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Objective:To screen the optimal process of ambi-extracting of Xinyi Powder and inclusion of volatile oil.Methods:Single factor experiment was used to optimize the extraction process of Xinyi Powder by taking crushing particle size, extraction times, the amount of water added and extraction time as the investigation factors. L 9(3 4) orthogonal test was used to optimize the inclusion process of volatile oil in Xinyi Powder. Results:The optimal extraction process of ambi-extracting of Xinyi Powder was as follows: the slices were not crushed, 10 times the amount of water was added, and extracted for 3 hours; the best inclusion process of volatile oil as follows: β-cyclodextrin:water=1:25, β-cyclodextrin:volatile oil=6:1, inclusion temperature 35 ℃, inclusion time 3 hours.Conclusion:The ambi-extracting process and volatile oil inclusion process are simple, stable and feasible.
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Objective: To optimize the extraction technology and inclusion process of volatile oil for Qingxiangrukang Granules (QG). Methods: Box-Behnken was used to optimize the extraction technology of volatile oil in QG. With yield of inclusion compound and inclusion rate of volatile oil-β-CD as evaluation indexes, and with volatile oil-pure water ratio, β-CD-volatile oil ratio, and inclusion time as investigate factors, the optimal inclusion technology for volatile oil of QG was ensured based on PCA-G1-entropy method and orthogonal design and by using colloid milling. Results: The optimum extraction technology of volatile oil were as follows: extracting time was 6 h, liquid-material ratio was 10, immersion was 0 h. The optimal inclusion technology for volatile oil were as follows: pure water-volatile oil ratio was 1:80, β-CD-volatile oil ratio was 6 g, and the inclusion time was 30 min. Under such condition, there was no significant difference between verification groups of three batches. Conclusion: This optimal extraction technology and inclusion process is stable and workable and can provide experimental basis for industrial production of QG.
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Objective To optimize ambi-extracting and inclusion process of volatile oil from Chuanxiong Rhizoma and Angelicae Sinensis Radix. Methods With yield ratio of volatile oil and ferulic acid content in water extract as evaluation indexes, single factor experiments were used to study the extraction process. With the inclusion rate of volatile oil and yield of inclusion as evaluation indexes, saturated aqueous solution was used to L9(34) orthogonal experiments to reach optimum inclusion process. Results The optimum extraction process of Chuanxiong Rhizoma and Angelicae Sinensis Radix was extracted for 8 hours with 8 folds the amount of water, and without soaking. The validation experiments of extraction of volatile oil and ferulic acid content in water extract were 1.23 mL and 0.387 9 mg/g. The optimum conditions of inclusion process were as follows: volatile oil (mL): β-CD (g) was 1:8;inclusion temperature was 40 ℃; inclusion time was 3 hours. The validation experiments of inclusion rate of volatile oil and yield of inclusion were 74.89% and 72.81%. Conclusion Optimum ambi-extracting and inclusion process of volatile oil from Chuanxiong Rhizoma and Angelicae Sinensis Radix are feasible and stable, witch can provide certain supporting data for preparation production.
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Objective To optimize the processes of extraction and inclusion of volatile oil from Citri Grandis Exocarpium. Methods With yield ratio of volatile oil as evaluation index, single factor experiments were used to study the extraction process of volatile oil. With the inclusion rate of the volatile oil and the yield of inclusion as evaluation indexes, saturated aqueous solution was used to the L9(34) orthogonal experiments to reach the best inclusion process optimization. And the microscopic imaging analysis and X-ray scattering technology were adopted to character the inclusion compound. Results The optimum extraction process of volatile oil was extracted for 10 hours with 10 folds the amount of water, and without soaking. The optimum conditions of inclusion process were as follows: volatile oil (mL): β-CD (g): water (mL) ratio was 1:8:80; inclusion temperature was 50 ℃; inclusion time was 3 hour. The validation experiments of the inclusion rate of the volatile oil and the yield of inclusion were 91.50% and 88.36%. Microscopic imaging analysis and X-ray scattering technology proved the inclusion compound had been formed. Conclusion Optimal extraction and inclusion process are feasible and stable, which can provide certain supporting data for preparation and production.
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Objective To optimize the processes of extraction and inclusion of volatile oil from Citri Grandis Exocarpium. Methods With yield ratio of volatile oil as evaluation index, single factor experiments were used to study the extraction process of volatile oil. With the inclusion rate of the volatile oil and the yield of inclusion as evaluation indexes, saturated aqueous solution was used to the L9(34) orthogonal experiments to reach the best inclusion process optimization. And the microscopic imaging analysis and X-ray scattering technology were adopted to character the inclusion compound. Results The optimum extraction process of volatile oil was extracted for 10 hours with 10 folds the amount of water, and without soaking. The optimum conditions of inclusion process were as follows: volatile oil (mL): β-CD (g): water (mL) ratio was 1:8:80; inclusion temperature was 50 ℃; inclusion time was 3 hour. The validation experiments of the inclusion rate of the volatile oil and the yield of inclusion were 91.50% and 88.36%. Microscopic imaging analysis and X-ray scattering technology proved the inclusion compound had been formed. Conclusion Optimal extraction and inclusion process are feasible and stable, which can provide certain supporting data for preparation and production.
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In this paper, tanshinone-ⅡA (Tan-IIA)/β-cyclodextrin (β-CD) inclusion complexes were prepared by saturated aqueous solution method. Based on the single factor experiment, Box-Benhnken design and response surface method were utilized to optimize the preparation procedures of tanshinone-ⅡA/β-cyclodextrin inclusion complexes. The ratio of β-CD to Tan-ⅡA, experimental temperature and time were defined as independent variables, while the yield of the inclusion complexes, encapsulation efficiency and the generalized "normalized value" were set as the response value. In addition, the inclusion complexes were characterized by infrared spectroscopy (IR) and nuclear magnetic resonance (NMR). The results showed that optimum preparation conditions for Tan-ⅡA/β-CD inclusion complex were as follows: Tan-ⅡA/β-CD ratio of 1:7, the temperature of 48 ℃ and the time of 3 h. Under the optimized conditions, the encapsulation efficiency of Tan-ⅡA/β-CD inclusion complex was 84.75%. The Tan-IIA and β-CD inclusion complex can significantly improve the dissolution of Tan-ⅡA.
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Objective: To optimize the inclusion process of volatile oil in Xiao' er Jiegan particle.Methods: β-Cyclodextrin was used as the inclusion material.Orthogonal experiments were performed,and the yield of volatile oil inclusion complex and the inclusion rate of volatile oil were taken as the indices to study the influence of inclusion temperature, inclusion time and the ratio of β-cyclodextrin to volatile oil (g∶ml) on the inclusion process.The β-CD-volatile oil inclusion complex was added to Xiao' er Jiegan particle and the stability studies were conducted as well.Results: The optimum volatile oils inclusion process of Xiao'er Jiegan particle was as follows: the inclusion temperature was 40℃, the inclusion time was 3 h , and the ratio of β-cyclodextrin to volatile oil (g∶ml) was 8∶1.The loss of volatile oil prepared by direct injection method was 51.27% after 6-month storage at room temperature, while that prepared by the inclusion method was only 3.13% after 24-month storage at room temperature.Conclusion: The optimized inclusion process of volatile oil is reasonable and feasible, and the stability of the prepared particle is also promising.
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Objective To optimize the extraction process of mixed volatile oil from Forsythiae Fructus, Saposhnikoviae Radix and Magnoliae Flos and inclusion process of β-cyclodextrin (β-CD). Methods With yield ratio of volatile oil as evaluation index, single factor experiments were used to study the extraction process of volatile oil;saturated aqueous solution was used, with inclusion rate of volatile oil as index, and orthogonal design was adopted to examine effects of charge ratio of volatile oil and β-CD, inclusion temperature and inclusion time on the inclusion process; X-ray scattering technique, infrared spectroscopy and scanning electron microscopy were used to characterize the inclusion compound. Results The optimum extraction process of volatile oil was soaking fine powder extracted 5 hours with 10 folds the amount of water. The optimum conditions of inclusion process were as follows:mixed ratio of volatile oil (mL) and β-CD (g) was 1:10; inclusion temperature was 50 ℃; the inclusion time was 2 h. X-ray scattering technique, infrared spectroscopy and scanning electron microscopy proved the inclusion compound had been formed. Conclusion Optimum extraction and inclusion processes are stable and feasible, and can provide research foundation for further research and development of preparation.
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Objective To optimize the extraction of volatile oil from Qingjie Granules and process of inclusion compound of beta-cyclodextrin. Methods Water Distillation was used for extraction. Extraction time, grinding degree, and the amount of water were set as inspection factors, and volatile oil volume was set as the evaluation index to inspect extraction process of volatile oil from Qingjie Granules. With inclusion rate as the evaluation index, the single factor test and the Box-Behnken combined with the response surface method were used to choose the optimum inclusion process. Results The optimum extraction process for Schizonepetae Herba, Saposhnikoviae Radix and Forsythiae Fructus coarse powder should be with 10 times amount of water, extracting 3 h. Inclusion method should be saturated water solution method, and the inclusion process of volatile oil as feed and beta-cyclodextrin inclusion ratio was 1:12; the temperature was 40 ℃; inclusion time was 3.5 h. By means of TLC, UV and IR spectra, the formation of the inclusion compound of volatile oil in clear solution particles was preliminarily proved. Conclusion The optimum extraction and inclusion process of volatile oil from Qingjie Granules are stable and feasible, which can be used in industrial production.
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Objective: To optimize the preparation of β-cyclodextrin (β-CD) inclusion compound of forsythia oil and peppermint oil using the colloid mill method. Methods: With recovery ratio and inclusion rate of volatile oil-β-CD as evaluation indexes, the single factor test combining Box-Behnken response surface methodology was used to study the effects of β-CD-pure water ratio, β-CD-volatile oil ratio, and inclusion time on the inclusion process of volatile oil. Using TLC, IR spectrum, and microscopic image, the inclusion complexes were confirmed. Results: The optimum preparation conditions of inclusion compound were as follows: β-CD-pure water ratio was 1:3, mixture of forsythia oil and peppermint oil-β-CD ratio was 1:9, and the inclusion time was 25 min. The formation of inclusion complex was preliminary proved by TLC, IR spectrum, and microscopic image. Conclusion: The method is reasonable and feasible.
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Objective: To optimize the inclusion process of decomposed volatile oil from Atractylodes macrocephala (DVOA) with hydroxypropyl-β-cyclodextrin (HP-β-CD). Methods: The inclusion complex was prepared by the freeze drying method. The preparation process was evaluated using fluorescence spectrophotometry. The inclusion process conditions were screened by the orthogonal test, with the inclusion ratio and oil ratio as indexes, and mass ratio between HP-β-CD and DVOA, inclusion temperature and inclusion time as the impacting factors. The inclusion complex was characterized through ultraviolet-visible spectra (UV-vis), fluorescence spectra (FL) and microscopic imaging, and the stability test was performed. Simultaneously, the chemical composition in DVOA before and after inclusion was analyzed by GC-MS technique. Results: The DVOA and HP-β-CD had formed inclusion complex, the optimal inclusion conditions were as follows: The mass ratio of HP-β-CD to DVOA was 10:1, the inclusion temperature was 30℃, the inclusion time was 2.0 h, and the ratios of average inclusion and oil were 73.32% and 10.43%, respectively. The chemical composition of DVOA was consistent before and after inclusion, the inclusion just had the slight effects on proportion of each component. Conclusion: The preparation process of DVOA/HP-β-CD inclusion complex under the optimal conditions is reasonable, stable, and feasible, and can provide the reliable experimental basis for the anti-tumor new drug research and development of DVOA.
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Objective To optimize the volatile oil extraction and inclusion process of Wenweiyang capsules. Methods An orthogonal test was adopted in this study. The extraction technology was optimized for the yield of volatile oil regarding the amount of water loaded, grain size of medicinal material, and decoction time as factors. The inclusion technology was optimized for the inclusion yield and volatile oil inclusion rate using the ratio ofβ-CD:oil, amount of water and grinding time as factors. Results The optimized extraction parameters were as follows:breaking medicinal material through 10 mesh screen, adding 6 fold volume of water and extracting for 5 h. The optimized inclusion progress was grinding at theβ-CD:oil ratio of 81, loading equivalent amount of water and grinding for 30 minutes. The average yield of volatile oil is 1. 72%, the average inclusion rate is 93. 01% and the average volatile oil inclusion rate is 74. 82%. Conclusion The extraction and inclusion technology is simple, reliable, which can effectively retain the volatile oil and provide evidence for the preparation of Wenweiyang capsules.
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Objective To studyeffect of different processes for preparation ofβ- cyclodextrin inclusion pericarpium citri reticulatae - Radix Aucklandiae essential oil.Methods Extract pericarpium citri reticulatae-radix aucklandiae essential oil with steam distillation method, conductβ- cyclodextrin inclusion of pericarpium citri reticulatae-radix Aucklandiae essential oil with ultrasonic method, grinding method andsaturated aqueous solution method, and detect inclusion effect respectively by polarized light microscopy observation method and TG-DTA analysis method.Results Polarized lightphenomenon disappears under a microscope for the three inclusion preparation products, and TG-DTA curve of ultrasound method is superior to that of saturated aqueous solution method and grinding method.Conclusion Polarized light microscope observation method and TG-DTA method enjoysa good effect in determination of cyclodextrin inclusion, which provides a new method for determination of cyclodextrin inclusion results.
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Objective: To optimize the preparation process of volatile oil prepared from the aerial parts of Houttuynia cordata (Houttuynie Herba, HH)-β-cyclodextrin (β-CD) inclusion complex by central composite design-response surface method. Methods: To prepare the inclusion complex by stiring, with the overall desirability (OD) values of inclusion ratio, yield of the inclusion complex, and methyl-n-nonyl-ketone content as indexes, the influence of inclusion temperature, inclusion time, and ratio of β-CD-HH volatile-oil to inclusion process was investigated by response surface method, the results were fitted by multi-linear equation and second-order polynomial equation, and the optimal inclusion process was predicted according to formulation. The quality of inclusion complex was evaluated by IR and HS-SPME-GC-MS. Results: The optimal inclusion technologies of the HH volatile oil-β-CD inclusion complex were as follows: inclusion time 4.8 h, inclusion temperature 62°C, and ratio of β-CD-HH volatilel oil 7.79:1. Bias of inclusion ratio, yield of the inclusion complex, and methyl-n-nonyl-ketone content between observed and predicted values were 1.70%, 1.49%, and 2.22% respectively. Conclusion: Using the central composite design-response surface method to optimize the preparation of HH volatile oil-β-CD inclusion complex has a good prediction.
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Objective To optimize the extraction and inclusion process of mixed volatile oil of Rhizoma acori graminei, Fructus alpiniae oxyphyllae and Rhizoma chuanxiong in Huangpu Tongqiao Capsules. Methods With steam distillation method, extraction amount as indicator, the orthogonal experiment was used to optimze the extraction process of volatile oil from three factors such as water amount, soak time and extraction time. With saturated aqueous solution method, co-inclusion compound yield and volatile oil rate as indicators, the orthogonal experiment was used to optimize the inclusion process from three factors such as the proportion of volatile oil and β-CD, inclusion time and inclusion temperature. Results The optimum extraction was:adding eight times amount of water and soak for 2 hours to extract 7 hours. The optimum inclusion process was:the proportion of volatile oil andβ-CD was 1∶10, the inclusion time was 3 hours, the inclusion temperature was 40 ℃. Conclusion Optimal extraction process of oil has higher rate, and the volatile oil inclusion rate of inclusion process was also higher, the process is stable.
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Objective To study the stability of ligustilide and the inclusion process in ?-cyclodextrin to avoid its isomerization.Methods The content of ligustilide dropped severely even if it was kept away from layer and air under room temperature.The inclusion process with ?-cyclodextrin was carried out on orthogonal design.The optimum conditions were determined and inclusion complex was made sure by many ways.Results The validated trials by DCS,IR,and GC could exhibit the obvious difference between mixture and inclusion complex which showed the form of a new phase,because of ?-cyclodextrin and drugs in the molecular capsules.Conclusion Inclusion process with ?-cyclodextrin can improve stability of ligustilide that is unstable in normal situation.
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Objective: To study optimum inclusion process conditions for volatile oils from Herba Schizonepetae and Pericarpium Citri Reticulatae Methods : The grinding method was compared with the saturated water solution method by determining the ultilization ratio of volatile oil from both herbs. The optimum preparation conditions were investigated by the orthogonal design. The quality of inclusion compound of volatile oil before and after being included were analyzed by TLC. Results : The optimum preparation conditions for inclusion were established as follow ultilization ?-CD and oil was 8∶ 1, The proportion of water and ?-cyclodextrin was 4∶1 (g:mL), and inclusing time up to three hours, The ultilization ratio of oil was 87.1% . Conclusion : The grinding method is better than the saturated water solution method. The method is applicable.