摘要
用Varian Inova-400MHz超导核磁共振波谱仪,以氘代二甲基亚砜(DMSO-d6)为溶剂,对苯二酚为内标,在50℃,检测频率为399.74MHz,谱宽为6999.70Hz,90°脉冲宽度为12.10μs,采集时间为3.74s,延迟时间为10.00s,采集次数为40次的条件下采集样品1H-NMR谱图。以化学位移分别在δ9.89和δ6.55处的维生素B1单峰和对苯二酚的单峰作为定量峰,建立了一种用核磁共振内标法简单、快速且无需对照品测定维生素B1片中有效成分含量的方法。测得维生素B1的含量为15.20%,测定结果与标签示值的相对误差为1.56%,表明在没有对照品的情况下,核磁共振内标法可用于维生素B1片中有效成分含量测定和质量控制。
With a Varian Inova-400MHz superconducting NMR spectrometer collecting the 1H-NMR spectra of the sample under the condition of 50 ℃, substitute deuterium dimethyl sulfoxide (DMSO-d6) as solvent, hydroquinone as the internal standard, testing frequency is 399.74 MHz, spectral width is 6999.70 Hz, 90° pulse width is 12.10 μs, acquisition time is 3.74 s, delay time is 10.00 s, sampling frequency for 40 times. With the single peak of Vitamin B1 and hydroquinone, which chemical shift in the delta 9.89 and 6.55 respectively, as quantitative peak, developed a simple, rapid and without reference substance nuclear magnetic resonance (NMR) internal standard method for the determination of the content of Vitamin B1 in Vitamin B1 tablets. the measured Vitamin B1 content is 15.20 %, and the determination results with the tag value of relative error is 1.56 %, which indicates that in the absence of reference substance, the nuclear magnetic resonance (NMR) internal standard method can be used for the determination and quality control of Vitamin B1 in Vitamin B1 tablets.
作者
王斌
陈国通
Wang Bin;Chen Guotong(Physics and Chemistry Detecting Center, Xinjiang University, Urumqi 830046;Xinjiang Academy Of Analysis and Testing, Urumqi 830011, China)
出处
《广东化工》
CAS
2019年第10期153-154,共2页
Guangdong Chemical Industry
基金
新疆维吾尔自治区自然科学基金项目(2017D01C075)
关键词
核磁共振
内标法
维生素B1
Nuclear Magnetic Resonance
Internal Standard Method
Vitamin B1
