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Objective To optimize the process of ultrasonic extraction of polysaccharide in Anoectochilus roxburghii and to investigate the method of protein removal. Methods The extraction rate of polysaccharide was used as the detection index. On the basis of single factor investigation, Box-Behnken experimental design and response surface method were used to optimize the three factors of material-liquid ratio, ultrasonic time and ultrasonic extraction temperature. The five deproteinization methods including Sevage reagent method, TCA method, salt method (NaOH-CaCl2 and NaOH-NaCl) and hydrochloric acid method were investigated with the retention rate of polysaccharide and protein removal rate. Results The optimal extraction conditions of polysaccharide from Anoectochilus roxburghii were as follows: liquid-to-solid ratio was 10∶1, extraction temperature was 48 ℃ and extraction time was 36 min with extraction 2 times, ultrasonic power was 300 W, the extraction rate was 13.13%. NaOH-CaCl2 deproteinized methods∶ the loss rate of polysaccharide was 18.74%, and the removal rate of protein was 95.62%. Conclusion Ultrasonic extraction is easy to operate, and the optimized extraction method can achieve a high extraction rate. NaOH-CaCl2 deproteinization methods can get high protein removal rate and polysaccharide retention rate. This method is suitable for the research and development of the active components of the polysaccharides from Anoectochilus roxburghii.
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OBJECTIVE：To optimize ultrasonic-assisted ethanol-（NH4）2SO4 aqueous two-phase extraction technology of citru- sinol from Desmodium caudatum . METHODS ：Using the content of citrusinol as indexes ，with ethanol volume fraction ， solid-liquid ratio ，（NH4）2SO4 addition amount ，ultrasonic time and ultrasonic temperature as factors ，based on the single factor tests，Box-Behnken design-response surface methodology was used to optimize the extraction technology of citrusinol. RESULTS ： The optimized extraction technology of citrusinol included that ethanol volume fraction was 95.35％，the solid-liquid ratio was 1∶50.35 （g/mL），（NH4）2SO4 addition amount was 4.49 g，ultrasonic time was 48.7 min，ultrasonic temperature was 57.6 ℃. In 3 times of validation tests ，the extraction rates of citrusinol were 0.637 8，0.638 4，0.625 4 mg/g，respectively，which was close to predicted value（0.630 5 mg/g）. CONCLUSIONS ：The optimized ultrasonic-assisted ethanol- （NH4）2SO4 aqueous two-phase extraction technology is stable and feasible ，and can be used for the extraction of citrusinol from D. caudatum .
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Objective: To explore the high-efficiency green environmental extraction method of total flavones from Microcos paniculata (MPTF), and investigate its lipid-lowering activity. Methods: The ionic liquid was used to assist the ultrasonic extraction of MPTF, and the extraction process was investigated by single factor experiment and orthogonal test. Wistar rats were randomly divided into normal control group and positive control group (Resuvastatin Calcium Tablets 5.2 mg/kg) by high fat diet, high-fat model group and MPTF low, medium and high dose groups (ig dose MPTF 300, 600, 900 mg/kg), with 10 rats in each group. The total cholesterol (TC), glycerol lipid (TG), high density lipoprotein (HDL-C), low density lipoprotein (LDL-C) levels were determinated. Results: The optimum process conditions for ultrasonic-assisted extraction of MPTF by ionic liquid were as follow: ionic liquid was [BMIM]Cl at concentration of 0.30 mol/L; ratio of material to liquid was 1:40, extraction solvent was 60% ethanol aqueous solution with extraction time of 30 min at 50 ℃. The verification test results showed that the extraction rate of total flavonoids obtained from the extraction process was high and the process was stable. The results of lipid-lowering test showed that the levels of TC, TG and LDL-C were decreased in all doses of MPTF groups, and the level of HDL-C was increased (P < 0.05). With the increase of MPTF dose, the indicators showed obvious trends in a dese-dependent manner. Conclusion: The ionic liquid combined with ultrasonic- assisted extraction of MPTF is stable and feasible, which provides reference for ionic liquid synergistic ultrasound-assisted extraction of poorly soluble active ingredients in Chinese materia medica. MPTF extract has better lipid-lowering effect.
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OBJECTIVE： To establish a determination method for content of polysaccharide in Acanthopanax senticosus， and to conduct cluster analysis and ultrasonic extraction technology optimization. METHODS： The content of polysaccharide in A. senticosus was determined by phenol-sulfuric acid method. Cluster analysis was conducted by using SPSS 23.0 software of the polysaccharide in A. senticosus from 17 habitats. The ultrasonic extraction technology was optimized with L9（34）orthogonal test using extraction temperature， the ratio of material to liquid， extraction time as factors， the content of polysaccharides as index， and then validated. RESULTS： The linear range of glucose ranged from 0.007 75 to 0.151 mg/mL （r＝0.999 1）； the limits of quantification and detection were 2.854， 0.856 μg/mL； RSDs of precision， stability， and repeatability tests were less than 2％； recovery rates of the sample were 98.41％-101.58％（RSD＝1.23％，n＝6）. Cluster analysis results showed that 17 batches of samples could be clustered into three classes； S1， S6， S10， S12 and S13 were clustered into one class； S3-S5 and S7 were clustered into one class； and the rest samples were clustered into one class. The optimal ultrasonic extraction technology was extraction temperature 55 ℃， ratio of material to liquid 1 ∶ 10 （g/mL）， extraction time 35 min. Results of validation tests showed the content of the polysaccharide under the best process condition was 4.36％（RSD＝0.920％，n＝3）. CONCLUSIONS： Established method is simple，reproducible and suitable for determination of polysaccharide in A. senticosus； the optimized ultrasonic extraction technology is stable and feasible.
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OBJECTIVE： To optimize the ultrasonic extraction technology for Jinjuan shengban capsules. METHODS： Using comprehensive score of indexes as transfer rate of gallic acid， chlorogenic acid， baicalin， aloe emodin and emodin methyl ether， with ethanol volume fraction， ultrasonic power， ultrasonic extraction time and liquid-material ratio as factors， the ultrasound extraction technology of Jinjuan shengban capsules was optimized by Box-Behnken response surface methodology based on single factor test. The validation test was conducted. RESULTS： The best extraction technology was 50-fold 70％ ethanol， extracting 40 min under 300 W. In validation test， average transfer rates of gallic acid， chlorogenic acid， baicalin， aloe emodin and emodin methyl ether were 85.92％， 86.37％， 92.76％， 90.84％ and 87.26％ （RSD＜3.57％，n＝3） in 3 batches of samples； comprehensive score was 88.95％， relative error of which to predicted value of 88.27％ was 1.10％. CONCLUSIONS： The response surface method combined with multi-index comprehensive scoring can be used to optimize the extraction technology of Jinjuan shengban capsules which is simple and stable.
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OBJECTIVE:To optimize ultrasonic extraction technology for polysaccharide from Aconiti lateralis radix praepara-ta(ALRP). METHODS:Uniform design method was applied to investigate the effects of liquid material ratio,ultrasonic time and ultrasonic temperature on extraction rate of polysaccharide from ALRP. Verification test was conducted and compared with the re-sults of conventional decoction and boiling method. RESULTS:Optimized ultrasonic extraction technology was as follow as liquid material ratio of 10 mL/g,ultrasonic time of 34 min and ultrasonic temperature of 73 ℃. The polysaccharide extraction rate in veri-fication test was 19.05%(RSD=0.60%,n=3),relative error of the predicted value (19.44%) was 2.0%,while the extraction rate was higher than decoction and boiling method(16.42%). CONCLUSIONS:Optimized ultrasonic extraction technology is sim-ple,rapid and stable with high extraction rate,which is suitable for extracting polysaccharide from ALRP.
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OBJECTIVE:To optimize the ultrasonic extraction technology for Tianshu capsules. METHODS:Using the transfer rate of active ingredient ferulic acid in Ligusticum chuanxiong and gastrodin in Gastrodia elata of Tianshu capsules as investigation indexes,L9(34)orthogonal design test was adopted to investigate the effects of ethanol volume fraction,ethanol amount,extraction time and ultrasonic power on the extraction rate. Ultrasonic extraction technology for Tianshu capsules was optimized,and verifica-tion test was carried out. RESULTS:The optimized extraction technology for Tianshu capsules was as follow as 8-fold 70% etha-nol,extracting twice under 350 W,extracting 1.5 h every time. Results of verification test showed the average transfer rate was 94.06% for ferulic acid(RSD=0.18%,n=3)and 95.02% for gastrodin(0.47%,n=3). CONCLUSIONS:The optimized tech-nology is rapid,simple,stable and feasible,and can be used for extracting the active ingredients in Tianshu capsules.
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This study aimed to optimize the ultrasonic extraction of gardenia oils from Gardenia jasminoides Ellis.by response surface analysis methodology (RSM).The duration of extraction,ratio of liquid to materials and extracting times were selected as impact factors based on single-factor experiment.RSM was adopted to learn the effects of the three factors on the extraction rate of Gardenia oil from Gardeniajasminoides Ellis.As a result,it was found that the duration of extraction was 28.7 min,while the ratio of liquid to materials was 11.62:1,and the number of extracting times were 3.36.Under this extracting condition,the average extraction rate of the oil was 13.5％ according to three validation experiments,fitting the predicted value well.In conclusion,it was demonstrated that the ultrasonic extraction method effectively improved the extraction rate of gardenia oil,providing a certain basis for the development and utilization of gardenia oil.
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OBJECTIVE:To optimize the extraction technology of nucleoside from Codonopsis pilosula. METHODS:The ultra-sonic extraction was used to extract nucleoside from C. pilosula. The extraction technology was screened and optimized by single factor and orthogonal test with ethanol concentration (including water),extraction time,solid-liquid ratio and extraction times as factors using the total contents of cytidine,uridine,guanosine and adenosine as index. Validation test was conducted. RESULTS:The optimal extraction technology was that pure water was extraction solvent,extracting for 45 min,with material-liquid ratio of 1∶20 (g/ml),extracting for 2 times. Total amount of 4 kinds of nucleosides from in 100 g C. pilosula was (17.01 ± 0.005) mg (RSD=0.68%,n=3). CONCLUSIONS:Optimized extraction technology of nucleoside from C. pilosula is stable,feasible,rapid in operation and cost-saving.
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OBJECTIVE:To optimize ultrasonic extraction and purification technology of solanesol from tobacco leaf. METH-ODS:Using extraction rate and transport rate of solanesol as indexes,single factor test was used to investigate liquid-solid ratio, ultrasonic extraction temperature and time,ultrasonic power and extraction times,and the amount of soap alkali lye(volume ratio of soap alkali lye to extraction liquid),acidizing fluids (volume ratio of acidizing fluids to soap alkali lye extract),extraction times of purification technology. Optimized technology was validated,and the purity of solanesol was calculated;the amount of ex-tracted solanesol was compared between this method and traditional extraction method (spending 30 h),solvent continuous cyclic extraction (spending 5-6 h). RESULTS:Optimized extraction technology was as follows as volume ratio of soap alkali lye to ex-traction liquid 1∶14,ultrasonic extraction temperature 70 ℃,ultrasonic extraction time 60 min,ultrasonic power 120 W,extract-ing for 3 times;optimized purification technology was as follows as volume ratio of soap alkali lye to extraction liquid 2∶35,vol-ume ratio of acidizing fluids to soap alkali lye extract 2∶14,extracting for 4 times. In validation test,extraction rate,transport rate and purity were 92.45%(RSD=0.46%,n=3),79.88%(RSD=0.30%,n=3)and 55.86%(RSD=0.40%,n=3). The amount of solanesol extracted with 3 methods were 52.22,45.22 and 26.10 mg/g. CONCLUSIONS:The optimized technology is simple and stable,costs less time and saves source with high extraction amount and purity,which is suitable for production,extraction and purification of solanesol from tobacco leaf.
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This paper is to investigate the optimization conditions of ultrasonic technique for extraction process of Xiaoqinglong granules in medium scale. First of all, single factor experiment was used to determine the overall impact tendency and range of each factor； secondly, Box-Behnken method was used for optimization and detecting the content of paeoniflorin, ephedrine hydrochloride, glycyrrhizic acid of the liquid medicine. Their respective extraction rate was calculated and the comprehensive evaluation was carried out. The results were used as the evaluation basis for the efficacy of Xiaoqinglong granules ultrasonic extraction. The test results showed that the optimum extraction process of Xiaoqinglong granules by ultrasonic extraction was under the following conditions: ultrasonic power 600 W, liquid-solid ratio 10∶1, extraction for 31 min. Under this condition, the predicted value of extraction rate for Xiaoqinglong granules was 85.90%, and the test value was 85.87%. The mathematical model(P<0.01) established in this paper was significant, and can be used for the analysis and prediction of the ultrasonic extraction process of Xiaoqinglong granules.
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Objective To study the ultrasonic extraction technology of tyrosol in Rhodiolae Crenulatae Radix et Rhizoma;To mathematically simulate the extraction process.Methods The content of tyrosol was set as index;HPLC was used;the ultrasonic extraction process of tyrosol in Rhodiolae Crenulatae Radix et Rhizoma was optimized by an orhogonal experiment and mathematic simulation.Results The optimum ultrasonic extraction conditions were as follows:80%ethanol was used as extraction solvent, the ratio of material to liquid was 1:35 (g:mL), with the extraction time of 30 min and ultrasonic power of 240 W. In these conditions, the extracting rate of tyrosol was 0.150 1%. Compared with the heating reflux method, the extraction time should be shortened by 66.7% and the extracting rate should be increased by 12%.Conclusion The extraction method is simple and the extraction rate of effective components is high. Mathematical simulation values based on ultrasonic extraction are consistent with experiment values.
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A high performance liquid chromatography-inductively coupled plasma mass spectrometric ( HPLC-ICP-MS) method for analysis of selenocystine (SeCys2), selenite (SeⅣ), selenomethionine (SeMet) and selenate ( SeⅥ) was described. Chromatographic separation was performed using 8 mmol/L citric acid solution (pH 5). The potentially interfering 40Ar40Ar+ at selenium masses of m/z 80 was reduced using CH4 as a reactive cell gas in the dynamic reaction cell. The selenium species was extracted using ultrasonic extraction system with a mixture of protease K and lipase. The limits of detection for SeCys2 , SeⅣ, SeMet, and SeⅥwere observed as 0. 088, 0. 033, 0. 30, and 0. 17 ng/mL, respectively. The correlation coefficients were greater than 0 . 9995 . The recoveries were observed in the range of 95 . 1%-114 . 6%. The developed method was successfully applied for the determination of selenium species in Burdock and Panax notoginseng.
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OBJECTIVE:To optimize the ultrasonic extraction process of total alkaloids from mulberry leaves. METHODS:Based on the single factor experiment,response surface method was adopted to investigate the effects of ultrasonic extraction time, ultrasonic power,ethanol volume fraction,solid-liquid ratio and pH of solvent on the extraction rate of total alkaloids from mulber-ry leaves,then test data were analyzed by Design Expert 8.0.5 software,and the optimized process was confirmed and verified. RE-SULTS:The multiple correlation coefficient of established binomial equation fitting model was 0.969 9;the optimized condition for extracting alkaloid from mulberry leaf was ultrasonic extraction time of 48 min,ultrasonic extraction power of 800 W,ethanol vol-ume fraction of 70%,material-liquid ratio of 1∶25,pH 5. Under these conditions,the extraction rate of total alkaloids was 0.422%, with the bias ratio was less than 2% compared with the model predictions. CONCLUSIONS:The established model has good fit-ting performance,the extraction process is stable and reliable,and can be used for the extraction of alkaloids from mulberry leaves.
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OBJECTIVE:To optimize the ultrasonic extraction technology of salidroside in Rhodiola rosea. METHODS:With the content of salidroside as the index,L16(45)orthogonal test was designed to observe the effects of 4 factors including the mass fraction of ethanol,solid-liquid ratio,extraction time and ultrasonic power on the content of salidroside in R. rosea extraction solu-tion. By using Matlab 6.5 software,mathematical simulation of ultrasonic extraction process of salidroside was made with the data of orthogonal test. Multiple regression analysis method was adopted to optimize the ultrasonic extraction technology of salidroside, and then the extraction result of optimal technology and that of traditional heating reflux technology were compared. RESULTS:The optimal extraction technology of salidroside was as follows as ethanol mass fraction of 77%,solid-liquid ratio of 1∶34 (g∶ml),extraction time of 34 min,ultrasonic power of 237 W(ultrasonic frequency of 40 kHz). Under the above-mentioned condi-tions,the content of salidroside was up to 0.982 4%,close to the predicted value of 0.989 4%. Compared to heating reflux meth-od,the ultrasonic method has similar content of salidroside but extraction time was shortened by 62.2%. CONCLUSIONS:The ul-trasonic extraction method for extracting the salidroside in R. rosea is simple,requires shorter time,and giving rise to higher extrac-tion rate.
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Objective To select the optimum ultrasonic extracting method of polysaccharides from Rosa Laevigatae Michx in Guizhou. Methods Independent variables were solid-liquid ratio, extraction time and extraction temperature, dependent variable was extraction rate ratio of polysaccharides from Rosa Laevigatae Michx.Linear or nonlinear mathematic models were used to estimate the relationship between independent and dependent variables. Response surface methodology was used to optimize the process of extraction.Prediction was carried out through comparing the observed and predicted value. Results The optimum extraction condition for the polysaccharides was as follows: extracting at 75 ℃ for 60 min and ratio of liquid to solid 30??1 ( mL??g ) . The average extraction yield of polysaccharides was 37. 54% under the optimum extraction condition. Conclusion This optimized extraction process is simple and reliable for the extraction of polysaccharides from Rosa Laevigatae Michx in Guizhou.
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INTRODUCCIÓN: la especie Moringa oleifera Lam. conocida como Moringa, se ha introducido en Cuba principalmente con propósitos alimenticios. Sin embargo, no se han informado estudios de la composición de ácidos grasos del aceite obtenido de las semillas de esta especie en la región habanera. OBJETIVO: determinar la composición de ácidos grasos en el aceite de las semillas de las plantas de M. oleifera que crecen en La Habana, Cuba. MÉTODOS: las semillas se recolectaron, molieron y se extrajeron con hexano en un baño ultrasónico. Los extractos fueron filtrados y el disolvente fue evaporado. Los ácidos grasos obtenidos de los aceites fueron determinados como ésteres metílicos por cromatografía de gases con una columna capilar BPX-70. RESULTADOS: los principales ácidos grasos encontrados fueron el oleico (C18:1; 73,1 %), palmítico (C16:0; 7,4 %) y docosanoico (C22:0; 5,8 %), mientras que otros 19 ácidos grasos, entre estos los ácidos C12:0, C14:0, C15:0, C17:0,C18:1 (n-10), C18:2, C18:3, C20:0, C20:1, C21:0, C22:1, C23:0, C24:0, C25:0, C26:0 C27:0 y C28:0, se encontraron en menores proporciones. Este es el primer reporte de la presencia de los ácidos C15:0, C27:0 y C28:0 en esta especie, y el primero que identifica los ácidos C12:0, C14:0, C17:0, C18:3, C20:0, C23:0, C25:0 y C26:0 en la especie M. oleífera que crece en Cuba. CONCLUSIONES: la composición de ácidos grasos del aceite presente en las semillas de la especie M. oleífera que crece en La Habana muestra al ácido oleico como componente mayoritario. Se informa por primera vez la presencia de los ácidos C15:0, C27:0 y C28:0 en las semillas de esta especie, y de los ácidos C12:0, C14:0, C17:0, C18:3, C20:0, C23:0, C25:0 y C26:0 en la especie en Cuba. Estos resultados sobre la composición química del aceite de las semillas de la especie M. oleífera, pudieran contribuir a establecer su posible utilidad nutricional.
INTRODUCTION: the species Moringa oleifera Lam., known as Moringa, has been introduced in Cuba mainly for nutritional purposes. However, no study has been reported about the fatty acid composition of the seed oil obtained from this species in Havana. OBJECTIVE: determine the fatty acid composition of seed oil from M. oleifera plants growing in Havana, Cuba. METHODS: the seeds were collected, milled and extracted with hexane in an ultrasonic bath. Extracts were filtered and the solvent evaporated. Fatty acids obtained from the oils were determined as methyl esters by gas chromatography with a BPX-70 capillary column. RESULTS: the main fatty acids found were oleic (C18:1; 73.1%), palmitic (C16:0; 7.4%) and docosanoic (C22:0; 5.8%). Another 19 fatty acids, among them C12:0, C14:0, C15:0, C17:0, C18:1 (n-10), C18:2, C18:3, C20:0, C20:1, C21:0, C22:1, C23:0, C24:0, C25:0, C26:0 C27:0 and C28:0 were found in smaller proportions. This is the first report of the presence of acids C15:0, C27:0 and C28:0 in this species, and the first one to identify C12:0, C14:0, C17:0, C18:3, C20:0, C23:0, C25:0 and C26:0 acids in the species M. Oleifera growing in Cuba. CONCLUSIONS: oleic acid is the most abundant fatty acid component in seed oil from M. oleifera growing in Havana. This is the first report of the presence of acids C15:0, C27:0 and C28:0 in the seeds of this species, and of acids C12:0, C14:0, C17:0, C18:3, C20:0, C23:0, C25:0 and C26:0 in the species in Cuba. These results about the chemical composition of seed oil from the species M. oleifera could contribute to elucidate its potential nutritional usefulness.
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Chromatography, Gas/methods , Moringa oleifera , Plant Preparations/therapeutic use , CubaABSTRACT
Extraction process plays an important role in Chinese herbal medicine applications. Traditional extraction method has some disadvantages, such as long processing time, high solvent consumption and low efficiency. Thus, some new technologies and methods have been introduced in this paper, including ultrasonic extraction, microwave extraction, supercritical fluid extraction. On the basis of advantages and disadvantages of traditional Soxhlet extrac-tion, this paper mainly described the principles, characteristics, influencing parameters and applications.
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Objective To compare the effects of accelerated solvent extraction (ASE), ultrasonic extraction (USE) and soxhlet extraction (SE), by extraction and determination of pesticide residues in Chinese herbal medicines. Methods Pesticide residues of Chinese herbal medicines were extracted by accelerated solvent extraction, ultrasonic extraction and soxhlet extraction, then the extract were cleaned up by sulfonation treatment, alumina neutral-florisil column and gel permeation chromatography (GPC). The extract was separated by HP-5 capillary column and detected by electron-capture detector. Results Extraction efficiency of USE was significantly lower than that of ASE and SE, there was no significant difference between ASE and SE. Pairwise comparison of the recoveries of three purification methods showed no significant difference. Conclusion The extraction efficiency of three methods was ASE>SE>USE. The extraction method should be selected according to the requirement.
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Objective To optimize the extraction process of Euphorbia hirta L.by Central composite design/response surface methodology with ethanol by the ultrasonic extraction technology.Methods Based on the single factor experiment and central composite design-response surface methodology,the content of quercitroside was regarded as evaluation index,select ethanol concentration,extraction time,and solid-liquid ratio as three evaluation factors to achieve the purpose. Results The results indicated that the optimal extraction process was obtained as follows:10 times the amount of 60% ethanol under ultrasound for 2 times,50 min each;the average content of the quercitroside was 2.39 mg/g.Conclusion The method to optimize the extraction process is simple and reasonable.