| Hesleya amabilis is a traditional Chinese medicine which could treat coronary heart disease and gastroenteritis, bronchitis and other diseases.It has analgesic, antibacterial, anti-inflammatory, heat detoxification and other pharmacological effects. Due to the low hemsleyin extraction rate and content of Yunnan Yizhihao Pharmaceutical Co. Ltd., so the main content of this paper is to improve the relevant technology.Because the acquisition of a number of pharmaceutical raw materials need to be separate and extraction and the product is obtained before content analysis of raw materials, but the analysis process is too loug which seriously affect the purchase of raw materials. Therefore, this study aims to improve the extraction rate and content of hemsleyin, and establish a short time and reliable detection method of hemsleyin which provide a theoretical basis and techniical reference for the actual production. This paper research on the extraction process improvement and new methods of detection of hemsleyin raw materials. The main research contents are as follows:Chapter 1 Improvement on the extraction technology of hemsleinUltrasound can destroy the cell walls of plants or cell swelliug which could make solvent extraction process to enter plant cells, and thus speediug up the extraction speed and improve the extraction efficiency. This study uses water as leachiug agent, and Hesleya amabilis root was pretreatment by ultrasonic.The optimum conditions of ultrasonic: Hesleya amabilis root pass 60 mesh sieve, and at a temperature of 55 ℃ and the solution under the condition of pH 4, ultrasound 90min. In hemsleyin prior to crystallization, it was treated by water and ultrasonic which can reduce the solubility of hemsleyin. Compariug with chromatography and Yunnan Yizhihao Pharmaceutical Co. Ltd. hemsleyin pigment extraction crystallization time, crystallization time of this study is shortened 22h; Purification of hemsleyin with acetone instead of ethanol, and the conditions of purification process:the volume of acetone is 5 times the amount of hemsleyin, refluxiug temperature is 58 ℃, time is 20min.Compariug with ethanol purification method, the content of hemsleyin increased by 7.56%. In this experiment, the extraction rate and content of hemsleyin were 1.46% and 90.31%.Compariug with chromatography and Yunnan Yizhihao Pharmaceutical Co. Ltd. hemsleyin pigment extraction, the extraction rate and content were increased by 44.6%,5.81%,9.85% and 12.54%, and crystallization time of this study is shortened 4 times。Chapter 2 Determination of Hemsleyin in Hesleya amabilis by Vortex assisted supramolecular solvent extraction (VA-SUPRASs) combined with high performance liquid chromatographyThis study break usiug a siugle organic solvent as extraction solvent extraction technology of vortex assisted supramolecular agent tradition method, and new supramolecular composite solvent was selected as the extractant, combiniug with high performance liquid chromatography method in hemsleyin of Hesleya amabilis content detection. The technique can shorten the detection time snow bravery element. After VA-SUPRASs extraction optimum condition was obtained:the optimization solution of butanol and tetrahydrofuran as the ratio of 2:1 as supramolecular solvent, optimum extraction dose was 70 uL, vortex 4min, centrifugal extraction system 3500rpm 5min, pH=7.0. VA-SUPRASs extraction of hemsleyin recoveries between 90.12-100.32%, the extraction rate and content of hemsleyin were 1.39% and 84.62%,and they increased 2.2% and 2.9% than Yunnan Yizhihao Pharmaceutical Co. Ltd. Xuedan raw material detection method.The detection and analysis time of hemsleyin is shortened by 44h.Chapter 3 Vortex-assisted dispersive liquid-liquid micro extraction(VA-DLLME) combined with high performance liquid chromatography for determination of Hemsleyin A in Hesleya amabilisIn this study, nonanoic acid was regarded as extractant, and hemslecin n he-nasleya.sinesis cogn was extracted by vortex assisted liquid-liquid micro extraction (VA-DLLME).Due to not usiug organic dispersant, the enrichment factor was greatly improved and the system limit of detection was reduced. Finally high performance liquid chromatography was used to determine hemslecin content and the accuracy detectionand sensitivity were raised.The optimum conditions of VA-DLLME was:60 μL (v/v) nonanoic acid, vortex 3min and centrifuged at 3500 rpm for 5 min,pH=4.0; VA-DLLME extraction of hemsleyin recoveries between 88.55-99.17%, extraction of bile pigment and snow extraction rate were respectively 1.36% and 94.3%, increased 1.1% and 1.3% than than Yunnan Yizhihao Pharmaceutical Co. Ltd, raw material detection time is reduced by 42h. |
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