固相萃取-定量核磁共振波谱法测定板蓝根饮片中的表告依春
发布时间：2019-05-17 11:13
【摘要】：建立了固相萃取(SPE)-定量核磁共振波谱(qNMR)技术测定板蓝根饮片中有效成分表告依春含量的方法。样品用水超声提取两次,采用SPE对提取液进行富集浓缩,用q NMR测定表告依春的含量。考察了样品预处理和qNMR实验条件对测定结果的影响,选择氘代二甲基亚砜为溶剂,用基准试剂邻苯二甲酸氢钾标定的2,3,5-三碘苯甲酸为内标,选择脉冲宽度P_1=14.1μs,延迟时间d_1=5 s,扫描次数N_S=256为qNMR定量测定表告依春的最佳实验条件。表告依春的定量峰为δ5.365~5.399(H-7b,d,1H)。结果表明,日内测量精密度(RSD)为0.5%,日间精密度为0.8%,表告依春与三碘苯甲酸峰面积比与质量比的零截距标准曲线线性相关系数为0.9991,且斜率与理论值相符。根据响应值标准偏差和标准曲线斜率法确定此法测定表告依春的检测限(LOD)为0.05 mg/g;定量限(LOQ,S/N≥150)为0.19 mg/g。包括样品提取过程的表告依春的回收率为97.4%~101.7%。采用本方法测定板蓝根饮片中的表告依春的含量为0.19~1.26 mg/g。研究结果表明,采用SPE进行富集,扩大了q NMR的应用范围,可用于低含量复杂样品的定量分析。
[Abstract]:A solid-phase extraction (SPE)-quantitative nuclear magnetic resonance spectroscopy (qNMR) technique was established to determine the content of indigowoad root in Radix Isatidis decoction pieces. The sample was extracted twice with water, and the extract was concentrated by SPE, and the content of Eichun was determined by q-NMR. The effect of sample pretreatment and qNMR experiment conditions on the determination results was studied. The determination of the effect of the sample pretreatment and qNMR experiment conditions on the determination results was studied. The 2,3,5-triiodobenzoic acid was used as the internal standard, and the pulse width, P _ 1 = 14.1. m, and the delay time d _ 1 = 5 s, were chosen as the internal standard. The number of scans N _ S = 256 is the best experimental condition for qNMR quantitative determination of Eichun. The quantitative peak of Eichun was 5.365-5.399 (H-7b, d, 1H). The results showed that the RSD was 0.5% and the day-day precision was 0.8%. The linear correlation coefficient of the peak area ratio of Eichun to triiodobenzoic acid and the mass ratio was 0.9991, and the slope was in line with the theoretical value. The detection limit (LOD) for the determination of Eichun according to the standard deviation of the response and the slope of the standard curve was 0.05 mg/ g; the limit of quantitation (LOQ, S/ N-150) was 0.19 mg/ g. And the recovery rate of the epideochun, which comprises the sample extraction process, is 97.4% to 101.7%. The content of the epidesulin in the radix isatidis decoction pieces is determined to be 0.19 to 1.26 mg/ g by the method. The results show that the application range of q-NMR is expanded by SPE, and can be used for quantitative analysis of complex samples with low content.
【作者单位】： 上海应用技术大学化学与环境工程学院;
【基金】：国家自然科学基金项目(No.31671928) 上海市自然科学基金项目(No.15ZR1440800)资助~~
【分类号】：O657;R286.0
本文编号：2479049
[Abstract]:A solid-phase extraction (SPE)-quantitative nuclear magnetic resonance spectroscopy (qNMR) technique was established to determine the content of indigowoad root in Radix Isatidis decoction pieces. The sample was extracted twice with water, and the extract was concentrated by SPE, and the content of Eichun was determined by q-NMR. The effect of sample pretreatment and qNMR experiment conditions on the determination results was studied. The determination of the effect of the sample pretreatment and qNMR experiment conditions on the determination results was studied. The 2,3,5-triiodobenzoic acid was used as the internal standard, and the pulse width, P _ 1 = 14.1. m, and the delay time d _ 1 = 5 s, were chosen as the internal standard. The number of scans N _ S = 256 is the best experimental condition for qNMR quantitative determination of Eichun. The quantitative peak of Eichun was 5.365-5.399 (H-7b, d, 1H). The results showed that the RSD was 0.5% and the day-day precision was 0.8%. The linear correlation coefficient of the peak area ratio of Eichun to triiodobenzoic acid and the mass ratio was 0.9991, and the slope was in line with the theoretical value. The detection limit (LOD) for the determination of Eichun according to the standard deviation of the response and the slope of the standard curve was 0.05 mg/ g; the limit of quantitation (LOQ, S/ N-150) was 0.19 mg/ g. And the recovery rate of the epideochun, which comprises the sample extraction process, is 97.4% to 101.7%. The content of the epidesulin in the radix isatidis decoction pieces is determined to be 0.19 to 1.26 mg/ g by the method. The results show that the application range of q-NMR is expanded by SPE, and can be used for quantitative analysis of complex samples with low content.
【作者单位】： 上海应用技术大学化学与环境工程学院;
【基金】：国家自然科学基金项目(No.31671928) 上海市自然科学基金项目(No.15ZR1440800)资助~~
【分类号】：O657;R286.0
【相似文献】
相关期刊论文 前1条
1 梁丽丽;王英姿;李环环;孙秀梅;;板蓝根饮片的浸润切制工艺优选[J];中国实验方剂学杂志;2012年21期
，本文编号：2479049
本文链接：https://www.wllwen.com/kejilunwen/huaxue/2479049.html
教材专著
