成分分析

定量核磁共振氢谱检测右佐匹克隆片的含量*

展开
  • 1.中国科学院南海海洋研究所仪器设备公共服务中心,广州 510301;
    2.中国科学院南海海洋研究所中国科学院热带海洋生物资源与生态重点实验室,广州 510301
第一作者 Tel:(020)89023100;E-mail: zhengxiaohong@scsio.ac.cn
**Tel:(020)89023100;E-mail: xzh@scsio.ac.cn

收稿日期: 2023-07-26

  网络出版日期: 2024-06-21

基金资助

*2021年度中国科学院技术支撑人才项目(2022006)

Determination of dexzopiclone tablets content by quantitative nuclear magnetic resonance*

Expand
  • 1. Equipment Public Service Center of South China Sea Institute of Oceanology, Chinese Academy of Sciences, Guangzhou 510301, China;
    2. Key Laboratory of Tropical Marine Bio-Resources and Ecology, South China Sea Institute of Oceanology, Chinese Academy of Sciences, Guangzhou 510301, China

Received date: 2023-07-26

  Online published: 2024-06-21

摘要

目的: 建立定量核磁共振氢谱(qHNMR)测定右佐匹克隆含量的方法。方法: 以1,3,5-三甲氧基苯δ 6.08处质子信号为内标峰,以右佐匹克隆 δ 8.54、8.38、8.12、7.78处质子信号为定量峰,以DMSO-d6为溶剂,在恒温298 K,弛豫延迟时间10 s,扫描次数32次条件下采集氢谱。结果: 定量核磁共振氢谱法测定右佐匹克隆片中右佐匹克隆平均含量为2.94%,即平均每片中含右佐匹克隆3.00 mg,RSD为0.15%,与药物说明标示的量基本一致。结论: 定量核磁共振氢谱可用于药物中右佐匹克隆含量的测定,并且具有快速、准确以及操作简单等优势。

本文引用格式

郑晓红, 车逸豪, 肖志会 . 定量核磁共振氢谱检测右佐匹克隆片的含量*[J]. 药物分析杂志, 2024 , 44(3) : 380 -385 . DOI: 10.16155/j.0254-1793.2024.03.02

Abstract

Objective: To establish a quantitative 1H-NMR (qHNMR) method for the determination of dexzopiclone tablets content. Methods: Proton signal at δ 6.08 of 1,3,5-trimethoxybenzene and δ 8.54,8.38,8.12,7.78 of dexzopiclone were served as the internal standard and quantitative peaks,respectively. DMSO-d6 was employed as the solvent. The qHNMR spectra were acquired at 298 K with 10 s relaxation delay and 32 scanning times. Results: The content of dexzopiclone was estimated to be 2.94% (RSD=0.15%)by qHNMR method,which indicated that 3.00 mg of dexzopiclone was in one tablet. The result was consistent with the description of the label. Conclusion: qHNMR method can be used to determine the content of dexzopiclone. The method is accurate,simple and efficient.

参考文献

[1] 黄挺,王静羽,张伟,等. 近十年定量核磁共振法应用研究进展[J]. 化学试剂,2023,45(6): 123
HUANG T, WANG JY, ZHANG W, et al. Research progress in the application of quantitative nuclear magnetic resonance method in recent decade[J]. Chem Reagents, 2023, 45(6):123
[2] 张芬芬,沈文斌,徐开兵,等. 定量核磁共振氢谱测定新药替格瑞洛[J]. 波谱学杂志,2020,37(2):216
ZHANG FF, SHEN WB, XU KB, et al. A proton nuclear magnetic resonance method for quantitative analysis of ticagrelor[J]. Chin J Magn Reson, 2020, 37(2):216
[3] 卢爱民,蒋红梅,吕波,等. 核磁共振氢谱内标法测定饮料中咖啡因含量[J]. 南京农业大学学报,2014,37(6):119
LU AM, JIANG HM, LÜ B, et al. Quantitative determination of caffeine in beverages by 1H-NMR with internal standard method[J]. J Nanjing Agric Univ, 2014, 37(6):119
[4] HOLZGRABE U. Quantitative NMR spectroscopy in pharmaceutical applications[J]. J Progr Nuclear Magn Reson Spectrosc, 2010, 57(2):229
[5] 王瑾,陈忠兰,朱雪坤,等. 核磁共振氢谱法定性和定量分析伐地那非[J]. 药物分析杂志,2021,41(7):1272
WANG J, CHEN ZL, ZHU XK, et al. Qualitative and quantitative analysis of vardenafil by 1 H-NMR [J]. Chin J Pharm Anal,2021, 41(7):1272
[6] 马惠钟,杨宏天,王和欣,等. 核磁共振定量法测定连翘苷的绝对含量[J]. 药物分析杂志,2022,42(5):913
MA HZ, YANG HT, WANG HX, et al. Quantitative determination of phillyrin by qNMR [J]. Chin J Pharm Anal, 2022, 42(5):913
[7] 中华人民共和国药典 2020 年版.四部[S] 2020:52
Ch P 2020. Vol Ⅳ[S]. 2020:52
[8] 曹伶俐,杨宁辉,张智强. 氢核磁共振定量法测定盐酸伊托必利片含量[J]. 化学研究与应用,2019,31(8):1548
CAO LL, YANG NH, ZHANG ZQ. Quantitative nuclear magnetic resonance to determine the content of itopride hydrochloride tables[J]. Chem Res Appl, 2019, 31(8):1548
[9] 霍美娣,雷勇胜,蒋庆峰,等. 右佐匹克隆的波谱分析及结构确证[J]. 中南药学,2017,15(1):39
HUO MD, LEI YS, JIANG QF, et al. Spectral analysis and structure identification of dexzopiclone[J]. Cent South Pharm,2017, 15(1):39
[10] 刘惠军,吴丽红. 佐匹克隆原料及片剂有关物质的HPLC测定[J]. 中国药学杂志,2008,43(12):954
LIU HJ, WU LH. Determination of related substances of zopiclon and its tablets by HPLC[J]. Chin Pharm J, 2008, 43(12):954
[11] 中华人民共和国药典2020年版.二部[S]. 2020:197
Ch P 2020. Vol Ⅱ[S]. 2020:197
[12] HOLZGRABE U, DEUBNER R, SCHOLLMAYER C, et al. Quantitative NMR spectroscopy-applications in drug analysis[J]. J Pharm Biomed Anal, 2005, 38(5):806
[13] 马晓丽,邹萍萍,雷伟,等. 定量核磁技术参数的优化及其在中草药定量分析领域的应用[J]. 药学学报,2014,49(9):1248
MA XL, ZOU PP, LEI W, et al. Optimization of experimental parameters for quantitative NMR (qNMR)and its application in quantitative analysis of traditional chinese medicines[J]. Acta Pharm Sin, 2014, 49(9):1248
[14] 李铮,季加威,杜小伟,等. 款冬花及蜜款冬花HPLC特征图谱和一测多评分析方法建立和应用[J]. 药物分析杂志,2023,43(12):2053
LI Z, JI JW, DU XW, et al. Establishment and application of HPLC characteristic chromatogram and determination by QAMS for Farfarae Flos and honeyed Farfarae Flos[J]. Chin J Pharm Anal, 2023, 43(12):2053
文章导航

/