Three extraction techniques have been recently used for the quantitative extraction of semi-volatile organic pollutants in sediments, i.e. accelerated solvent extraction （ASE）, microwave assisted extraction （MAE） ...Three extraction techniques have been recently used for the quantitative extraction of semi-volatile organic pollutants in sediments, i.e. accelerated solvent extraction （ASE）, microwave assisted extraction （MAE） and ultrasonic assisted extraction （UAE）. However, their extraction efficiencies have rarely been quantitatively compared using rigorous mathematical methods. In this paper, one-way analysis of variance （ANOVA） was employed to evaluate the performance of ASE, MAE and UAE in the overall extraction of PCBs, DDTs and HCHs by analysis of their recoveries from the Standard Reference Material IAEA-417, a sediment sample certified by many international laboratories. Conclusions were drawn at a significance level of P〈 0.05. No significant differences were found among the mean values for method recoveries using ASE, MAE and UAE. The mean values for real recoveries using ASE and MAE were nearly identical, but the real recovery using UAE was much lower. The concentrations of all PCBs, DDTs and HCHs except for CB52 and o,p＇-DDT using UAE were the lowest. Comparing the results obtained using ASE with MAE, the concentrations of CB28, CB52, CB138, ct-HCH, [3-HCH, p,p＇-DDE and p,p＇-DDD were nearly identical, while the concentrations of other compounds were significantly different. Based on the low recoveries, it was concluded that UAE is a relatively inefficient extraction method, while ASE and MAE are equivalent methods. Taking into consideration the relative standard deviation （RSD） values, solvent volume, extraction time, and purchasing costs of the apparatus, MAE was considered superior to ASE for extraction of PCBs, DDTs and HCHs.展开更多
It takes flavonoid extraction rate as indicator and adopts the method of orthogonal experiment to study process of total flavonoid in Trollius chinensis through ultrasonic wave assisted extraction, microwave assisted ...It takes flavonoid extraction rate as indicator and adopts the method of orthogonal experiment to study process of total flavonoid in Trollius chinensis through ultrasonic wave assisted extraction, microwave assisted extraction and backflow extraction, as well as optimization of process parameter. The result indicates that in terms of extraction efficiency, microwave extraction method is better than ultrasonic radiation extraction method, which is better than backflow extraction method. Optimal process parameter through backflow extraction is： backflow temperature 60℃, fluid material ratio 1：20, ethanol density 65%, backflow time 60min; optimal process parameter through ultrasonic wave assisted extraction is： ultrasonic radiation temperature 70℃, fluid material ratio 1：20, ethanol density 65%, ultrasonic wave radiation time 45rain; optimal process parameter of microwave assisted extraction is： microwave radiation temperature 60℃, fluid material ratio 1：20, ethanol density 75%, microwave radiation time 45min.展开更多
This paper reports the extraction of aloe-emodin from aloe by microwave-assisted extraction. The effects of various factors, including the solvent, the ratio （mL/g） of the solvent to the sample, microwave irradiatio...This paper reports the extraction of aloe-emodin from aloe by microwave-assisted extraction. The effects of various factors, including the solvent, the ratio （mL/g） of the solvent to the sample, microwave irradiation time and microwave power, were discussed in the experiments. The yield of aloe-emodin was determined by HPLC. The optimized conditions for micro- wave-assisted extraction of aloe-emodin were concluded as follows： the solvent is 80% ethanol （V/V） solution, microwave ir- radiation time is 3 rain and microwave power is 340 W. Additionally, HPLC fingerprint was developed for consistency evalua- tion of aloe. The similarities of 3 aloe samples obtained by microwave-assisted extraction, ultrasound-assisted extraction and Soxhlet extraction were more than 0.9, indicating that 3 aloe samples were consistent. Compared with Soxhlet extraction and ultrasound-assisted extraction, microwave extraction is a rapid method with higher yield and less solvent consumption. Aloe samples treated by microwave-assisted extraction, ultrasound-assisted extraction and Soxhlet extraction were observed using transmission electronic microscopy. The micrographs provide evidence of more breakage of chloroplasts treated by micro- wave-assisted extraction as compared to Soxhlet extraction and ultrasound-assisted extraction.展开更多
基金Supported by the National High Technology Research and Development Program of China (No. 2007AA09Z126)the Marine Science Foundation for Young Scholars of SOA (No. 2011519)Marine Commonwealth Scientific Support Fund of SOA (Nos. 201005034, 201105013)
文摘Three extraction techniques have been recently used for the quantitative extraction of semi-volatile organic pollutants in sediments, i.e. accelerated solvent extraction （ASE）, microwave assisted extraction （MAE） and ultrasonic assisted extraction （UAE）. However, their extraction efficiencies have rarely been quantitatively compared using rigorous mathematical methods. In this paper, one-way analysis of variance （ANOVA） was employed to evaluate the performance of ASE, MAE and UAE in the overall extraction of PCBs, DDTs and HCHs by analysis of their recoveries from the Standard Reference Material IAEA-417, a sediment sample certified by many international laboratories. Conclusions were drawn at a significance level of P〈 0.05. No significant differences were found among the mean values for method recoveries using ASE, MAE and UAE. The mean values for real recoveries using ASE and MAE were nearly identical, but the real recovery using UAE was much lower. The concentrations of all PCBs, DDTs and HCHs except for CB52 and o,p＇-DDT using UAE were the lowest. Comparing the results obtained using ASE with MAE, the concentrations of CB28, CB52, CB138, ct-HCH, [3-HCH, p,p＇-DDE and p,p＇-DDD were nearly identical, while the concentrations of other compounds were significantly different. Based on the low recoveries, it was concluded that UAE is a relatively inefficient extraction method, while ASE and MAE are equivalent methods. Taking into consideration the relative standard deviation （RSD） values, solvent volume, extraction time, and purchasing costs of the apparatus, MAE was considered superior to ASE for extraction of PCBs, DDTs and HCHs.
文摘It takes flavonoid extraction rate as indicator and adopts the method of orthogonal experiment to study process of total flavonoid in Trollius chinensis through ultrasonic wave assisted extraction, microwave assisted extraction and backflow extraction, as well as optimization of process parameter. The result indicates that in terms of extraction efficiency, microwave extraction method is better than ultrasonic radiation extraction method, which is better than backflow extraction method. Optimal process parameter through backflow extraction is： backflow temperature 60℃, fluid material ratio 1：20, ethanol density 65%, backflow time 60min; optimal process parameter through ultrasonic wave assisted extraction is： ultrasonic radiation temperature 70℃, fluid material ratio 1：20, ethanol density 65%, ultrasonic wave radiation time 45rain; optimal process parameter of microwave assisted extraction is： microwave radiation temperature 60℃, fluid material ratio 1：20, ethanol density 75%, microwave radiation time 45min.
基金supported by the National Key Technology R&D Program (2006BAI09B07-02)
文摘This paper reports the extraction of aloe-emodin from aloe by microwave-assisted extraction. The effects of various factors, including the solvent, the ratio （mL/g） of the solvent to the sample, microwave irradiation time and microwave power, were discussed in the experiments. The yield of aloe-emodin was determined by HPLC. The optimized conditions for micro- wave-assisted extraction of aloe-emodin were concluded as follows： the solvent is 80% ethanol （V/V） solution, microwave ir- radiation time is 3 rain and microwave power is 340 W. Additionally, HPLC fingerprint was developed for consistency evalua- tion of aloe. The similarities of 3 aloe samples obtained by microwave-assisted extraction, ultrasound-assisted extraction and Soxhlet extraction were more than 0.9, indicating that 3 aloe samples were consistent. Compared with Soxhlet extraction and ultrasound-assisted extraction, microwave extraction is a rapid method with higher yield and less solvent consumption. Aloe samples treated by microwave-assisted extraction, ultrasound-assisted extraction and Soxhlet extraction were observed using transmission electronic microscopy. The micrographs provide evidence of more breakage of chloroplasts treated by micro- wave-assisted extraction as compared to Soxhlet extraction and ultrasound-assisted extraction.
