[Objectives] This study was conducted to optimize the ethanol extraction technology of monoester alkaloids from Radix Aconiti Preparata. [Methods]On the basis of defined extraction times,ethanol concentration,ethanol ...[Objectives] This study was conducted to optimize the ethanol extraction technology of monoester alkaloids from Radix Aconiti Preparata. [Methods]On the basis of defined extraction times,ethanol concentration,ethanol times and extraction time were investigated by HPLC-MS combined with orthogonal test to optimize extraction process using the content of monoester alkaloids( the sum of benzoyl neoaconitine,benzoyl hypoaconitine and benzoyl aconitine) as an index.[Results]The optimum ethanol extraction technology was as follows: 75% ethanol,ethanol amount 25 times of the medicinal material,and each extraction for 1. 5 h.[Conclusions] The optimal extraction technology is simple,feasible,stable and reliable. It can provide reference for the industrial production and quality control of monoester alkaloids from Radix Aconiti Preparata.展开更多
目的建立RP-HPLC法同时测定骨刺消痛胶囊中3种单酯型生物碱含量。方法色谱柱为Inert Sustain C18柱(5μm,4.6 mm×250 mm);流动相A为乙腈-四氢呋喃(25∶8),流动相B为0.1mol·L-1醋酸铵溶液(每1000 m L加冰醋酸0.5 m L),梯度洗脱...目的建立RP-HPLC法同时测定骨刺消痛胶囊中3种单酯型生物碱含量。方法色谱柱为Inert Sustain C18柱(5μm,4.6 mm×250 mm);流动相A为乙腈-四氢呋喃(25∶8),流动相B为0.1mol·L-1醋酸铵溶液(每1000 m L加冰醋酸0.5 m L),梯度洗脱;流速:1.0 m L·min-1;检测波长:234nm;柱温:30℃。结果苯甲酰新乌头原碱在进样量为0.0246~0.615μg与峰面积具有良好的线性关系(r=0.9997),低、中、高浓度平均加样回收率分别为96.8%、98.9%、97.8%,RSD分别为0.94%、0.88%、0.95%;苯甲酰乌头原碱在进样量为0.0987~2.4675μg与峰面积具有良好的线性关系(r=0.9999),低、中、高浓度平均加样回收率分别为100.1%、99.8%、100.3%,RSD分别为0.43%、0.25%、0.19%;苯甲酰次乌头原碱在进样量为0.0118~0.295μg与峰面积具有良好的线性关系(r=0.9998),低、中、高浓度平均加样回收率分别为97.7%、99.8%、98.1%,RSD分别为0.91%、1.2%、0.97%。结论本方法操作简便、灵敏度高、重复性好,结果准确,可作为骨刺消痛胶囊中单酯型生物碱的含量测定方法。展开更多
基金Supported by Traditional Chinese Medicine Science and Technology Development Program of Shandong Province (2017-1982019-0400)Major Science and Technology Innovation Project of Shandong Province (2018CXGC1304)。
文摘[Objectives] This study was conducted to optimize the ethanol extraction technology of monoester alkaloids from Radix Aconiti Preparata. [Methods]On the basis of defined extraction times,ethanol concentration,ethanol times and extraction time were investigated by HPLC-MS combined with orthogonal test to optimize extraction process using the content of monoester alkaloids( the sum of benzoyl neoaconitine,benzoyl hypoaconitine and benzoyl aconitine) as an index.[Results]The optimum ethanol extraction technology was as follows: 75% ethanol,ethanol amount 25 times of the medicinal material,and each extraction for 1. 5 h.[Conclusions] The optimal extraction technology is simple,feasible,stable and reliable. It can provide reference for the industrial production and quality control of monoester alkaloids from Radix Aconiti Preparata.
文摘目的建立RP-HPLC法同时测定骨刺消痛胶囊中3种单酯型生物碱含量。方法色谱柱为Inert Sustain C18柱(5μm,4.6 mm×250 mm);流动相A为乙腈-四氢呋喃(25∶8),流动相B为0.1mol·L-1醋酸铵溶液(每1000 m L加冰醋酸0.5 m L),梯度洗脱;流速:1.0 m L·min-1;检测波长:234nm;柱温:30℃。结果苯甲酰新乌头原碱在进样量为0.0246~0.615μg与峰面积具有良好的线性关系(r=0.9997),低、中、高浓度平均加样回收率分别为96.8%、98.9%、97.8%,RSD分别为0.94%、0.88%、0.95%;苯甲酰乌头原碱在进样量为0.0987~2.4675μg与峰面积具有良好的线性关系(r=0.9999),低、中、高浓度平均加样回收率分别为100.1%、99.8%、100.3%,RSD分别为0.43%、0.25%、0.19%;苯甲酰次乌头原碱在进样量为0.0118~0.295μg与峰面积具有良好的线性关系(r=0.9998),低、中、高浓度平均加样回收率分别为97.7%、99.8%、98.1%,RSD分别为0.91%、1.2%、0.97%。结论本方法操作简便、灵敏度高、重复性好,结果准确,可作为骨刺消痛胶囊中单酯型生物碱的含量测定方法。