目的: 建立采用核磁共振氢谱（1H NMR）对伐地那非进行定性和定量分析的方法。方法: 将样品与经氢氧化钠碱化后的美国药典委员会（USP）对照品进行1H NMR 比对鉴别;采用Bruker AVANCE NEOAscend 600 型核磁共振波谱仪,脉冲序列zg90,恒温25 ℃,驰豫延迟时间（D1）30 s。以1,3,5- 三甲氧基苯为内标物,氘代二甲基亚砜（DMSO-d6）为溶剂,采用定量核磁共振氢谱法（qHNMR 法）测定伐地那非的含量,同时含量测定结果与质量平衡法和外标法测定结果进行比较。结果: 伐地那非样品的1H NMR 图谱和转化后的对照品的图谱一致;定量核磁共振氢谱法测得的伐地那非含量（99.8%）与质量平衡法（99.7%）、外标法（99.9%）测得结果一致。结论: NMR 法可用于伐地那非定性鉴别和定量分析,简便准确。
Objective： To establish a proton nuclear magnetic resonance（1H NMR） method for the qualitative and quantitative study of vardenafil. Methods： The qualitative identification of vardenafil was based on the comparison of its 1H NMR spectrum with that of USP reference standard after alkalization by sodium hydroxide. Quantitative 1H NMR spectra were obtained in dimethylsulfoxide-d6（ DMSO-d6） with the internal standard 1,3,5-trimethoxybenzene by a Bruker AVANCE NEO 600 spectrometer. The parameters were set up as follows： zg90 for pulse sequence,30 s for the relaxation delay time,and the experiment temperature was controlled at 25 ℃ . Meanwhile,the determination result was compared with those of mass balance method and external standard method. Results： The 1H NMR spectra of vardenafil and reference standard after alkalization by sodium hydroxide were consistent. The content of vardenafil determinated by qHNMR was 99.8%,which was consistent with that by mass balance method（ 99.7%） and external standard method（ 99.9%）. Conclusion： NMR method is simple and accurate for the qualitative identification and quantitative analysis of vardenafil.
[1] V IDAL DTR,AUGGELLI MA,LAGO CLD.Determination of sildenafil and vardenafil by capillary zone electrophoresis using capacitively coupled contactless conductivity detection[J].Anal Methods,2013,5(8):2041
[2] LIATSIKOS E,KYRIAZI S,NEUHAUS J,et al.Direct effects of vardenafil on the ureter:in vitro investigation and potential clinical applications of intralumenal administration[J].J Endourol,2013, 27(11):1400
[3] KYRIAZI S,KAGADIS GC,KALLIDONIS P,et al.PDE-5 inhibition against acute renal ischemia reperfusion injury in rats: does vardenafil offer protection[J].World J Urol,2013,31(3): 597
[4] 李锐,陈国彪.UPLC-Q-TOF-MS 法快速检测补肾壮阳类中成药中11 个PDE-5 型抑制剂类药物[J].药物分析杂志,2014,34(5):879
LI R,CHEN GB.Simultaneous determination of 11 phosphodiesterase-5 inhibitors added illegally in Chinese medicine preparations for invigorants by UPLC-Q-TOF-MS[J].Chin J Pharm Anal,2014,34(5):879
[5] USP42-NF 37[S].2020:4287
[6] 张永权,冯艳春,李进,等.酮康唑相关杂质国家标准物质的研制[J].药物分析杂志,2015,35(3):532
ZHANG YQ,FENG YC,LI J,et al.Establishment of national reference standards of ketoconazole impurities[J].Chin J Pharm Anal,2015,35(3):532
[7] 张芬芬,蒋孟虹,沈文斌,等.定量核磁共振(QNMR)技术及其在药学领域的应用进展[J].南京师范大学学报(工程技术版), 2014,14(2):8
ZHANG FF,JIANG MH,SHEN WB,et al.Progress in quantitative nuclear magnetic resonance technology in pharmaceutical applications[J].J Nanjing Norm Univ(Eng Technol Ed),2014,14(2):8
[8] 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
YU XB,SHEN WB,XIANG BR.Advances in application of quantitative nuclear magnetic resonance technique in pharmaceutical field[J].Prog Pharm Sci,2010,34(1):17
[9] 马晓丽,邹萍萍,雷伟,等.定量核磁技术参数的优化及其在中草药定量分析领域的应用[J].药学学报,2014,49(9): 1248
MA XL,ZOU PP,LEI W,et al.Optimization of experimental parameters for quantitative NMR and its application in quantitative analysis of traditional Chinese medicines[J].Acta Pharm Sin, 2014,49(9):1248
[10] 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):45l
HU M,HU CQ,LIU WY.Determination of drug reference substance content by 1H-nuclear magnetic resonance(NMR) spectroscopy[J].Chin J Anal Chem,2004,32(4):45l
[11] 易进海,刘云华,陈燕,等.核磁共振波谱法测定藁本内酯对照品的含量[J].药物分析杂志,2010,30(4):680
YI JH,LIU YH,CHEN Y,et al.Quantitative determination of ligustilide by H-nuclear magnetic resonance spectroscopy[J].Chin J Pharm Anal,2010,30(4):680
[12] 仙云霞,耿岩玲,周洪雷,等.核磁共振内标法测定覆盆子酮对照品的含量[J].山东科学,2015,28(1):76
XIAN YX,GENG YL,ZHOU HL,et al.1 H-NMR spectroscopy based content determination of 4-(p-hydroxyphenyl)-2-butanone[J].Shandong Sci,2015,28(1):76
[13] 耿岩玲,马然,刘伟,等.核磁共振内标法测定苏丹红I 对照品的含量[J].山东科学,2013,26(5):11
GENG YL,MA R,LIU W,et al.Content determination of Sudan 1 with 1H-NMR spectroscopy[J]. Shandong Sci,2013,26(5):11
