加拿大一枝黄花总酚超声提取工艺

利用超声提取的方法,通过单因素和正交实验分析了溶液浓度、超声时间、料液比、提取次数4个主要因素对总酚提取率的影响。确立了加拿大一枝黄花总酚的最佳提取工艺条件为:60%甲醇、超声50min、料液比1∶20、提取3次。在此条件下,总酚的提取率为44.61mg/g。     

Ultrasound-assisted extraction of ginseng saponins from ginseng roots and cultured ginseng cells

Ultrasound-assisted extraction was evaluated as a simpler and more effective alternative to conventional extraction methods for the isolation of ginsenosides (saponins) from various types of ginseng. The ginseng samples were extracted with different solvents, under either direct sonication by an ultrasound probe horn or indirect sonication in an ultrasound cleaning bath. The ultrasonic extraction was compared with the conventional method of refluxing boiling solvents in a soxhlet extractor, on the yields of both the total saponin isolated by thin-layer chromatography and the individual ginsenosides by high performance liquid chromatography. It was found that the sonication-assisted extraction of ginseng saponins was about three times faster than the traditional extraction method. The ultrasonic extraction was not only more efficient but also convenient for the recovery and purification of the active ingredients of plant materials. In addition, the sonication-assisted extraction can be carried out at lower temperatures which are favorable for the thermally unstable compounds.     

分子印迹材料选择性截留卷烟烟气中芳胺的研究

采用分子印迹技术合成了一种对1-萘胺有高度选择性的分子印迹聚合物材料。应用固相萃取吸附试验研究了该聚合物对1-萘胺及其结构类似物的选择特性,表明印迹聚合物材料对4种芳胺类物质表现出良好的选择性结合能力。将所制备的印迹聚合物按不同剂量添加到卷烟嘴棒中,考察其对卷烟烟气中芳胺的截留效果。结果显示,该分子印迹材料能选择性截留卷烟烟气中的1-萘胺、2-萘胺、3-氨基联苯和4-氨基联苯等烟气有害成分;当印迹聚合物添加量为50mg时,卷烟烟气中芳胺的降低率达到30%。     

Ultrasound-assisted polysaccharide extraction from Cercis chinensis and properites,antioxidant activity of polysaccharide

The purpose of the study was to improve the extraction of polysaccharide from the leaves of Cercis chinensis Bunge using ultrasound, and compare the difference between boiling and ultrasound extraction in terms of polysaccharide content, monosaccharide compounds, and evaluate how the factors affected the bioactivity. The best conditions, according to the single factor experiments and the Box-Bohnken design (BBD), were an intensity of ultrasound of 180 W, duration of extraction of 40 min, proportion of water to material of 15:1 (g/g), and a higher polysaccharide yield of 20.02 ± 0.55 (mg/g) than in boiling extraction (16.09 ± 0.82 mg/g). The antioxidative experiment suggested the polysaccharide by ultrasound exhibited higher DPPH, hydroxyl radical scavenging capacities, and reducing power at 1.2–1.4 mg/mL, which was superior to the boiling polysaccharide. Further analysis showed that the ultrasonic purified polysaccharides like Gla, N-Glu, and GluA contained more total sugar and uronic acids than the boiling method did. This may indicate that the ultrasonic isolation of the polysaccharides increase the antioxidant activity of the polysaccharides.     

Off-line SFE-CGC-ECD analysis of 2,4-D and Dicamba residues in real sugar cane,rice and corn samples

Determination of 2,4-D (2,4-dichlorophenoxyacetic acid) and Dicamba (2-methoxy-3,6-dichlorobenzoic acid) residues in sugar cane, rice, and corn was carried out both by solid liquid extraction (SLE), as already described in the literature, and by a supercritical fluid extraction (SFE) method developed in our laboratory. The extracts were esterified and cleaned-up by passing through a Florisil column. Extracts were analyzed by high resolution gas chromatography, with electron capture detection. The tested methods presented good recoveries (above 90%); the SFE CO₂/acetone method showed better extraction efficiencies (extracted 30 % more herbicide in real samples), shorter extraction time and lower organic solvent consumption than the SLE method.     

碘-四氯化碳萃取光度法间接测定食品中的痕量过氧化氢

在 p H1.0— 3.0稀硫酸介质中 ,一定的反应条件下 ,过氧化氢与碘化钾反应 ,释放出一定量的碘 ,建立了碘 -四氯化碳萃取光度法间接测定痕量过氧化氢。共存离子基本上不干扰测定 ,过氧化氢的检测限为0 .0 5 μg·m L-1;回收率在 94 %— 98%之间 ,结果令人满意     

微波辅助提取刺梨中总黄酮的工艺参数优化

以刺梨果实为原料,对微波辅助提取刺梨中的总黄酮的工艺进行研究,采用单因素试验法对影响微波辅助提取刺梨果实中总黄酮的影响因素进行分析,利用正交试验优化提取总黄酮的工艺条件。研究表明,微波辅助提取刺梨总黄酮的最佳工艺条件为:料液比1:20(g/mL),乙醇浓度60%,微波萃取功率400W,微波辐射时间3min。最佳工艺条件下的总黄酮的提取率为1.39%。     

Determination of 2,4-D and Dicamba in food crops by MEKC

Summary The determination of 2,4-D (2,4-dichlorophenoxyacetic acid) and Dicamba (2-methoxy-3,6-dichlorobenzoic acid) residues in sugar cane, rice and corn was performed by a supercritical fluid extraction (SFE) method using CO₂/acetone as extraction mix and an SFE apparatus developed in our laboratory. The extracts were cleaned up after extraction by both liquid-liquid partition and a Florisil column. Micellar electrokinetic capillary chromatography (MEKC) coupled with ultraviolet on-column detection was used for the analysis of these pesticides. The detection limits were improved by the preparation of a special detection cell with an increased pathlength that gave detection limits of ca. 0.6 pg for 2,4-D and Dicamba. Our results demonstrated that capillary electrophoresis can be a powerful new analytical tool for pesticide residue analysis.     

Cyclic and acyclic S2O2 donor-type ionophores. Ion-pair extraction and transport of Ag(I) picrate, and X-ray confirmation of existence of the ion-pair complex

Extraction and transport behaviors of isomeric oxathia macrocycles (L₂, ortho-; L₃, meta- and L₄, para-isomer) and their structure related open-chain compound (L₁) towards Ag(I) picrate have been examined. From the plot of log (D_Ag(I)/[pic⁻]) vs. log [L]₀ for all of the ionophores were linear with slope near unity, thereby confirming the 1:1:1 complex formations of Ag(I)/ligand/picrate ion to be extracted into the dichloromethane phase. The extractability of an acyclic ionophore was superior to those of the corresponding cyclic ones. In membrane transport experiments, the slow rate of release of Ag(I) from the membrane into the receiving phase seems to be responsible for lower transport efficiency. Upon addition of sodium thiosulfate as a stripping reagent in receiving phase, the efficiency of transport is significantly enhanced in the order of L₁ (acyclic)>L₂ (ortho-)>L₃ (meta-)>L₄ (para-) in accordance with those of log K_ex values. It is hypothesized that the ion-pair complexation of L₁ in extraction step would be more favorable in extraction and transport of Ag(I). Its structure have been confirmed by X-ray diffraction analysis of [Ag(L₁)pic], where L₁=1,10-bis(mercaptobenzylyl)-4,7-dioxadecane.     

Retention effects of oxidized polyphenols during analytical extraction of phenolic compounds of virgin olive oil

The hydrophilic extract of virgin olive oil contains several phenolic compounds such as simple phenols, lignans, and secoiridoids that have been widely studied in recent years. Interest in the hydrophilic extract has also been extended to the fraction of oxidized phenols that form during storage as a consequence of oxidative stress. The present investigation compares the two most commonly used extraction methods, namely liquid-liquid extraction and SPE, on fresh virgin olive oil and that kept at different temperatures in the presence of oxygen to promote the formation of oxidative products. The selective retention of these natural and oxidized phenolic compounds in relation to the extraction method was assessed. Quantification of eight identified phenolic molecules and 11 unknown peaks was performed by HPLC-DAD/MSD.