| 固相萃取/定量核磁共振波谱法测定乳增宁胶囊中的淫羊藿苷 |
| 点此下载全文 |
|
| 基金项目:国家自然科学基金项目(31671928);上海市自然科学基金项目(15ZR1440800) |
|
| 中文摘要:建立了固相萃取(SPE)/定量核磁共振波谱(qNMR)无标样测定乳增宁胶囊中有效成分淫羊藿苷含量的方法。样品用10%乙醇室温下超声提取，以HC-C18型SPE柱对提取液进行浓缩除杂后，用qNMR测定淫羊藿苷的含量。考察了超声时间、SPE样品前处理条件以及定量核磁共振实验条件对定量结果的影响。选择氘代二甲基亚砜为溶剂，2,3,5-三碘苯甲酸为内标，并用基准试剂邻苯二甲酸氢钾对其进行标定。选择脉冲宽度P1=14.1 μs，扫描次数NS=256为qNMR定量淫羊藿苷的实验条件。淫羊藿苷的定量峰为δ 7.9(2,6-H,d,2H)。结果显示，所建方法的日内精密度RSD为0.43%，日间精密度RSD为0.75%，淫羊藿苷与2,3,5-三碘苯甲酸峰面积比与质量比的零截距标准曲线的线性相关系数为0.999 9，且斜率与理论值相符。该法测定淫羊藿苷的LOD为0.122 mg/g；LOQ为0.368 mg/g。样品经SPE预处理后淫羊藿苷的回收率为99.8%~103.0%。可在不用对照品的情况下对乳增宁胶囊中淫羊藿苷的含量进行测定。 |
| 中文关键词:定量核磁共振波谱法 固相萃取 淫羊藿苷 乳增宁胶囊 |
| |
| Determination of Icariin in Ruzengning Capsule by Solid Phase Extraction/Quantitative Nuclear Magnetic Resonance Spectroscopy |
|
|
| Abstract:The quantitative nuclear magnetic resonance spectroscopy(qNMR)method for the determination of icariin in Ruzengning capsule was established based on solid phase extraction(SPE).The sample powder in capsule was ultrasonically extracted using 10%alcohol as solvent at room temperature.The extraction solution was enriched and cleaned with an HC-C18 SPE cartridge.The effects of ultrasonic extraction and SPE,qNMR experimental conditions were investigated.The qNMR experiment conditions were selected as follows：using deuterated DMSO as solvent,2,3,5-triiodobenzoate as internal standard,a P1(pulse width)of 14.1 μs,and a NS(number of scan)of 256.The 1H NMR peak of δ 7.9(2,6-H,d,2H)of icariin was chosen as the quantitative peak.Method validation was performed with the intra-day RSD of 0.43%and the inter-day RSD of 0.75%.The linear correlation coefficient(r)was 0.999 9 between the peak area ratio and mass ratio of icariin to internal standard.LOD was 0.122 mg/g and LOQ was 0.368 mg/g.The recoveries of the SPE-qNMR were in the range of 99.8%-103.0%.The result showed that the method was stable,accurate and reliabile.With no need of icariin standard,the method was applied in the determination of icariin in 3 batches of real Ruzengning capsule. |
| Key Words:quantitative nuclear magnetic resonance solid phase extraction icariin Ruzengning capsule |
| 引用本文：刘晓婷，李苗苗，肖坤，郭强胜，许旭.固相萃取/定量核磁共振波谱法测定乳增宁胶囊中的淫羊藿苷[J].分析测试学报,2018,37(4):452-458. |
| 摘要点击次数: 1749 |
| 全文下载次数: 812 |
| 查看全文 下载PDF阅读器 |
|
|
|
|
|
