首页|基于定量核磁共振与色谱含量测定相结合的相对校正因子测定技术研究

基于定量核磁共振与色谱含量测定相结合的相对校正因子测定技术研究

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目的 建立基于定量核磁共振(qNMR)与色谱融合的相对校正因子(RCF)测定方法,探讨方法的可行性与准确性。方法 充分利用qNMR同一次测定中,所有激发原子的光谱常数相同的特点,由核磁信号计算化合物的物质的量之比,运用色谱技术测定色谱峰面积之比,进而将两者结果融合,计算出RCF;以对苯二甲酸二甲酯相对于香豆素的校正因子为例,验证方法的可靠性,并将该方法用于前维生素D3的RCF的计算。结果 实验结果显示,斜率比值法、多点法、融合技术3种方法测得的RCF值相同,验证了方法的可靠性。此外使用该方法测定了前维生素D3相对于维生素D3的RCF,测定结果与文献报道的结果一致,进一步证明了该计算方法准确可靠。结论 液相色谱与定量核磁共振融合技术,为在缺乏对照品的情况下,计算化合物RCF提供了新思路,解决了性质不稳定、对照品不易获得的化合物RCF测定难的问题。
Determination of Relative Correction Factor Based on Quantitative Nuclear Magnetic Resonance and Chro-matography
OBJECTIVE To establish a method for determining the relative correction factor(RCF)based on quantitative nucle-ar magnetic resonance(qNMR)and chromatography,and explore the suitability and accuracy of the method.METHODS The spec-tral constants of all excited atoms are the same in the qNMR experiment.The ratio of the amount of the substances was calculated by qNMR,and the chromatographic peak area was determined by chromatography.Then the RCF was calculated from the above two results.Taking the correction factor of dimethyl terephthalate relative to coumarin as an example,the reliability of the method was veri-fied.Then the method was used to calculate the RCF of pre-vitamin D3.RESULTS The RCF values obtained by slope ratio method,multi-point method,fusion technology were the same.The experimental result verified the reliability of the method.In addition,this method was used to determine the RCF of pre-vitamin D3 relative to vitamin D3.The results were consistent with those reported in the literature,which further proved that the calculation method was accurate and reliable.CONCLUSION This method provides a new idea for calculating RCF in the absence of reference substance,and solves the problem of difficult determination of RCF of compounds with unstable properties or unavailable standards.

quantitative nuclear magnetic resonanceliquid chromatographyrelative correction factorvitamin D3pre-vitamin D3

王娇娇、葛志伟、陆诗燕、袁京群、唐宇、王迎超

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浙江大学农生环测试中心,杭州 310058

浙江大学药学院,杭州 310058

定量核磁共振 液相色谱法 相对校正因子 维生素D3 前维生素D3

浙江省自然科学基金浙江大学实验技术研究项目(2022)

LTGY23H290006SYBJS202210

2024

中国药学杂志
中国药学会

中国药学杂志

CSTPCD北大核心
影响因子:0.957
ISSN:1001-2494
年,卷(期):2024.59(5)
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