There is a constant search for biomaterials from natural products like plants for food and industrial applications.The work embodied in this report aimed at investigating the effects of microwave-assisted and soxhlet ...There is a constant search for biomaterials from natural products like plants for food and industrial applications.The work embodied in this report aimed at investigating the effects of microwave-assisted and soxhlet extraction(MAE and SE) techniques on the functional physicochemical quality characteristics of Moringa oleifera seed oil and proteins extracts. M. oleifera seeds were ground to fine powders and oil was extracted by microwave-assisted and soxhlet extraction techniques using petroleum ether. Quality attributes including yield percent, moisture content,iodine, saponification, specific gravity, viscosity, p H, thiobarbituric acid, acid and peroxide values were measured. Mineral and vitamin contents, chemical/functional groups, fatty acid(FA) composition, and reducing power of the oil were evaluated. Metabolomics of protein extracted from the defatted powders were analyzed by nuclear magnetic resonance(NMR). M. oleifera oil from MAE and SE methods had good yield(34.25 ± 0.0%,28.75 ± 0.0%), low moisture content(0.008 ± 0.0%, 0.011 ± 0.0%), non-drying and unsaturated, moderately saponified, less dense(0.91 ± 0.01, 0.92 ± 0.02 g m L^(-1)), had Newtonian flow, were weakly acidic, showed good content of FAs, recorded strong potential for long shelf-life, showed stability against oxidative rancidity and enzymatic hydrolysis, had very rich deposits of micro-and macro-nutrients as well as water-soluble and lipidsoluble vitamins, and functional groups in the oil were reflective of its content of long-and medium-chain triglycerides(LCT and MCT). Monounsaturated and saturated fatty acids(MUFA and SFA) were detected and the oil has excellent ferric ion reducing power. NMR metabolomic assay revealed the presence of nine essential amino acids(EAAs) in the protein extract. MAE technique is a feasible and acceptable alternative for high throughput extraction of M. oleifera oil with high yield and excellent quality attributes. The study revealed that MAE did not impart any remarkable advantage(s) on the physicochemical properties of M. oleifera seed oil and protein compared to SE technique.展开更多
[Objective] This study was aimed to determine the optimal parameters for the extraction of perilla seed oil to obtain high-quality perilla seed oil and analyze its compositions. [Method] In this study, perilla seed oi...[Objective] This study was aimed to determine the optimal parameters for the extraction of perilla seed oil to obtain high-quality perilla seed oil and analyze its compositions. [Method] In this study, perilla seed oil was extracted using supercritical CO2 (SC-CO2). The effects of extraction time, temperature and pressure were investigated by single-factor experiments and orthogonal array testing (ORT). The chemical compositions of extracted perilla seed oil were investigated by GC-MS. [Result] The optimal conditions for the extraction of perilla seed oil using SC-CO2 were extraction time of 4 h, extraction temperature at 40 ℃, and extraction pressure at 23 MPa. Under these conditions, the extraction yield of perilla seed oil was maximized to 12.43%. GC-MS analysis revealed that perilla seed oil was a complex mixture containing 76.183% α-linolenic acid. [Conclusion] Supercritical CO2 extraction was proven to be an effective technology to extract oil from perilla seed, and GCMS was also a satisfactory method for analyzing the compositions of perilla seed oil.展开更多
The physical properties and chemical components of three oil samples extracted from Illicium verum Hook. f. by steam distillation (SD), solvent extraction (SE) and supercritical fluid extraction (SFE) were compa...The physical properties and chemical components of three oil samples extracted from Illicium verum Hook. f. by steam distillation (SD), solvent extraction (SE) and supercritical fluid extraction (SFE) were compared with one another and analyzed by Gas Chromatography-Mass Spectrometry (GC-MS). The quality parameters of star anise essential oil from SFE were close to that of those came from SD and SE. Although the extraction yield of star anise by SFE (9.2 %) was close to the value from SE (9.3%), it was yet higher than that came from SD (8.2%). For sensory evaluation, however, three oils were significantly different. The odor and taste of the products from SFE and SE were generally more natural and vivid than that came from distilled oil. The volatile compound revealed that significant differences of the composition existed in the distilled oil and the oleoresins prepared by SFE and SE.展开更多
The total volatile components were extracted from safflower by ultrasonic-assisted solvent extraction (USE) and their chemical constituents were analyzed by gas chromatographymass spectrometry (GC-MS) to provide s...The total volatile components were extracted from safflower by ultrasonic-assisted solvent extraction (USE) and their chemical constituents were analyzed by gas chromatographymass spectrometry (GC-MS) to provide scientific basis for the quality control of safflower. Five different solvents (diethyl ether, ethanol, ethyl acetate, dichloromethane and acetone) were used and compared in terms of number of volatile components extracted and the peak areas of these components in TIC. The results showed that USE could be used as an efficient and rapid method for extracting the volatile components from safflower. It also could be found that the number of components in the TIC of ethyl acetate extract was more than that in the TIC of other solvent ones. Meanwhile, the volatile components of safflower from Xinjiang Autonomous Region and Henan Province of China were different in chemical components and relative contents. It could be concluded that both the extraction solvents and geographical origin of safflower are responsible for these differences. The experimental results also indicated that USE/GC-MS is a simple, rapid and effective method to analyze the volatile oil components of safflower.展开更多
As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more effici...As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more efficient technologies. Taking economic and environmental concerns into account, subcritical fluid extraction as a faster and more efficient method has stood out as a sample pre-treatment technology. This new extraction technology can overcome the shortcomings of supercritical fluid and achieve higher extraction efficiency at relatively low pressures and temperatures. In this experiment, a simple, sensitive and efficient method has been developed for the determination of diethylstilbestrol(DES) in fish tissue using subcritical 1,1,1,2-tetrafluoroethane(R134a) extraction in combination with gas chromatography-mass spectrometry(GC-MS). After extraction, freezing-lipid filtration was utilized to remove fatty co-extract. Further purification steps were performed with C_(18) and NH_2 solid phase extraction(SPE). Finally, the analyte was derived by heptafluorobutyric anhydride(HFBA), followed by GC-MS analysis. Response surface methodology(RSM) was employed to optimizing the extraction condition, and the optimized was as follows: extraction pressure, 4.3 MPa; extraction temperature, 26℃; amount of co-solvent volume, 4.7 m L. Under this condition, at a spiked level of 1, 5, 10 μg kg^(-1), the mean recovery of DES was more than 90% with relative standard deviations(RSDs) less than 10%. Finally, the developed method has been successfully used to analyzing the real samples.展开更多
Soxhlet extraction is a common method of sample preparation. However, there has been no discussion about the efficiency of Soxhlet extraction from different batches and the factors that cause content fluctuation. In t...Soxhlet extraction is a common method of sample preparation. However, there has been no discussion about the efficiency of Soxhlet extraction from different batches and the factors that cause content fluctuation. In this study, Panax ginseng was selected as a model sample. Soxhlet extraction by means of a water bath, which has always been neglected, was identified as a novel key factor in the poor repeat- ability in different batches of Soxhlet extraction, as it can affect the siphon times and reflux time, which have been positively correlated with the ginsenoside contents. By substituting round bottom flasks in the same column, the relative standard deviation of the most fluctuated compound, ginsenoside Rbl, was decreased from 24.6% to 5.02%. Scanning electron microscopy analysis confirmed that the breakdown of the surface of the ginseng powder in the Soxhlet extraction led to a better dissolution of ginsenosides, indicating that chloroform may promote the extraction of ginsenosides by disrupting the cell structure. Moreover, 70% methanol was regarded as the better solvent for extracting the ginsenosides. Overall, this work offers a practical and effective protocol for improving the accuracy and repeatability of Soxhlet extraction methodology for ginsenosides and other analytes.展开更多
The application of soxhlet, ultrasonic and accelerated solvent extractiontechniques to the analysis of six organochlorine pesticides (α-HCH, β-HCH, γ-HCH, o, p'-DDT,p,p'-DDT and p,p'-DDE) in Taihu Lake ...The application of soxhlet, ultrasonic and accelerated solvent extractiontechniques to the analysis of six organochlorine pesticides (α-HCH, β-HCH, γ-HCH, o, p'-DDT,p,p'-DDT and p,p'-DDE) in Taihu Lake sediment samples is described. It was found that the limits ofquantification ranged from 0.002 μg g^(-1) to 0.004 μg g^(-1), and the recoveries oforganochlorine pesticides with the three extraction techniques were acceptable ( 】80.7%). With amass selective detector, better results were obtained by accelerated solvent extraction usinghexane-acetone (1:1) as compared with soxhlet and ultrasonic extraction. It was shown that theaccelerated solvent extraction was the optimum technique for the analysis of organochlorinepesticides in sediments. The general features of the three extraction techniques are also presented.展开更多
Extraction of castor oil from castor seeds was investigated using different green solvents which include d-limonene, p-cymene, α-pinene, ethanol, and furfural at the temperature range of (323 - 413) K. The Soxhlet ex...Extraction of castor oil from castor seeds was investigated using different green solvents which include d-limonene, p-cymene, α-pinene, ethanol, and furfural at the temperature range of (323 - 413) K. The Soxhlet extraction method was employed to investigate the effect of temperature at atmospheric pressure. The focus of the study was to investigate a potential green solvent that can produce the high yields compared to the traditional solvent (hexane). The results show that at the average time of 3 hours and 30 minutes, the castor oil yield for green solvents were ranked as furfural (47.13%) > ethanol (45.37%) > p-cymene (39.15%) > d-limonene (39.13%) > α-pinene (38.11%). These castor oil yields were obtained at optimum temperatures for each green solvent. The castor oil yields were compared to the yield of hexane (31.36%) at same average time. The green solvents were recovered by using simple distillation, except furfural which was difficult to be recovered.展开更多
In this study,a GC-MS/SIM method was used to analyze 16 PAHs in soil by ASE on-line clean-up.The average recoveries were ranged from 67% to 129%.The relative standard deviations were between 2.7% and 21.1%.The calcula...In this study,a GC-MS/SIM method was used to analyze 16 PAHs in soil by ASE on-line clean-up.The average recoveries were ranged from 67% to 129%.The relative standard deviations were between 2.7% and 21.1%.The calculated limits of detection were no more than 0.95 ng/g.This method was fast,simple,and cost-saving,and can be used in the large quantities of samples analysis.展开更多
In this paper,the Illilium verum Hook.f.grow at mountain of Dayao of Jinxiu in Guangxi,Volatile oil was extracted by soxhet method and steam distillation.All the volatile oil was analyzed by GC-MS,the result show the ...In this paper,the Illilium verum Hook.f.grow at mountain of Dayao of Jinxiu in Guangxi,Volatile oil was extracted by soxhet method and steam distillation.All the volatile oil was analyzed by GC-MS,the result show the ingredients and rate of product were change greatly,The major chemical constituents were trans-anethole,estragole and anisaldehyde etc.展开更多
A method was established for determination of the reducing substances released from plastic blood bags to anticoagulant.The samples were extracted with a solid-phase extraction procedure using dichloromethane as extra...A method was established for determination of the reducing substances released from plastic blood bags to anticoagulant.The samples were extracted with a solid-phase extraction procedure using dichloromethane as extract solvents.The extracts were measured with GC-MS.Several reducing substances,such as 1,2-benzenedicarboxylic acid,alkane and bis(2-ethylhexyl) phthalate,etc were found in anticoagulant.The method was simple and can be used for the quality control of plastic blood bags.展开更多
[Objective] The aim of this study was to find a better method to exactly quantify the residual polycyclic aromatic hydrocarbons(PAHs)in the long-term contaminated soil in the field so as to provide basis for the rem...[Objective] The aim of this study was to find a better method to exactly quantify the residual polycyclic aromatic hydrocarbons(PAHs)in the long-term contaminated soil in the field so as to provide basis for the remediation for PAHs contaminated soil.[Method]The comparisons of soxhlet extraction,ultrasonic extraction and shaking extraction were studied in the agricultural soil irrigated with oil sewage over a long period of time.[Result]The total PAHs extracted by soxhlet extraction were the highest(6 873.7 μg/kg),followed by shaking extraction(6 698.8 μg/kg)and ultrasonic extraction(5 737.6 μg/kg).Among these methods,the highest extracted 4 and 6 rings PAHs were in the soxhlet extraction,the highest extracted 2 and 5 rings PAHs were in the shaking extraction,and the highest extracted 3 rings PAHs were in the ultrasonic extraction.[Conclusion]This study had provided basis for the selection of the assessment method of residual PAHs in the field soil.展开更多
基金funded by International Foundation for Science(IFS)and Organisation for the Prohibition of Chemical Weapons(OPCW)research grant awarded to Dr.Chukwuebuka Emmanuel Umeyor in 2019(Grant number:I-2-F-6448-1).
文摘There is a constant search for biomaterials from natural products like plants for food and industrial applications.The work embodied in this report aimed at investigating the effects of microwave-assisted and soxhlet extraction(MAE and SE) techniques on the functional physicochemical quality characteristics of Moringa oleifera seed oil and proteins extracts. M. oleifera seeds were ground to fine powders and oil was extracted by microwave-assisted and soxhlet extraction techniques using petroleum ether. Quality attributes including yield percent, moisture content,iodine, saponification, specific gravity, viscosity, p H, thiobarbituric acid, acid and peroxide values were measured. Mineral and vitamin contents, chemical/functional groups, fatty acid(FA) composition, and reducing power of the oil were evaluated. Metabolomics of protein extracted from the defatted powders were analyzed by nuclear magnetic resonance(NMR). M. oleifera oil from MAE and SE methods had good yield(34.25 ± 0.0%,28.75 ± 0.0%), low moisture content(0.008 ± 0.0%, 0.011 ± 0.0%), non-drying and unsaturated, moderately saponified, less dense(0.91 ± 0.01, 0.92 ± 0.02 g m L^(-1)), had Newtonian flow, were weakly acidic, showed good content of FAs, recorded strong potential for long shelf-life, showed stability against oxidative rancidity and enzymatic hydrolysis, had very rich deposits of micro-and macro-nutrients as well as water-soluble and lipidsoluble vitamins, and functional groups in the oil were reflective of its content of long-and medium-chain triglycerides(LCT and MCT). Monounsaturated and saturated fatty acids(MUFA and SFA) were detected and the oil has excellent ferric ion reducing power. NMR metabolomic assay revealed the presence of nine essential amino acids(EAAs) in the protein extract. MAE technique is a feasible and acceptable alternative for high throughput extraction of M. oleifera oil with high yield and excellent quality attributes. The study revealed that MAE did not impart any remarkable advantage(s) on the physicochemical properties of M. oleifera seed oil and protein compared to SE technique.
基金Supported by Undergraduate Innovation Training Program of Jiangsu Province(201610327010Z)~~
文摘[Objective] This study was aimed to determine the optimal parameters for the extraction of perilla seed oil to obtain high-quality perilla seed oil and analyze its compositions. [Method] In this study, perilla seed oil was extracted using supercritical CO2 (SC-CO2). The effects of extraction time, temperature and pressure were investigated by single-factor experiments and orthogonal array testing (ORT). The chemical compositions of extracted perilla seed oil were investigated by GC-MS. [Result] The optimal conditions for the extraction of perilla seed oil using SC-CO2 were extraction time of 4 h, extraction temperature at 40 ℃, and extraction pressure at 23 MPa. Under these conditions, the extraction yield of perilla seed oil was maximized to 12.43%. GC-MS analysis revealed that perilla seed oil was a complex mixture containing 76.183% α-linolenic acid. [Conclusion] Supercritical CO2 extraction was proven to be an effective technology to extract oil from perilla seed, and GCMS was also a satisfactory method for analyzing the compositions of perilla seed oil.
基金Supported by the Science and Technology Key Project of Guangxi Province (0424008-1C)
文摘The physical properties and chemical components of three oil samples extracted from Illicium verum Hook. f. by steam distillation (SD), solvent extraction (SE) and supercritical fluid extraction (SFE) were compared with one another and analyzed by Gas Chromatography-Mass Spectrometry (GC-MS). The quality parameters of star anise essential oil from SFE were close to that of those came from SD and SE. Although the extraction yield of star anise by SFE (9.2 %) was close to the value from SE (9.3%), it was yet higher than that came from SD (8.2%). For sensory evaluation, however, three oils were significantly different. The odor and taste of the products from SFE and SE were generally more natural and vivid than that came from distilled oil. The volatile compound revealed that significant differences of the composition existed in the distilled oil and the oleoresins prepared by SFE and SE.
文摘The total volatile components were extracted from safflower by ultrasonic-assisted solvent extraction (USE) and their chemical constituents were analyzed by gas chromatographymass spectrometry (GC-MS) to provide scientific basis for the quality control of safflower. Five different solvents (diethyl ether, ethanol, ethyl acetate, dichloromethane and acetone) were used and compared in terms of number of volatile components extracted and the peak areas of these components in TIC. The results showed that USE could be used as an efficient and rapid method for extracting the volatile components from safflower. It also could be found that the number of components in the TIC of ethyl acetate extract was more than that in the TIC of other solvent ones. Meanwhile, the volatile components of safflower from Xinjiang Autonomous Region and Henan Province of China were different in chemical components and relative contents. It could be concluded that both the extraction solvents and geographical origin of safflower are responsible for these differences. The experimental results also indicated that USE/GC-MS is a simple, rapid and effective method to analyze the volatile oil components of safflower.
基金supported by the National Natural Science Foundation of China (31071541)a program for Changjiang Scholars and Innovative Research Team in University (IRT1188)
文摘As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more efficient technologies. Taking economic and environmental concerns into account, subcritical fluid extraction as a faster and more efficient method has stood out as a sample pre-treatment technology. This new extraction technology can overcome the shortcomings of supercritical fluid and achieve higher extraction efficiency at relatively low pressures and temperatures. In this experiment, a simple, sensitive and efficient method has been developed for the determination of diethylstilbestrol(DES) in fish tissue using subcritical 1,1,1,2-tetrafluoroethane(R134a) extraction in combination with gas chromatography-mass spectrometry(GC-MS). After extraction, freezing-lipid filtration was utilized to remove fatty co-extract. Further purification steps were performed with C_(18) and NH_2 solid phase extraction(SPE). Finally, the analyte was derived by heptafluorobutyric anhydride(HFBA), followed by GC-MS analysis. Response surface methodology(RSM) was employed to optimizing the extraction condition, and the optimized was as follows: extraction pressure, 4.3 MPa; extraction temperature, 26℃; amount of co-solvent volume, 4.7 m L. Under this condition, at a spiked level of 1, 5, 10 μg kg^(-1), the mean recovery of DES was more than 90% with relative standard deviations(RSDs) less than 10%. Finally, the developed method has been successfully used to analyzing the real samples.
基金financial support of the key project at the central government level:The Ability Establishment of Sustainable Use for Valuable Chinese Medicine Resources(No.2060302)the Independent Research Grant of National Resource Center for Chinese Materia Medica,China Academy of Chinese Medical Sciences(No.ZZXT201608)the National Natural Science Foundation of China(No.81603293)
文摘Soxhlet extraction is a common method of sample preparation. However, there has been no discussion about the efficiency of Soxhlet extraction from different batches and the factors that cause content fluctuation. In this study, Panax ginseng was selected as a model sample. Soxhlet extraction by means of a water bath, which has always been neglected, was identified as a novel key factor in the poor repeat- ability in different batches of Soxhlet extraction, as it can affect the siphon times and reflux time, which have been positively correlated with the ginsenoside contents. By substituting round bottom flasks in the same column, the relative standard deviation of the most fluctuated compound, ginsenoside Rbl, was decreased from 24.6% to 5.02%. Scanning electron microscopy analysis confirmed that the breakdown of the surface of the ginseng powder in the Soxhlet extraction led to a better dissolution of ginsenosides, indicating that chloroform may promote the extraction of ginsenosides by disrupting the cell structure. Moreover, 70% methanol was regarded as the better solvent for extracting the ginsenosides. Overall, this work offers a practical and effective protocol for improving the accuracy and repeatability of Soxhlet extraction methodology for ginsenosides and other analytes.
文摘The application of soxhlet, ultrasonic and accelerated solvent extractiontechniques to the analysis of six organochlorine pesticides (α-HCH, β-HCH, γ-HCH, o, p'-DDT,p,p'-DDT and p,p'-DDE) in Taihu Lake sediment samples is described. It was found that the limits ofquantification ranged from 0.002 μg g^(-1) to 0.004 μg g^(-1), and the recoveries oforganochlorine pesticides with the three extraction techniques were acceptable ( 】80.7%). With amass selective detector, better results were obtained by accelerated solvent extraction usinghexane-acetone (1:1) as compared with soxhlet and ultrasonic extraction. It was shown that theaccelerated solvent extraction was the optimum technique for the analysis of organochlorinepesticides in sediments. The general features of the three extraction techniques are also presented.
文摘Extraction of castor oil from castor seeds was investigated using different green solvents which include d-limonene, p-cymene, α-pinene, ethanol, and furfural at the temperature range of (323 - 413) K. The Soxhlet extraction method was employed to investigate the effect of temperature at atmospheric pressure. The focus of the study was to investigate a potential green solvent that can produce the high yields compared to the traditional solvent (hexane). The results show that at the average time of 3 hours and 30 minutes, the castor oil yield for green solvents were ranked as furfural (47.13%) > ethanol (45.37%) > p-cymene (39.15%) > d-limonene (39.13%) > α-pinene (38.11%). These castor oil yields were obtained at optimum temperatures for each green solvent. The castor oil yields were compared to the yield of hexane (31.36%) at same average time. The green solvents were recovered by using simple distillation, except furfural which was difficult to be recovered.
文摘In this study,a GC-MS/SIM method was used to analyze 16 PAHs in soil by ASE on-line clean-up.The average recoveries were ranged from 67% to 129%.The relative standard deviations were between 2.7% and 21.1%.The calculated limits of detection were no more than 0.95 ng/g.This method was fast,simple,and cost-saving,and can be used in the large quantities of samples analysis.
文摘In this paper,the Illilium verum Hook.f.grow at mountain of Dayao of Jinxiu in Guangxi,Volatile oil was extracted by soxhet method and steam distillation.All the volatile oil was analyzed by GC-MS,the result show the ingredients and rate of product were change greatly,The major chemical constituents were trans-anethole,estragole and anisaldehyde etc.
文摘A method was established for determination of the reducing substances released from plastic blood bags to anticoagulant.The samples were extracted with a solid-phase extraction procedure using dichloromethane as extract solvents.The extracts were measured with GC-MS.Several reducing substances,such as 1,2-benzenedicarboxylic acid,alkane and bis(2-ethylhexyl) phthalate,etc were found in anticoagulant.The method was simple and can be used for the quality control of plastic blood bags.
基金Supported by Important Direction Project of Knowledge Innovation Program in Chinese Academy of Science(KZCX2-YW-446)~~
文摘[Objective] The aim of this study was to find a better method to exactly quantify the residual polycyclic aromatic hydrocarbons(PAHs)in the long-term contaminated soil in the field so as to provide basis for the remediation for PAHs contaminated soil.[Method]The comparisons of soxhlet extraction,ultrasonic extraction and shaking extraction were studied in the agricultural soil irrigated with oil sewage over a long period of time.[Result]The total PAHs extracted by soxhlet extraction were the highest(6 873.7 μg/kg),followed by shaking extraction(6 698.8 μg/kg)and ultrasonic extraction(5 737.6 μg/kg).Among these methods,the highest extracted 4 and 6 rings PAHs were in the soxhlet extraction,the highest extracted 2 and 5 rings PAHs were in the shaking extraction,and the highest extracted 3 rings PAHs were in the ultrasonic extraction.[Conclusion]This study had provided basis for the selection of the assessment method of residual PAHs in the field soil.