| This topic in the State Administration of traditional Chinese medicine industry research and special "Epimedium different cooked with pieces in clinical practice using qualitative research" (project number NO.20110700717) basis, to at the beginning of the study the collected samples difficult to carry out accurate base original and identify the origin as the breakthrough point, combined with TCM formula granule for supplement of Chinese herbal medicine, using near infrared spectroscopy technology (hereinafter referred to as NIR) has, quantitative and monitor the production process characteristics, intends to carry on systematic research to the Yinyanghuo granules by NIR and TCM formula granule realize online real-time monitoring to provide the basic research.Objective1. Using infrared diffuse reflectance technique to establish discriminative model for Epimedium from different origins and origin, for rapidly identification of the origins and origin of Epimedium to ensure its quality from the source;2. Using near infrared diffuse reflectance technique to establish content detection model for Epimedium herbs, pieces, dry extract powder as well as formula granule for rapid detection of indicated components and water content;3. Using near infrared intelligent transmission technology to establish model to determine Epimedium extract, concentrated extract, extract end point and concentrated end point, to allow rapid determination of the extract end point and concentrate end point, so as to achieve real-time monitoring during production process.MethodCombine literature research, chemical determination, spectral measurement and computer technology to carry out the quality control of Epimedium granule production process.1. Infrared spectroscopic technology is used to acquire spectral information from different origins, regions, batches of Epimedium, in addition computer model is used to establish a qualitative model, then using unknown sample to test identification ability of the model, and the results were compared to that from the traditional identification methods to investigate whether the near infrared spectroscopic technology is able to differentiate Epimedium collected from different origins and regions;2. Using near infrared spectroscopic technology to acquire spectral information from each batch of Epimedium, tablet, granule, while processing via the computer model to establish a determination model, then using multiply batches of unknown sample to test identification ability of the model, and comparing the results to that from HPLC, so as to decide whether near infrared spectroscopic technology is able to accurately determine indicated content of Epimedium;3. Using near infrared spectroscopic technology to acquire spectral information from Epimedium extract, concentrated extract and dry extract powder, while using computer model to establish a quantitative measurement model, then using multiple batches of unknown samples to test identification ability of the model, while compare the results to that from HPLC, to decide whether near infrared spectroscopic technology is able to accurately determine the concentrated end point of Epimedium.Result1. In different Epimedium species identification model, set of Epimedium, set of Korean Epimedium, set of Epimedium sagittatum and set of Epimedium pubescens Maxim are independent species, and there is no intersection,10 unknown samples,7 positive controls and 3 negative controls were correctly identified through establishment of Epimedium four species identification model. In Epimedium different origin identification model, no intersection exists in 14 samples, although Mahalanobis distance in the samples in Sichuan Province is small, there are greater Mahalanobis distances among samples from different provinces,10 unknown samples,7 positive controls and 3 negative controls were correctly passed through the identification for the establishment of Epimedium from 14 places;2. In the raw Epimedium herbal determination model, differences exist between near infrared predictive value and chemical determined value.10 records indicate that HPLC determined icariin value is 1.2640?6.1536 mg·g-1,while NIR determined value is 1.0816?6.2933 mg·g-1, the average difference is±0.3107 mg·g-1; UV Spectrophotometer determined value of epimedium total flavonoids is 64.6119? 85.4800 mg·g-1, while NIR determined value is 59.2349?89.7321 mg·g-1, the average difference is ±4.5718 mg·g-1; drying method determined value of water content is 10.46%?11.86%; while NIR determined value is 10.95%?11.91%, the average difference is ±0.377%. In the Epimedium herb pieces determination model, 10 records indicate that HPLC determined value of Epimedium herb pieces is 2.8859?7.6657 mg·g-1, while NIR determined value is 2.4857?7.8972 mg·g-1, the average difference is ±0.2562 mg·g-1; Determined value of Baohuoside by IHPLC is 0.3242?1.4676 mg·g-1, while determined by NIR is 0.3509?1.4533 mg·g-1, the average difference is ±0.0642 mg·g-1; drying method determined value of water content is 3.38%?5.34%, NIR determined value is 3.44%?5.33%, the average difference is ±0.144%;3. In the extraction end point determination model of Epimedium herb pieces, 10 records indicate the first extract of icariin determined value by HPLC is 26.9788? 111.5537 mg·L-1, NIR determined value is 26.1775?107.3869 mg·L-1, the average difference is ?4.4975mg·L-1, in the second extract of icariin determined value by HPLC is 12.8385?46.0887 mg·L-1, NIR determined value is 0.9775?1.0958 g·ml-1, the average difference is ±0.1505 g·ml-1;4. In the partially prepared products of Epimedium extract power determination model,10 records indicate that HPLC determined value is 21.1089?27.5953 mg·g-1, NIR determined value is 21.0689?27.2844 mg·g-1, the average difference is ±0.2855mg·g-1; drying method determined water content is 2.85%?3.51%, NIR determined value is 2.83%?3.56%, the average difference is ±0.235%. In the complete Epimedium formula granule quantitative determination model,10 records indicate that HPLC determined value is 9.5846?27.4815 mg·g-1, NIR determined value is 9.9510?28.0265 mg·g-1, the average difference is ±0.6520 mg·g-1; drying method determined water content is 3.24%?4.25%, while NIR determined value is 3.43%?4.37%, the average difference is ±0.233%.ConclusionUsing the infrared spectroscopy technology to identify the species and origins of Epimedium has advantages of fast and accuracy, while the whole plant is not required, thus providing new idea and way for TCM identification. Computer model can be established for quantitative content determining on either solid or liquid samples, although difference exists when compared to HPLC, however, the differences are quite small so that determination of contents of Epimedium herbal, tablet, dry extract power as well as finished formula granule are possible. Meanwhile, this technology can also monitor the processes of Epimedium extracting and concentration, determine the indicated contents and density of concentrated extract. In summary, the near infrared spectroscopy technology can be used for monitoring the quality during the whole process of TCM formula granule production, 'herbal material-tablet-extract-concentrate-dry extract-finished product'.Innovation Point1. This topic for the first time using NIR to study the different groups of the original identification, from the source to control the quality of the formula granules;2. This topic for the first time using NIR to determine the end point of the preparation process of the preparation of Herba Herba formula, to achieve the precise control of the production process of the extraction process;3. This topic for the first time using NIR to study the rapid test of the content and water content of the composition of the formula granule of Herba Herba, which can effectively reduce the detection cost and shorten the detection time. |
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