磺胺甲基嘧啶纯度定值研究  

Purity Determination of Sulfadiazine

作　　者：孙余娟 孙永跃[1] 李蔚 全灿[2] 陈刚[3] 王艺玮 赵程祥 尹伊 SUN Yu-juan;SUN Yong-yue;LI Wei;QUAN Can;CHEN Gang;WANG Yi-wei;ZHAO Cheng-xiang;YIN Yi(Tianjin Key Laboratory of Drug Targeting and Bioimaging,School of Chemistry and Chemical Engineering,Tianjin University of Technology,Tianjin 300384,China;Division of Metrology in Chemistry,National Institute of Metrology,Beijing 100029,China;Key Laboratory of Agro-Product Quality and Safety,Institute of Quality Standards and Testing Technology for Agro-Products,Chinese Academy of Agricultural Sciences(CAAS),Beijing 100081,China)

机构地区：[1]天津理工大学化学化工学院天津市药物靶向与生物成像重点实验室,天津300384 [2]中国计量科学研究院化学计量与分析科学研究所,北京100029 [3]中国农业科学院农业质量标准与检测技术研究所,北京100081

出　　处：《化学试剂》2021年第4期499-504,共6页Chemical Reagents

基　　金：“十三五”国家重点研发课题项目(2018YFC-1602304)。

摘　　要：采用氢定量核磁共振法和质量平衡法对磺胺甲基嘧啶纯度进行定值。通过Bruker-AvanceⅢ400型核磁共振波谱仪,noesyigld 1d脉冲序列,以尼泊金乙酯为内标、氘代DMSO为溶剂,在恒温298 K、谱宽为15×10^(-4)%、中心激发偏置为5.41×10^(-4)%、弛豫时间为7 s、扫描次数为32、空扫16次的条件下,采集^(1)H-qNMR光谱数据。以磺胺甲基嘧啶化学位移(δ6.56)为定量峰,尼泊金乙酯化学位移(δ4.25)为内标峰,^(1)H-qNMR测得磺胺甲基嘧啶纯度为96.55%,测定精密度RSD为0.089%,重复性RSD为0.24%。质量比Y(m_(s)/m_(r))在2.014~4.051范围内与峰面积比X(A_(s)/A_(r))呈线性关系,线性回归方程为y=0.6071x+0.0049(R2=0.9999)。结果表明,^(1)H-qNMR与质量平衡法测定结果具有一致性。因此,氢定量核磁共振法可用于磺胺甲基嘧啶含量测定,该方法具有准确、简便的优势。Establish hydrogen quantitative nuclear magnetic resonance method and mass balance method to determine the purity of sulfamethazine.Bruker-AvanceⅢ400 nuclear magnetic resonance spectrometer,noesyigld 1 d pulse sequence,ethylparaben as internal standard,deuterated DMSO as solvent,constant temperature is 298 K,spectrum width(SW)is 15×10^(-4)%,the excitation bias(O1 P)is 5.41×10^(-4)%,the relaxation time(D1)is 7 s,a scan number of 32,and an empty scan of 16,^(1)H-qNMR spectra were collected.The sulfamethazine chemical shift(δ6.56)was used as the quantitative peak,and the ethylparaben chemical shift(δ4.25)was used as the internal standard peak.The purity of sulfamethazine measured by^(1)H-qNMR was 96.55%.The precision RSD was 0.089%,and the repeatability RSD was 0.24%.The mass ratio(m_(s)/m_(r))is 2.014~4.051,and the linear regression equation of the mass ratio Y(m_(s)/m_(r))and its peak area ratio X(A_(s)/A_(r))is y=0.6071x+0.0049(R2=0.9999).The results of^(1)H-qNMR measurement are basically consistent with the mass balance method.Therefore,the hydrogen quantitative nuclear magnetic resonance method can be used for the determination of sulfadiazine content.The method has the advantages of accuracy and simplicity.

关 键 词：氢定量核磁共振(^(1)H-qNMR) 磺胺甲基嘧啶 质量平衡法 含量测定 

分 类 号：O657.61[理学—分析化学]