正交实验法在小麦粉中甲醛振荡提取条件的应用研究

小麦粉中甲醛的提取问题是一个比较复杂的多因素问题。采用正交实验法,选用L9(34)正交实验表,在提取试剂、提取温度、提取时间等多个因素和水平中优选小麦粉中甲醛振荡提取的最佳条件。实验中甲醛提取量采用Nash试剂柱前衍生高效液相色谱法测定。结果表明,提取温度是小麦粉中甲醛提取的最主要因素,最佳的提取条件为提取温度30℃、提取液为硫酸钠、提取时间为40min。     

Pressurized liquid extraction followed by high-performance liquid chromatography for determination of seven active compounds in Cortex Dictamni

A new method based on pressurized liquid extraction (PLE) followed by a sensitive and specific HPLC-DAD analysis is developed for determination of seven compounds in Cortex Dictamni. The operational parameters of PLE, such as extraction solvent, extraction temperature, extraction pressure, static extraction time, flush volume and extraction cycles were optimized, using the extraction efficiencies of dictamnine, obacunone and fraxinellone as targets. The optimized procedure employed MeOH as extraction solvent, 150 degrees C of extraction temperature, 1,500 psi extraction pressure, 5 min of static extraction time, 60% flush volume and the extraction recoveries of the three compounds were nearly to 100% for only one cycle. The following HPLC analysis was performed on a reversed-phase C(18) column with methanol-water as mobile phase in gradient manner, detected at 236 and 218 nm. The limits of detection (LOD) and limits of quantification (LOQ) of the seven compounds were in the range of 0.4-15.6 ng and 1.2-38.8 ng. This assay can be readily utilized as a quality control method for Cortex Dictamni and other related medicinal plants.     

Miniaturized solid-phase extraction as a sample preparation technique for the determination of phthalates in water

Miniaturized solid-phase extraction (SPE) has been developed and successfully employed for the determination of organic species in water samples by liquid chromatography (LC). The method is based on the concept of a microscale extraction technique using a fused-silica capillary column for gas chromatography (GC), so-called in-tube solid-phase microextraction (SPME). The extraction conditions, such as the extraction time and flow-rate for the extraction and desorption process, were investigated as well as the effect of the internal structure of the extraction capillary on the efficiency. By inserting a stainless steel wire into the extraction capillary to reduce the internal volume of the capillary with the same surface area of the coating, an improved extraction and pre-concentration effects were obtained. Further pre-concentration was accomplished by the extraction device with a novel fiber-in-tube configuration. The direct coupling of the extraction method with a LC system has made it possible to determine low levels of phthalates in water samples without high consumption of organic solvents. The system developed must have potential applications for the analysis of environmental and biological samples in aqueous sample matrices.     

Optimization and comparison of MAE, ASE and Soxhlet extraction for the determination of HCH isomers in soil samples

The microwave-assisted extraction (MAE), accelerated solvent extraction (ASE) and Soxhlet extraction of two isomers of hexachlorocyclohexane, alpha-HCH and gamma-HCH, from a polluted landfill soil have been optimized following different experimental designs. In the case of microwave-assisted extraction, the following variables were considered: pressure, extraction time, microwave power, percentage of acetone in n-hexane mixture and solvent volume. When ASE extraction was studied the variables were pressure, temperature and extraction time. Finally, the percentage of acetone in n-hexane mixture and the extraction time were the only variables studied for Soxhlet extraction. The concentrations obtained by the three extraction techniques were, within their experimental uncertainties, in good agreement. This fact assures the possibility of using both ASE and MAE techniques in the routine determination of lindane in polluted soils and sediments.     

Evaluation of microwave-assisted extraction for aristolochic acid from Aristolochiae Fructus by chromatographic analysis coupled with nephrotoxicity studies

In this paper, a microwave-assisted extraction (MAE) method was established for aristolochic acid-I from Aristolochiae Fructus, and the advantage of MAE was evaluated by chromatographic analysis coupled with nephrotoxicity studies. The experimental parameters of MAE for aristolochic acid-I in Aristolochiae Fructus were investigated and MAE was compared with Soxhlet extraction and ultrasound-assisted extraction in terms of extraction yields and extraction conditions. Under the optimum conditions, MAE could provide higher extraction yields of aristolochic acid-I (1.10 mg/g) than ultrasound-assisted extraction (0.82 mg/g) and Soxhlet extraction (0.95 mg/g), in addition to using less solvent and having a shorter extraction time. Furthermore, the nephrotoxicities of the extracts of Aristolochiae Fructus from different extraction procedures were investigated in Sprague-Dawley rats. The results of nephrotoxicity studies of, for example, general conditions, biochemistry parameters and histopathology examination showed no significantly differences in the nephrotoxicity levels of the extracts from MAE and that from Soxhlet extraction. These results indicated that MAE technique is a simple, rapid and effective extraction method, and the microwave irradiation during MAE procedure did not have any influence on the nephrotoxicity of Aristolochiae Fructus compared with Soxhlet extraction.     

Dynamic Microwave-assisted Extraction of Flavonoids from Radix Scutellariae

IntroductionRadix Scutellariaeis the root ofScutellaria bai-calensis Georgi(Labiatae), which is widely cultivatedand used as traditional Chinese medicine. It has beendemonstrated to be anti-inflammatory, anti-metamor-phic, antiviral, anti-hot, and live pr…     

A comparison of accelerated solvent extraction,Soxhlet extraction,and ultrasonic-assisted extraction for analysis of terpenoids and sterols in tobacco

The performance of accelerated solvent extraction in the analysis of terpenoids and sterols in tobacco samples was investigated and compared with those of Soxhlet extraction and ultrasonically assisted extraction with respect to yield, extraction time, reproducibility and solvent consumption. The results indicate that although the highest yield was achieved by Soxhlet extraction, ASE appears to be a promising alternative to classical methods since it is faster and uses less solvent, especially when applied to the investigation of large batch tobacco samples. However, Soxhlet extraction is still the preferred method for analyzing sterols since it gives a higher extraction efficiency than other methods.     

Ionic liquids based microwave-assisted extraction of lichen compounds with quantitative spectrophotodensitometry analysis

Ionic liquids based extraction method has been applied to the effective extraction of norstictic acid, a common depsidone isolated from Pertusaria pseudocorallina, a crustose lichen. Five 1-alkyl-3-methylimidazolium ionic liquids (ILs) differing in composition of alkyl chain and anion were investigated for extraction efficiency. The extraction amount of norstictic acid was determined after recovery on HPTLC with a spectrophotodensitometer. The proposed approaches (IL-MAE and IL-heat extraction (IL-HE)) have been evaluated in comparison with usual solvents such as tetrahydrofuran in heat-reflux extraction and microwave-assisted extraction (MAE). The results indicated that both the characteristics of the alkyl chain and anion influenced the extraction of polyphenolic compounds. The sulfate-based ILs [C(1)mim][MSO(4)] and [C(2)mim][ESO(4)] presented the best extraction efficiency of norstictic acid. The reduction of the extraction times between HE and MAE (2 h-5 min) and a non-negligible ratio of norstictic acid in total extract (28%) supports the suitability of the proposed method. This approach was successfully applied to obtain additional compounds from other crustose lichens (Pertusaria amara and Ochrolechia parella).     

Dynamic microwave-assisted extraction

An apparatus for extraction of solid matrices has been constructed which utilizes a microwave technique for heating in a dynamic mode. During the extraction, fresh solvent is continuously pumped through the extraction cell, which is maintained at a slight overpressure in order to keep the solvent in a liquid state. The extraction efficiency, which can be easily monitored, has been investigated in a factorial design and validated for polycyclic aromatic hydrocarbons in a reference sediment sample (EC-1). Important parameters were found to be temperature and duration of extraction. Flow-rate had no significant first-order effect on the recovery, but interaction effects with flow-rate were found to be significant. The dynamic microwave-assisted extraction apparatus was demonstrated to yield recoveries equivalent to Soxhlet extraction, but in a much shorter time. Each extraction of EC-1 typically takes 40 min.     

An investigation into the sorption of benzoic acids by polyurethane membrane

The extraction mechanism of organic compounds by ether- and ester-type polyurethane membrane has been investigated through a detailed study of sorption of monobromobenzoic acids. The effects of solution concentration, extraction time, surface area, pH, salts, and temperature on extraction were studied. It was found that monobromobenzoic acids are extracted in their neutral form, and that the extraction is controlled primarily by the relative strength of intra- and intermolecular hydrogen bonding. The ether-type polyurethane membrane allows a more efficient removal of monobromobenzoic acids from solution than the ester-type membrane. The extraction of benzoic acids with the ether-type membrane decreases as the temperature increases. When the ester-type polyurethane membrane is used, an extraction maximum is observed at room temperature with a decrease in extraction at lower and higher temperatures.     

正交试验优化土壤萃取法及常见无机阴离子的离子色谱分析

实验采用超声提取离子色谱法测定土壤中常见无机阴离子的含量,以正交试验优化土壤中阴离子的提取条件。研究土壤粒径、料液比、提取功率、提取时间对土壤中阴离子提取量的影响。结果表明:土壤中阴离子提取的最佳条件为A1B2C3D3。即超纯水为提取液,土壤粒径为180μm,料液比为1:30,超声波作用时间为40 min,提取功率为320W,提取次数为一次。该方法可用于土壤中常见可溶性无机阴离子含量的提取测定。     

Comparison of different extraction techniques for the determination of polychlorinated organic compounds in sediment

The performance of various enhanced extraction techniques, such as accelerated solvent extraction, microwave-assisted extraction, Soxhlet extraction, ultrasonic extraction and fluidized-bed extraction for the determination of polychlorinated organic compounds in dry sediment was investigated in two laboratories. The results of the two laboratories were in good agreement. The extraction yields from the batch extraction methods were lower than those from the dynamic techniques. Accelerated solvent extraction, especially, exhibited higher extraction efficiency than the standard procedure, Soxhlet extraction, whereas the results of fluidized-bed extraction were comparable.     

山楂叶中熊果酸提取工艺研究

以熊果酸的提取率为指标,采用单因素与正交实验相结合的方法对提取工艺进行了优化,得到最佳提取参数为:乙醇体积分数95%、提取温度85℃、提取时间110min、液固比5:1、提取次数3次。在该条件下,熊果酸提取率为93.47%。该工艺简单合理,为工业生产提供了理论参考。     

Development of Green and Efficient Extraction of Bioactive Ginsenosides from Panax ginseng with Deep Eutectic Solvents

The extraction of active constituents from natural sources in a green and efficient manner is considered an important field in the pharmaceutical industry. In recent years, deep eutectic solvents (DESs), a new type of green solvent, have attracted increasing attention. Therefore, we aimed to establish a green and high-efficiency extraction method for ginsenosides based on DESs. This study takes Panax ginseng as a model sample. Eighteen different DESs were produced to extract polar ginsenosides. Ultrasound-assisted extraction (UAE) was applied for simplicity and efficiency. A binary DES synthesized using choline chloride and urea at a proportion of 1:2 prepared by a heating stirring method is proven to be more effective than other solvents, such as the widely used 70% ethanol for the extraction of ginsenosides. Three variables that might affect the extraction, including the DES content in the extraction solvent, liquid/solid ratio, and ultrasound extraction time, were evaluated for optimization. The optimum extraction conditions for ginsenosides were determined as follows: DES water content of 20 wt%, liquid/solid ratio of 15 mL g⁻¹, and an ultrasonic extraction time of 15 min. The extraction yield for the optimized method is found to be 31% higher than that for 70% ethanol, which achieves efficient extraction. This study shows that DESs are available to extract ginsenosides for use in traditional Chinese medicine. The discovery also contributes to further research into the green extraction of ginsenosides.     

Pressurized liquid extraction as a green approach in food and herbal plants extraction: A review

Pressurized liquid extraction is a “green” technology for the extraction of nutraceuticals from foods and herbal plants. This review discusses the extraction principles and the optimization of the extraction parameters that improves the extraction efficiency. The use of different solvent mixtures and other extraction additives to enhance the efficiency of the extraction are discussed. Dynamic mode of extraction in Pressurized liquid extraction, and the use of combined and hyphenated sample preparation and analytical techniques are presented. This work discusses how different studies used Pressurized liquid extraction to enrich phenolic compounds, lignans, carotenoids, oils and lipids, essential oils and other nutraceuticals from foods and herbal plants.     

Enhanced extraction of polychlorinated organic compounds from soil samples by fluidized-bed extraction (FBE)

Summary The extraction and determination of polychlorinated organic compounds, like hexachlorobenzene, pentachlorobenzene, octachlorostyrene and polychlorinated biphenyls in soils and solid wastes continues to be a subject for study. In this work Soxhlet extraction and a new extraction technique, fluidized-bed extraction, have been compared. The extraction of polychlorinated organic compounds by this technique has been optimized using experiemental design procedures. The variation of the number of extraction cycles, composition of extraction solvent (mixtures ofn-hexane-acetone) and the holding time after reaching the heating temperature were considering as experimental variables to generate a surface response design. Gas chromatography with mass spectrometric detection was used to determine levels of the analytes in the extracts. Extraction and analysis of a certified reference material (BCR CRM 392) showed the applicability of the method.     

Optimum Ultrasound Assisted Extraction Conditions of Some Flavonoids from Green Tea Leaves. Control Quality of Green Tea Product by TLC Fingerprinting

The optimization of the green tea flavonoid extraction conditions was investigated. The experiments were carried out with two extraction methods: ultrasound assisted extraction (UAE) and reflux extraction (RE). The parameters that were varied in this study were: the extraction solvent system composition, the type of organic modifier of the extraction mixture, temperature, and time. The highest efficiency was obtained with an extraction mixture of ethanol: water, 80:20, v/v. An extraction performed at temperature of 45°C in 50–60 minutes led to optimum results. Moreover, a new fingerprinting procedure based on thin layer chromatography (TLC) image analysis was employed in order to compare the chemical composition of green tea in comparison with white and black tea.     

Development of a magnetic solid‐phase extraction coupled with high‐performance liquid chromatography method for the analysis of polyaromatic hydrocarbons

A novel magnetic solid phase extraction coupled with high‐performance liquid chromatography method was established to analyze polyaromatic hydrocarbons in environmental water samples. The extraction conditions, including the amount of extraction agent, extraction time, pH and the surface structure of the magnetic extraction agent, were optimized. The results showed that the amount of extraction agent and extraction time significantly influenced the extraction performance. The increase in the specific surface area, the enlargement of pore size, and the reduction of particle size could enhance the extraction performance of the magnetic microsphere. The optimized magnetic extraction agent possessed a high surface area of 1311 m²/g, a large pore size of 6–9 nm, and a small particle size of 6–9 μm. The limit of detection for phenanthrene and benzo[g,h,i]perylene in the developed analysis method was 3.2 and 10.5 ng/L, respectively. When applied to river water samples, the spiked recovery of phenanthrene and benzo[g,h,i]perylene ranged from 89.5–98.6% and 82.9–89.1%, respectively. Phenanthrene was detected over a concentration range of 89–117 ng/L in three water samples withdrawn from the midstream of the Huai River, and benzo[g,h,i]perylene was below the detection limit.     

Comparison of supercritical fluid and ultrasound-assisted extraction of carotenoids and chlorophyll a from Dunaliella salina

In the work described here the extraction processes of carotenoids and chlorophylls were analysed using two extraction techniques, namely ultrasound-assisted extraction and supercritical fluid extraction, and the results are compared. The solvents used for the ultrasound-assisted extraction were N,N′-dimethylformamide and methanol and for the supercritical fluid extraction, carbon dioxide. The raw material studied was Dunaliella salina, a microalgae characterized by the high levels of carotenoids present in its cellular structure. The results indicate that the supercritical fluid extraction process is comparable to the ultrasound-assisted extraction when methanol is used as solvent. In addition, the supercritical extraction process is more selective for the recovery of carotenoids than the conventional technique since it leads to higher values for the ratio carotenoids/chlorophylls. Finally, the effects of pressure and temperature on the extraction yields of the supercritical fluid extraction process were studied.     

微波萃取在中药提取中的应用

微波萃取是一种新型高效的萃取技术,对中药的现代化发展尤为重要。微波萃取技术具有选择性好、萃取速度快、提取效率高等特点,可应用于黄酮类、多糖类、苷类、挥发油、蒽醌类、有机酸类、生物碱类等中药有效成分的提取中。