核磁共振内标法测定依巴斯汀片中有效成分含量
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摘要
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依巴斯汀片中有效成分含量的方法。用Varian Inova-400 MHz超导核磁共振波谱仪,在50℃,以氘代二甲基亚砜(DMSO-d6)为溶剂,对苯二酚为内标,检测频率为399.74 MHz,谱宽为6999.70 Hz,90°脉冲宽度为12.10μs,采集时间为3.74 s,延迟时间为10.00 s,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δ1.30和δ6.55处的依巴斯汀单峰和对苯二酚的单峰作为定量峰,测得依巴斯汀的含量为7.40%,测定结果与标签示值的相对误差为3.40%,表明在没有对照品的情况下,核磁共振内标法可用于依巴斯汀片中有效成分含量测定和质量控制。
A simple, rapid and without reference substance nuclear magnetic resonance(NMR) internal standard method for the determination of the content of Ebastine in Ebastine tablets has been developed. With a Varian Inova-400 MHz superconducting NMR spectrometer collecting the 1 H-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 o 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 Ebastine and hydroquinone, which chemical shift in the delta 1.30 and 6.55 respectively, as quantitative peak, the measured Ebastine content is 7.40 %, and the determination results with the tag value of relative error is 3.40 %, 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 Ebastine in Ebastine tablets.
A simple, rapid and without reference substance nuclear magnetic resonance(NMR) internal standard method for the determination of the content of Ebastine in Ebastine tablets has been developed. With a Varian Inova-400 MHz superconducting NMR spectrometer collecting the 1 H-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 o 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 Ebastine and hydroquinone, which chemical shift in the delta 1.30 and 6.55 respectively, as quantitative peak, the measured Ebastine content is 7.40 %, and the determination results with the tag value of relative error is 3.40 %, 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 Ebastine in Ebastine tablets.
引文
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[3]祁慧雪.核磁共振技术在化学物质定量分析中的应用[J].广东化工,2012,39(6):121.
[4]李彭,赵阳,赵彦彪,等.核磁共振技术及定量核磁共振技术在毒品分析中的应用[J].刑事技术,2017,42(4):312-316.
[5]沈桂平,戴晓侠,邓伶莉,等.家族性甲亢患者血清和尿液的核磁共振代谢组学研究[J].高等学校化学学报,2013,10(34):2290-2295.
[6]国家药典委员会.中华人民共和国药典(二部,2010年版)[S].北京:中国医药科技出版社,2010:附录页81-83.
[7]徐蕾,庞靖.高效液相梯度洗脱法测定依巴斯汀片的有关物质[J].齐鲁药事,2007,26(12):720-721.
[8]林琼,杨伟峰,陈爽.依巴斯汀原料药及其片剂有关物质测定方法的改进[J].中国现代应用药学,2015,32(4):489-492.