1H和19F核磁共振定量法测定塞来昔布含量

Content Determination of Celecoxib by 1H and 19F Quantitative Nuclear Magnetic Resonance

关键词:  塞来昔布  含量测定  氢核磁共振定量法  氟核磁共振定量法

Key words:  celecoxib  content determination  ¹H quantitative nuclear magnetic resonance  ¹⁹F quantitative nuclear magnetic resonance

摘要:

目的 分别采用¹H核磁共振定量法和¹⁹F核磁共振定量法测定塞来昔布绝对含量，并将2种方法的测定结果与质量平衡法测定结果进行比较。方法 ¹H核磁共振定量法以CD₃OD为溶剂，塞来昔布δ 6.92处质子峰作为定量峰，马来酸δ 6.33处为内标峰。在弛豫延迟时间10 s，采样时间4.01 s，扫描次数为32条件下采集混合物的氢谱。¹⁹F核磁共振定量法以CD₃OD为溶剂，4-溴-2-氟-乙酰苯胺为内标，在谱宽240 ppm，中心频率-94.26 ppm，样品扫描次数为16次条件下采集氟谱，计算¹H和¹⁹F核磁共振定量法的测试结果。结果 ¹H核磁共振定量法和¹⁹F核磁共振定量法测定结果相近，且与质量平衡法测定结果基本一致。结论 核磁共振定量法可以用来测定塞来昔布含量，具有准确、高效的优势。

Abstract:

OBJECTIVE To determine the content of celecoxib by ¹H quantitative nuclear magnetic resonance and ¹⁹F quantitative nuclear magnetic resonance, and compare the results of the two methods of quantitative nuclear magnetic resonance with mass balance method. METHODS CD₃OD was employed as solvent, proton signal peaks of celecoxib at δ 6.92 and δ 6.33 of maleic acid were served as quantitative peaks and inner peak, respectively. The spectra of the mixture were collected at 10 s relaxation delay, 4.01 s acquisition time and 32 scanning times. In the ¹⁹F quantitative fluorine nuclear magnetic resonance, CD₃OD was used as solvent, 4-bromo-2-fluoroacetanilide was employed as internal standard, the spectra were obtained with spectral width of 240 ppm, transmitter frequency offset was -94.26 ppm and the scanning times was 16. The results of ¹H quantitative nuclear magnetic resonance and ¹⁹F quantitative nuclear magnetic resonance were calculated. RESULTS The results of ¹H quantitative nuclear magnetic resonance and ¹⁹F quantitative nuclear magnetic resonance were very close, which were generally consistent with that of the mass balance method. CONCLUSION Quantitative nuclear magnetic resonance can be used for the quantitative determination of celecoxib with the superiority of accurate and effective.