氢核磁定量分析技术测定人参皂苷Rd对照品含量的研究
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摘要
建立了氢核磁定量技术准确、快速测定人参皂苷Rd对照品含量的方法。考察了核磁共振实验条件对测定结果的影响。选择混合溶剂氘代DMSO-d6∶D2O(9∶1,V/V)为溶剂,苯甲酸为内标,观测频率400.13 MHz,脉冲延迟时间5 s,采样次数32次,采集人参皂苷Rd和苯甲酸内标混合物的1H NMR谱图。定量峰为苯甲酸2位和6位质子信号δ7.94,人参皂苷Rd 24位质子信号δ5.07。结果表明,氢核磁定量测定的线性相关系数R=0.997 8,精密度相对标准偏差为0.65%,回收率分别为98.69%~102.54%,相对标准偏差为1.92%,说明该方法准确性良好。实际测定3批人参皂苷Rd的质量分数分别为98.87%,98.79%和98.92%。氢核磁定量技术测得对照品的质量分数略低于HPLC的面积归一化法。该方法无需待测物对照品,且对检测样品无破坏性、重现性好,可用于人参皂苷Rd对照品的含量测定和质量控制。
To establish an accurate and rapid method for content determination of ginsenoside Rd with quantitative1 H NMR. Benzoic acid served as internal standard,DMSO-d6 and D2 O(9:1,V/V) as solution.1 H NMR spectra of the mixture of ginsenoside Rd and benzoic acid were acquired with spectrometer frequency 400. 13 MHz scanning 32 times,relaxation delay time 4 s. Ginsenoside Rd proton peak atδ 5. 07 and benzoic acid signal δ 7. 94 served as quantification peaks. Linear regression equation of correlation coefficient of 0. 997 8,RSD of precision were less than 0. 65%,the average recoveries were in the range of 98. 69% to 102. 54% with RSD less than 1. 92%. The contents of 3 batches of ginsenoside Rd were 98. 87%,98. 79% and 98. 92%. Experimental results show that the concentration of quantitative1 H NMR determined ginsenoside Rd is slightly lower than that by HPLC without reference substance. The method is simple,accurate,and has good application value,can be used for the content determination and quality control of ginsenoside Rd.
To establish an accurate and rapid method for content determination of ginsenoside Rd with quantitative1 H NMR. Benzoic acid served as internal standard,DMSO-d6 and D2 O(9:1,V/V) as solution.1 H NMR spectra of the mixture of ginsenoside Rd and benzoic acid were acquired with spectrometer frequency 400. 13 MHz scanning 32 times,relaxation delay time 4 s. Ginsenoside Rd proton peak atδ 5. 07 and benzoic acid signal δ 7. 94 served as quantification peaks. Linear regression equation of correlation coefficient of 0. 997 8,RSD of precision were less than 0. 65%,the average recoveries were in the range of 98. 69% to 102. 54% with RSD less than 1. 92%. The contents of 3 batches of ginsenoside Rd were 98. 87%,98. 79% and 98. 92%. Experimental results show that the concentration of quantitative1 H NMR determined ginsenoside Rd is slightly lower than that by HPLC without reference substance. The method is simple,accurate,and has good application value,can be used for the content determination and quality control of ginsenoside Rd.
引文
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[15]耿岩玲,马然,刘伟,等.核磁共振内标法测定苏丹红I对照品的含量[J].山东科学,2013,26(5):11-13.
[16]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):1248-1257.
[2]黎阳,张铁军,刘素香,等.人参化学成分和药理研究进展[J].中草药,2009,40(1):164-166.
[3]高俊杰,翟延君,王荣祥,等.石柱参中8种人参皂苷的含量测定[J].中国中药杂志,2010,35(8):989-991.
[4]张金秋,夏娟,孙光芝,等.RP-HPLC法测定人参花中11个人参皂苷含量[J].药物分析杂志,2015,35(9):1596-1600.
[5]胡紫艳,孙夏荣,史达,等.UPLC同时测定脑安颗粒中6种人参皂苷类成分的含量[J].中国职业药师,2016,13(12):28-31.
[6]许丹丹,杜纳纳,耿一玄,等.HPLC-ELSD测定柴胡加龙骨牡蛎汤改善睡眠有效部分中5种皂苷类成分的含量[J].中国药学杂志2017,52(10):861-864.
[7]李月茹,王艳红,杨秀伟,等.高效液相色谱串联质谱法分析紫红参中人参皂苷类成分[J].药物分析杂志,2013,33(5):812-817.
[8]高红梅,王志伟,闫慧娇,等.氢核磁定量分析技术的研究进展[J].山东化工,2016,45(22):60-62.
[9]易进海,刘云华,陈燕,等.核磁共振波谱法测定藁本内酯对照品的含量[J].药物分析杂志,2010,30(4):680-682.
[10]禹珊,郭强胜,王会琳,等.定量核磁共振波谱法同时测定中药虎杖中白藜芦醇和虎杖苷的含量[J].分析化学,2015,43(1):69-74.
[11]仙云霞,耿岩玲,周洪雷,等.核磁共振内标法测定覆盆子酮对照品的含量[J].山东科学,2015,28(1):76-11.
[12]The United States Pharmacopoeia Commission.United States Pharmacopoeia[M].US:US Pharmacopoeia Convention,Inc.,2000:1221-1222.
[13]European Pharmacoloeia Commission.European Pharmacoloeia[M].8th ed.Strashourg:European Directorate for the Quality of Medicines and Health Care of the Council of Europe,2013:52-55,109.
[14]国家药典委员会.中华人民共和国药典2010年版一部[M].北京:中国医药科技出版社,2010:1208.
[15]耿岩玲,马然,刘伟,等.核磁共振内标法测定苏丹红I对照品的含量[J].山东科学,2013,26(5):11-13.
[16]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):1248-1257.