目的: 建立低场与高场核磁共振技术测定盐酸吡哆辛的含量,比较分析方法学验证结果和样品含量测定结果的差异。方法: 分别使用80 MHz低场核磁共振仪和500 MHz高场核磁共振仪,以氘代水为溶剂,马来酸为内标,用氢核磁共振定量法进行分析方法学验证,并测定盐酸吡哆辛含量。结果: 盐酸吡哆辛在10~30 mg·mL-1浓度范围内线性关系良好,低场与高场核磁共振仪测定线性相关系数分别为0.999 8和0.999 6;5次测定结果精密度,低场和高场核磁共振仪的RSD分别为1.4%和0.040%;含量测定结果为100.4%和100.8%,与质量平衡法结果(100.0%)基本一致,重复性RSD均为0.20%。对相同浓度样品,高场核磁共振信噪比(S/N)约为低场核磁共振的100倍,半峰宽为低场核磁的1/15。结论: 低场与高场核磁共振仪在盐酸吡哆辛含量测定中均能得到准确的结果,但低场核磁共振仪只适用于结构较简单的化合物。实际含量测定过程中,需要根据待测样品结构及溶解性选择适当的仪器。
Abstract
Objective: To establish a low-field and high-field nuclear magnetic resonance (NMR) technique for the determination of pyridoxine hydrochloride. To compare the differences between the results of method validation and sample content. Methods: Using deuterated water as the solvent and maleic acid as the internal standard, method validation of quantitative nuclear magnetic resonance (qNMR) was accomplished with both 80 MHz low-field NMR and 500 MHz high-field NMR instruments. The content of pyridoxine hydrochloride was also determined. Results: The linearity of pyridoxine hydrochloride was good in the range of 10-30 mg·mL-1, and the linear correlation coefficients were 0.999 8 and 0.999 6 for the low-field and high-field NMR, respectively. RSDs of the low-field and high-field NMR measurements were 1.4% and 0.040%, respectively. The contents were 100.4% and 100.8%, which were in agreement with the results from the mass balance method (100.0%). And the repeatability RSD was 0.20%. For the same concentration of the sample, the signal-to-noise ratio (S/N) of high-field NMR was about 100 times that of low-field NMR, and the half-peak width was 1/15 of that of low-field NMR. Conclusion: Both low-field and high-field NMR instruments gave accurate results in the determination of pyridoxine hydrochloride content. However, low-field NMR was only suitable for compounds with simple structures. In the actual content determination, it is necessary to choose the appropriate instrument according to the structure and solubility of the sample to be tested.
关键词
低场核磁共振仪 /
高场核磁共振仪 /
氢核磁共振定量 /
盐酸吡哆辛 /
含量测定 /
方法学验证
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Key words
low-field NMR /
high-field NMR /
quantitative hydrogen NMR /
pyridoxine hydrochloride /
determination /
methodological validation
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脚注
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基金
*中检院关键技术研究基金(GJJS-2022-4-2)
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