Objective: To determine the absolute content of phillyrin by 1H nuclear magnetic resonance quantitative method(qNMR). Methods: DMSO-d6 and deuterated chloroform (1∶1) were used as the solvent and dimethyl terephthalate (DMT) was used as the internal standard. Through comparing the internal standard peak area of DMT at δ 3.92 and the quantitative peak area of phillyrin at δ 7.06, the absolute content of phillyrin was determined by qNMR. Results: The precision of this method was less than 0.031%, and the linear correlation coefficient was 0.999 9. The content of phillyrinin the sample prepared in our laboratory was within 93.01%-93.32% by qNMR. Conclusion: The NMR quantitative method established in this paper is simple, rapid and accurate, and provides a new method for the determination of phillyrin.
MA Hui-zhong, YANG Hong-tian, WANG He-xin, XIN Xiu-lan, CHEN Liang, LIU Yu-feng, LIU Wen-bao
. Quantitative determination of phillyrin by qNMR*[J]. Chinese Journal of Pharmaceutical Analysis, 2022
, 42(5)
: 913
-916
.
DOI: 10.16155/j.0254-1793.2022.05.21
[1] 姜维. 《黄帝内经》外科疾病理论研究[D].沈阳:辽宁中医药大学, 2016
JIANG W. The Research of Huangdi Neijing Surgical Theory[D].Shenyang:Liaoning University of Traditional Chinese Medicine, 2016
[2] YUAN A, ZHAO MJ, LI Y, et al. The review of pharmacological effects of Lianqiao[J].Pharm Clin Chin Mater Med, 2015, 6(5):56
[3] 付云飞, 李清, 毕开顺. RP-HPLC法同时测定不同产地连翘中的7种成分[J].中草药, 2013, 44(8):1043
FU YF, LI Q, BI KS. Determination of seven components in Forsythia suspensa by RP-HPLC[J].Chin Tradit Herb Drugs, 2013, 44(8):1043
[4] 赵咏梅, 李发荣, 杨建雄, 等. 连翘苷降血脂及抗氧化作用的实验研究[J].天然产物研究与开发, 2005, 17(2):3
ZHAO YM, LI FR, YANG JX, et al. Study on the reducing blood lipid and antioxidition effects of phillyrin[J].Nat Prod Res Dev, 2005, 17(2):3
[5] MALZ F, JANCKE H. Validation of quantitative NMR[J].J Pharm Biomed Anal, 2005, 38:813
[6] HOLZGRABE U, DENBNER R, SCHOLLMAYER C, et al. Quantitative NMR spectroscopy-applications in drug analysis[J].J Pharm Biomed Anal, 2005, 38:806
[7] 杨秀伟. NMR在布地奈德-R结构确定及其产品质量控制上的应用[J].分析测试学报, 2004, 23(5):29
YANG XW. Application of NMR for structure elucidation and quality control of budesonide-R products[J].J Instrum Anal, 2004, 23(5):29
[8] 周晓力, 陈华, 南楠.1H NMR定量测D3-吗啡对照品的含量[J].药物分析杂志, 2020, 40(11):906
ZHOU XL, CHEN H, NAN N. Determination of D3-morphine by 1H NMR[J].Chin J Pharm Anal, 2020, 40(11):906
[9] BHARTI SK, ROY R. Quantitative 1H NMR spectroscopy[J].Trends Anal Chem, 2012, 35:5
[10] 中华人民共和国药典2020年版. 四部[S]. 2020:52
ChP 2020. Vol Ⅳ[S]. 2020:52
[11] 李娜. 质量平衡法与定量核磁法对叶酸与人胰岛素纯度的测定研究[D]北京:北京化工大学, 2017
LI N. The Assessment of Folic Acid and Human Insulin by Mass Blance Method and Quantitative Nuclear Magnetic Resonance Method[D].Beijing:Beijing University of Chemical Technology, 2017
[12] 张芬芬, 蒋孟虹, 沈文斌, 等. 定量核磁共振(QNMR)技术及其在药学领域的应用进展[J].南京师范大学学报(工程技术版), 2014, 14(2):8
ZHANG FF, JIANG MH, SHEN WB, et al. Progress in quantitative nuclear magnetic resonancetechnology in pharmaceutical applications[J].J Nanjing Normal Univ(Eng Technol Ed), 2014, 14(2):8
[13] 黄挺, 张伟, 全灿, 等. 定量核磁共振法研究进展[J].化学试剂, 2012, 34(4):327
HUANG T, ZHANG W, QUAN C, et al. Review on quantitative nuclear magnetic resonance[J].Chem Reagents, 2012, 34(4):327
[14] 唐励静, 文翔昊, 李冲, 等. HPLC同时测定复方金银花颗粒中绿原酸、连翘苷、黄芩苷、汉黄芩素、芹菜素的含量[J].中国实验方剂学杂志, 2014, 20(21):71
TANG LJ, WEN XH, LI C, et al. Simultaneous determination of chlorogenic acid, forsythin, baicalin, wogonin and apigenin in compound Jinyinhua granules by HPLC[J].Chin J Exp Tradit Med Form, 2014, 20(21):71
[15] 王姝君, 李石飞, 张立伟. 连翘含量测定方法优化及青(老)翘质量控制标准建立探讨[J].中国中药杂志, 2018, 43(15):3157
WANG SJ, LI SF, ZHANG LW. Optimization of method for determination of Forsythia Fructus and discussion on the establishment of quality control standard for green (old) Forsythia Fructus[J].China J Chin Mater Med, 2018, 43(15):3157
[16] 徐雪晶, 万向勇, 赵锦漪, 等. 氢核磁共振定量法初探[J].广东化工, 2020, 47(4):104
XU XJ, WAN XY, ZHAO JY, et al. The study on quantitative hydrogen nuclear magnetic resonance[J].Guangdong Chem Ind, 2020, 47(4):104