紫外光谱法快速测定醒脑静注射液一次提取过程中9种成分(1)
[摘要] 该研究建立了一种基于紫外光谱的醒脑静注射液一次提取过程分析方法，用于快速测定蒸馏提取液中异佛尔酮、4-亚甲基-异佛尔酮、莪术双环烯酮、莪术烯醇、莪术二酮、莪术酮、莪术呋喃二烯酮、莪术醇、吉马酮9种成分含量。在醒脑静注射液一次提取过程中收集郁金-栀子水蒸气蒸馏液样品166份，扫描紫外光谱，并用高效液相色谱测定9种成分含量，使用最小二乘支持向量机和径向基人工神经网络等方法建立紫外光谱与各成分含量之间的多元校正模型。实验结果表明，该研究建立的紫外光谱分析方法能较准确地测定蒸馏提取液中9种成分含量，预测误差均方根分别为0.068， 0.147， 0.215， 0.319， 1.01， 1.27， 0.764， 0.147， 0.610 mg·L-1。该方法具有快速、简便、低成本的优点，有助于醒脑静注射液提取过程监测和提取终点判断，减少产品质量缺陷和质量差异。
[关键词] 醒脑静注射液； 紫外光谱； 过程分析； 郁金； 栀子； 水蒸气蒸馏； 支持向量机； 人工神经网络
, http://www.100md.com
[Abstract] In this study， an analytical method based on ultraviolet spectroscopy was established for the rapid determination of nine components including isophorone， 4-methylene-isophorone， curcumenone， curcumenol， curdione， curzerenone， furanodienone， curcumol and germacrone in the first extraction process of Xingnaojing injection. 166 distillate samples of Gardeniae Fructus and Radix Curcumae were collected in the first extraction process of Xingnaojing injection. The ultraviolet spectra of these samples were collected， and the contents of the nine components in these samples were determined by high performance liquid chromatography. Least squares support vector machine and radial basis function artificial neural network were used to establish the multivariate calibration models between the ultraviolet spectra and the contents of the nine components. The results showed that the established ultraviolet spectrum analysis method can determine the contents of the nine components in the distillates accurately， with root mean square error of prediction of 0.068， 0.147， 0.215， 0.319， 1.01， 1.27， 0.764， 0.147， 0.610 mg·L-1， respectively. This proposed method is a rapid， simple and low-cost tool for the monitoring and endpoint determination of the extraction process of Xingnaojing injection to reduce quality defects and variations.
, 百拇医药
[Key words] Xingnaojing injection； ultraviolet spectroscopy； process analysis； Curcumae Radix； Gardeniae Fructus； hydrodistillation； least squares support vector machine； radial basis function artificial neural network
醒腦静注射液是由麝香、郁金、栀子、冰片4味中药制成的注射剂，具有清热泻火、凉血解毒、开窍醒脑的功效，临床上主要用于中风、脑缺血、意识障碍、急性酒精中毒等病症[1-2]，是年销售额超20亿元的中药大品种。该注射液生产中采用水蒸气蒸馏法对药材中挥发性成分进行提取。首先将郁金、栀子加水进行第一次蒸馏提取，收集蒸馏液，然后将麝香加入蒸馏液中，并加水进行第二次蒸馏提取。以水蒸气蒸馏法提取这些药材中的挥发性成分具有杂质提取量少的优点，但生产中存在提取时间长、能耗高、提取物批次间质量差异大等问题。
目前对醒脑静注射液的分析方法研究主要集中于成品质量检测[3-5]，测定麝香酮、龙脑以及源于郁金的倍半萜类生物活性成分[6]，如莪术双环烯酮、莪术烯醇、莪术二酮等[4]。此外，本课题组前期研究发现醒脑静注射液中源于栀子的2种主要成分为异佛尔酮和4-亚甲基-异佛尔酮，并建立了高效液相色谱(HPLC)分析方法用于测定一次提取过程中间体(即郁金-栀子蒸馏液)中源于栀子的这2种成分及源于郁金的7种倍半萜类成分(莪术双环烯酮、莪术烯醇、莪术二酮、莪术酮、莪术呋喃二烯酮、莪术醇、吉马酮)[7]。, 百拇医药(黄凯毅 魏丹妮 方金阳 李晞瑗 严斌俊)
[关键词] 醒脑静注射液； 紫外光谱； 过程分析； 郁金； 栀子； 水蒸气蒸馏； 支持向量机； 人工神经网络
, http://www.100md.com
[Abstract] In this study， an analytical method based on ultraviolet spectroscopy was established for the rapid determination of nine components including isophorone， 4-methylene-isophorone， curcumenone， curcumenol， curdione， curzerenone， furanodienone， curcumol and germacrone in the first extraction process of Xingnaojing injection. 166 distillate samples of Gardeniae Fructus and Radix Curcumae were collected in the first extraction process of Xingnaojing injection. The ultraviolet spectra of these samples were collected， and the contents of the nine components in these samples were determined by high performance liquid chromatography. Least squares support vector machine and radial basis function artificial neural network were used to establish the multivariate calibration models between the ultraviolet spectra and the contents of the nine components. The results showed that the established ultraviolet spectrum analysis method can determine the contents of the nine components in the distillates accurately， with root mean square error of prediction of 0.068， 0.147， 0.215， 0.319， 1.01， 1.27， 0.764， 0.147， 0.610 mg·L-1， respectively. This proposed method is a rapid， simple and low-cost tool for the monitoring and endpoint determination of the extraction process of Xingnaojing injection to reduce quality defects and variations.
, 百拇医药
[Key words] Xingnaojing injection； ultraviolet spectroscopy； process analysis； Curcumae Radix； Gardeniae Fructus； hydrodistillation； least squares support vector machine； radial basis function artificial neural network
醒腦静注射液是由麝香、郁金、栀子、冰片4味中药制成的注射剂，具有清热泻火、凉血解毒、开窍醒脑的功效，临床上主要用于中风、脑缺血、意识障碍、急性酒精中毒等病症[1-2]，是年销售额超20亿元的中药大品种。该注射液生产中采用水蒸气蒸馏法对药材中挥发性成分进行提取。首先将郁金、栀子加水进行第一次蒸馏提取，收集蒸馏液，然后将麝香加入蒸馏液中，并加水进行第二次蒸馏提取。以水蒸气蒸馏法提取这些药材中的挥发性成分具有杂质提取量少的优点，但生产中存在提取时间长、能耗高、提取物批次间质量差异大等问题。
目前对醒脑静注射液的分析方法研究主要集中于成品质量检测[3-5]，测定麝香酮、龙脑以及源于郁金的倍半萜类生物活性成分[6]，如莪术双环烯酮、莪术烯醇、莪术二酮等[4]。此外，本课题组前期研究发现醒脑静注射液中源于栀子的2种主要成分为异佛尔酮和4-亚甲基-异佛尔酮，并建立了高效液相色谱(HPLC)分析方法用于测定一次提取过程中间体(即郁金-栀子蒸馏液)中源于栀子的这2种成分及源于郁金的7种倍半萜类成分(莪术双环烯酮、莪术烯醇、莪术二酮、莪术酮、莪术呋喃二烯酮、莪术醇、吉马酮)[7]。, 百拇医药(黄凯毅 魏丹妮 方金阳 李晞瑗 严斌俊)