拉曼光谱法直接测定甲硝唑片含量

Direct Content Determination of Metronidazole Tablets by Raman Spectroscopy

关键词:  拉曼光谱  特征峰  甲硝唑片  高效液相色谱

Key words:  Raman spectroscopy  characteristic peak  metronidazol tablets  HPLC

摘要:

目的 建立拉曼光谱法直接测定甲硝唑片含量的方法。方法 从便携式激光拉曼光谱仪的标准光谱图库中选出甲硝唑标准拉曼光谱图，再从甲硝唑标准拉曼光谱图(200~3000 cm^-1)中筛选出适宜用于含量测定的特征峰，通过线性、重复性、回收率等方法学验证建立拉曼光谱直接测定甲硝唑片含量的方法，将甲硝唑片从药瓶中取出后直接用拉曼光谱法测定含量并将测定结果与HPLC测定结果做比较分析。结果 甲硝唑标准拉曼光谱图中1533 cm^-1处的特征峰未受辅料干扰，专属性和稳定性最好，适宜用作含量测定的特征峰。拉曼光谱直接测定甲硝唑片含量的方法在26~1000 mg·g^-1线性良好，线性方程为y=7.989 5x+0.3948，相关系数为0.9994；该方法的检测限和定量限分别为10和26 mg·g^-1。在高、中、低3个含量下，该方法的日内和日间精密度的RSD值分别为0.08%，0.12%，0.11%和0.47%，0.48%，0.65%。同一甲硝唑片重复测定6次的RSD值为0.41%。在回收率试验中，该方法测定高、中、低含量的平均回收率分别为99.87%，100.2%，100.1%，RSD值分别为0.04%，0.07%，0.18%。拉曼光谱法1测定结果的预测相对误差范围为-0.7%~0.5%，最大误差绝对值为0.7%，拉曼光谱法2测定结果的预测相对误差范围为-0.7%~1.1%，最大误差绝对值为1.1%。结论 本法快速、简便，可以实现甲硝唑片含量的无损检测。

Abstract:

OBJECTIVE To establish the direct content determination method of metronidazol tablets by raman spectroscopy. METHODS By selecting standard raman spectrum of metronidazol from standard spectrum database in portable laser reman spectrometer and then selecting proper characteristic peak from standard raman spectrum(200~3000 cm^-1) of metronidazol, using of methodological verification including linear, repeatability and recovery tests, the direct content determination method of metronidazol tablets by raman spectroscopy was established. The metronidazol tablets without any pretreatment were taken from bottles for content determination directly by using of reman spectroscopy and their determination results were compared with that of HPLC. RESULTS The characteristic peak at 1 533 cm^-1 in the standard raman spectrum of metronidazol was not affected by supplements, with best exclusivity and stability and proper to be used for its content determination. In the direct content determination method of metronidazol tablets, the good linear relationship was achieved in the range of 26-1000 mg·g^-1, its linear equation was y=7.989 5x+0.3948 with correlation coefficient of 0.9994 and its detection and quantitative limits were 10 and 26 mg·g^-1 respectively. The determination RSDs of same-day and between-days of high, middle and low contents were 0.08%, 0.12%, 0.11% and 0.47%, 0.48%, 0.65% respectively. The RSD of 6 repeated determinations of the same metronidazol tablet was 0.41%. In recovery test, the average recoveries of reman spectroscopy in determinating high, middle and low contents were 99.87%, 100.2%, 100.1%, RSDs were 0.04%, 0.07% and 0.18% respectively. The scope and max of relative prediction error of reman spectroscopy 1 were -0.7%-0.5% and 0.7% and that of reman spectroscopy 2 were -0.7%-1.1% and 1.1%. CONCLUSION The method is fast and simple, which can achieve nondestructive testing of metronidazole tablets.