of the Calibration of Macrolide Antibiotic Reference Standards Using Quantitative Nuclear Magnetic Resonance and Mass Balance Methods[J].Anal Chim Acta,2007,(602):114-121.
[12]Wu Y,He Y,He W Y,et al.Application of Quantitative1H NMR for the Calibration of Protoberberine Alkaloid Reference Standards[J].J Pharm Biomed Anal,2014,90:92-97.
[13]Stephen A.Wise,Hendrik Emons.Reference Materials for Chemical Analysis[J].Anal Bioanal Chem,2015,407:8557-8569.
[14]Michael A.Nelson,Mary Bedner,Brian E.Lang,et al.Metrological Approaches to Organic Chemical Purity:Primary Reference Materials for Vitamin D Metabolites[J].Anal Bioanal Chem,2015,407:8557-8569.
[15]中国药典:四部[S].2015:52-56.
[16]Pauli G F,Jaki B U,Lankin D C,et al.Quantitative 1H NMR Development and Potential of an Analytical Method:An Update[J].J Nat Prod,2005,68(1):133-149.