索氏提取器装置的改进与应用

索氏提取器是化学实验常用的提取装置，"茶叶中咖啡因的提取"是有机化学实验中的重要实验。针对传统索氏提取器提取温度低、提取时间长、提取效率低、虹吸管易碎、提取筒和虹吸管易污染或堵塞等弊端，在提取筒外增设外筒，可有效保护虹吸管且对提取筒起加热和保温作用，以提高提取温度和提取效率，缩短提取时间；冷凝管下端改设喇叭口和倒刺，便于悬挂样品袋，防止提取筒和虹吸管受污染或堵塞，由此得到改进装置。并用于茶叶中咖啡因的提取实验以对改进装置进行效果评价。实验数据表明，改进装置不仅克服了传统装置存在的弊端，更保持了传统装置的特点和功能，使用方便安全，提取效率高，值得在高校推广。     

索氏提取器的简易替代装置

索氏提取器是化学实验中常用的提取装置,其特点是操作简单,具有连续性,提取率较高,但该装置造价高,虹吸管易破碎,装料及清理较困难。因此,我们对其进行了一些改进。     

一种快速抽提微量成分的热逆流提取装置

液固萃取在化学实验及研究中常常遇到,索氏提取器是液团萃取普遍采用的装置,它具有简单、提取率高等特点,但采用索氏提取器从较大体积的固体样品中提取微量成分是很困难的。对于要求在较高温度下进行液固萃取也难于实现。为此我们设计了一种热逆流提取器,它不仅可满足上述要求,而且使萃取过程连续化。该装置主要由单口烧瓶、三颈烧瓶和热逆流提取器组成(图1)。     

改进的索氏萃取器在控制液固萃取终点时的应用

索氏萃取器是一种用有机溶剂从固体样品中连续萃取一定组分的仪器 ,在研究中药有效成分的提取方面有较为广泛的应用。但是用现有的索氏萃取器研究控制液固萃取终点时 ,只能在关闭热源待蒸馏瓶冷却下来后分析萃取室溶液中一定组分的含量 ,需要多次更换装有药粉的滤纸筒才能得到一组实验结果。这样既浪费时间 ,又消耗过多的费用。我们对索氏萃取器进行了改进 ,得到了一种便于控制液固萃取终点的索氏萃取器 (图 1 ) ,现以石油醚提取盾叶薯蓣水解残渣 (水解物 )中的薯蓣皂甙元为例介绍如下。图 1　改进的索氏萃取器　1　试剂与仪器　　 71 0型紫…     

油脂快速萃取装置萃取时间选择试验

3-86普及型油脂快速萃取装置是日本MRK公司的产品。该仪器对索氏提取器进行了改进,增加了煮沸萃取装置及程序定时器,使萃取时间大大减少,操作易于标准化。但对不同含油量的样品,说明书中没有     

回流液体柱色谱用于天然产物分析的研究

液体柱色谱是现代分离有机化合物的主要手段。但此法耗费溶剂多,溶剂在下滴过程中污染空气,回收洗出液的工作量大。索氏脂肪提取器(Soxhletextractor)用于提取某些组分,耗费溶剂少,操作方便。有人用索氏提取器分离马兜铃酸,取得较好效果。但与液体柱色谱相比,索氏提取器的分离效果很差。粗短尾析柱的广泛使用,取得了不少经验。我们对比这两种分离方法的优缺点以后,发现可以把二者结合起来。为此,设计了一种新的装置,取名为回流层析柱。它具有液体柱色谱及索氏提取器的优点。     

一种简单的抽提法

一种简单的抽提法王荣民张海涛何玉凤王云普（西北师范大学化学系兰州７３００７０）固体物质的抽提，一般是在所谓的索氏（Ｓｏｘｈｌｏｔ）抽提器中进行的。我们在实验过程中发现使用现成的磨口索氏抽提器有诸多不便：首先，索氏抽提器的成套性不好，这是因为索氏抽提器...     

一种用于从固体中提取溶质的热提取装置

一种用于从固体中提取溶质的热提取装置王杰，任仲皎，伍明（中南民族学院化学系，武汉４３００７４）在化学合成和天然产物的提取中，传统的方法一般是利用索氏或梯氏提取器来提取溶质，也可用容器直接浸提溶质￣［１］。上述方法一般均需将固体磨成微细颗粒，且提取效率...     

抽提液高度可调的索氏抽提器

对普通玻璃索氏抽提器提出了改进,改进后的抽提器能调节抽提溶剂高度,从而能够在同一个仪器中实现不同固体量的快速抽提。     

咖啡因提取的综合性实验教学

介绍了一个综合性化学实验。该实验以绿茶为原料,95%的乙醇为提取剂,通过索氏提取器提取、常压蒸馏及升华等实验操作,得到咖啡因产品。通过超高效合相色谱法（Ultra Performance Convergence Chromatography,UPC2）确定咖啡因的含量,熔点测定法及1H-NMR归属分析表征结构。本实验将经典的有机化学实验和先进的分析测试仪器相结合,提高了学生的实验综合能力,激发了学生的科研兴趣和探索精神。     

An eco-friendly efficient extractor

A microscale solid-liquid Pyrex extractor is described. The extractor has a novel detachable extraction vessel (H) containing a filter paper cylinder (C) over the reservoir. A filter paper cylinder (C) is firmly placed in the socket (E) with a plug (G) on which the cylinder has been placed. The sample is directly weighed in the extraction vessel (H) and the vessel is clamped (F) to the body (B). Contents in the extraction reservoir (H) are stirred (I) with a magnetic stirrer (J) and heated sufficiently (e.g. at 84.8 °C in using water) by the solvent vapor (D). Easy filtration (C) and continuous outflow (D) of the filtrates out of the reservoir (H) keeps a stable boiling condition (K), rather than batchwise conditions operative in a Soxhlet; this results in rapid and exhaustive extraction. The present extractor (8.0 mL extraction reservoir (H) capacity) equipped with a 25 mL solvent flask (K) was applied to fat extraction from powdered peanut by using 18 mL of ether. The extraction was complete in 30-60 min depending on reflux rate; in contrast, extraction with a commercial micro-Soxhlet device (23.9 mL extraction reservoir capacity) equipped with a 25 mL flask by using 34 mL of the solvent was incomplete in 120 min. Unlike filter paper thimbles used in Soxhlet devices, filter paper cylinder (C) in the new extractor could be reused many times and results in significant savings of the filter paper cylinders. Small reservoir and flask capacities of the new extractor minimize the use of organic solvents. The present apparatus permits fast and efficient extraction, sharply reduces waste, minimizes solvent consumption, and thus should find wide use aiming at the Green Solutions to Global Problems.     

Soxhlet extraction: Past and present panacea

An overview of Soxhlet extraction, the advantages and shortcomings of this centenary technique as well as the attempts to improve its performance and achievements reached is here presented. Assistance of high pressure, ultrasound or microwaves has decreased or minimized the negative characteristics of the conventional extractor. Automation of Soxhlet performance opened the door to commercialization of a number of different approaches. The evolution of Soxhlet extractor is here critically discussed, and the conclusion from this overview is that the adoption of new technologies to improve its performance converts Soxhlet extraction in almost a “panacea” in this field.     

A Combined Approach Employing Soxhlet Extraction and Linear Gradient Elution Reversed-Phase HPLC for the Fingerprinting of Soil Organic Matter According to Hydrophobicity

This paper reports the results of a study carried out to evaluate the potentiality of combining selective solvent extraction and linear gradient elution reversed-phase high performance liquid chromatography (RP-HPLC) for characterizing soil organic matter on the basis of polarity of its constituting organic compounds. Such approach comprises the sequential extraction of soil organic matter with organic solvents of increasing polarity in a Soxhlet extractor and the subsequent separation of each extract by RP-HPLC. Accordingly, each soil sample has been subjected to cycles of sequential extraction with n-hexane, dichloromethane, ethyl acetate, and methanol. Each sample extracted by one of the four solvents have been dried in a rotary evaporator device at 40°C and then dissolved again in the proper volume of extraction solvent to obtaining sample solutions of concentration ranging from 5.0 to 15 mg ml⁻¹. These sample solutions have been subjected to RP-HPLC separation using a Supelcosil LC-ABZ column that has been eluted by a linear acetonitrile gradient in water, having the same profile for all samples. The study has evidenced the possibility of producing highly repeatable chromatographic profiles, which are correlated to the polarity of organic solvents employed for extracting the organic matter in the Soxhlet extractor.

     

稀土富勒烯生成的影响因素初探

采用某些特殊的放电和提取方法，如反向放电和甲苯高温高压提取等可以有效地提高稀土富勒烯的生成效率［‘，‘’，并已先后成功高效地合成了许多含稀土富勒烯「‘’．对其提纯、表征、衍生和应用也进行了研究［‘－’j．但对影响稀土富勒烯生成的因素研究较少．在石墨律中同时填入La，Y，Sc的稀土氧化物，对其稀土富勒烯生成效率的情况进行了研究，认为稀土元素的第一电离能是影响稀土富勒烯生成的主要因素‘’，’‘．Moro等采用激光和热解吸质谱对稀土富勒烯的研究结果表明，稀土元素的氧化态是影响稀土富勒烯生成的决定性因素”’．本…     

Extraction of a quality assurance sediment sample for polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/F)

An experimental design for two variables at three and four levels was used to investigate the Soxhlet extraction of polychlorinated dibenzo-p-dioxins/ dibenzofurans (PCDD/F) from a quality assurance sediment. The first variable was the solvent: toluene/methanol, toluene (both Soxhlet) and toluene in Soxhlet-Dean-Stark equipment. The second variable were four different bulks: silica, sulfuric acid treated silica, sodium carbonate and no bulk. Extractions with toluene/methanol and sulfuric acid provided only a small contribution to the overall extraction efficiency. Toluene/methanol preferably improved the extraction of PCDD, and the sulfuric acid improved the PCDF extraction. This was likely to reflect improved extraction efficiency of substructures in the sediment as pulp effluent remains (fiber) and fly-ash particulate. A previously found PCDD formation in extractions using toluene/methanol in presence of sodium carbonate was reproduced. A designed supercritical fluid extraction (SFE) experiment was also accomplished, however even under the best used conditions some PCDD/F were retained on the particulate compared to Soxhlet extraction. Variations in extraction efficiency in Soxhlet and SFE indicated that different subfractions of PCDD/F are connected to the matrix with different mechanisms, thus indicating that different PCDD/F fractions had different abilities to equilibrate also in the real environment.     

Determination of the oil content of seeds by focused microwave-assisted soxhlet extraction

Sumamry Soybean, rape and sunflower lipids have been extracted with a focused microwave-assisted Saxhlet extractor. The main factors affecting extraction efficiency, namely microwave irradiation power, number of cycles and microwave irradiation time were optimised by means of a power, number of cycles and microwave irradiation time were optimised by means of a central composite design based on a two-level-three-factor factorial design. A study of the influence of particle size on the extraction procedure was also performed. The results obtained were compared with those obtained by use of an ISO method using a conventional Soxhlet extractor. Quantitative results for lipid content based on gravimetric determinations and qualitative results based on analysis of fatty acid methyl esters and polymeric compounds were similar to those obtained by Soxhlet extraction with hexane. Substantial reduction of sample manipulation. analysis time and solvent wastage is achieved by use of the proposed method.     

Extraction of a quality assurance sediment sample for polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/F)

An experimental design for two variables at three and four levels was used to investigate the Soxhlet extraction of polychlorinated dibenzo-p-dioxins/ dibenzofurans (PCDD/F) from a quality assurance sediment. The first variable was the solvent: toluene/methanol, toluene (both Soxhlet) and toluene in Soxhlet-Dean-Stark equipment. The second variable were four different bulks: silica, sulfuric acid treated silica, sodium carbonate and no bulk. Extractions with toluene/methanol and sulfuric acid provided only a small contribution to the overall extraction efficiency. Toluene/methanol preferably improved the extraction of PCDD, and the sulfuric acid improved the PCDF extraction. This was likely to reflect improved extraction efficiency of substructures in the sediment as pulp effluent remains (fiber) and fly-ash particulate. A previously found PCDD formation in extractions using toluene/methanol in presence of sodium carbonate was reproduced. A designed supercritical fluid extraction (SFE) experiment was also accomplished, however even under the best used conditions some PCDD/F were retained on the particulate compared to Soxhlet extraction. Variations in extraction efficiency in Soxhlet and SFE indicated that different subfractions of PCDD/F are connected to the matrix with different mechanisms, thus indicating that different PCDD/F fractions had different abilities to equilibrate also in the real environment. Received: 5 December 1997 / Revised: 9 February 1998 / Accepted: 15 February 1998     

Extraction of polychlorinated biphenyls from soils by automated focused microwave-assisted Soxhlet extraction

The application of a new focused microwave-assisted Soxhlet extractor for the extraction of polychlorinated biphenyls from differently aged soils is here presented. The new extractor overcomes the disadvantages of previous devices based on the same principle and enables a fully automated extraction of two samples simultaneously. The variables affecting the extraction step (namely, power of irradiation, irradiation time, extractant volume, extractant composition and number of extraction cycles) have been optimized using experimental design methodology. The optimized method has also been applied to a certified reference material (CRM910-050 "real" contaminated soil) for quality assurance validation. Quantification of the target compounds has been performed by GC with ion-trap MS. The mass spectrometer was operated in the electron-ionization mode, with selected-ion monitoring at m/z 152, 186, 292, 326 and 498. The results obtained have demonstrated that this approach is as efficient as conventional Soxhlet but with a drastic reduction of both extraction time (70 min vs. 24 h for the "real" contaminated soil) and organic solvent disposal, as 75-80% of the extractant is recycled.     

Sequential Automated Focused Microwave-Assisted Soxhlet Extraction of Compounds with Different Polarity from Marine Sediments Prior to Gas Chromatography Mass Spectrometry Detection

An extraction method based on the use of a focused microwave-assisted Soxhlet extractor with subsequent gas chromatography separation and mass spectrometry detection is proposed for the analysis of environmental pollutants from marine sediments collected at the outflow of an urban wastewater treatment plant to the sea. For the extraction of compounds with different polarity, sequential extraction with dichloromethane and water was performed on each sample. The experimental variables were optimized by the experimental design methodology for both the organic and aqueous extractant. The total time required for quantitative extraction of triclosan, bisphenol A, estrone, estradiol, oxyfluorofen and permethrin was 75 min, a short time as compared with the 24 h Soxhlet extraction (diethylstilbestrol, 4-octylphenol, procymidone and 2,7/2,8-dichlorodibenzo-p-dioxin isomer pair).Revised: 10 March and 18 April 2005     

气相色谱-质谱法测定食品接触材料表面印刷油墨中的光引发剂

建立了食品接触材料表面印刷油墨中光引发剂(PIs)二苯甲酮(BP)、4-甲基二苯甲酮(MBP)、对二甲氨基苯甲酸乙酯(EDAB)、N,N-二甲氨基苯甲酸异辛酯(EHDAB)和1-羟基环己基苯基甲酮(Irgacure 184)的气相色谱-质谱(GC-MS)分析方法。样品以乙酸乙酯为萃取溶剂进行索氏提取,萃取溶液经净化分离和富集以后,以5%苯基-95%甲基聚硅氧烷为固定相(DB-5MS),采用选择离子扫描(SIM)方式对上述5种PIs进行了定性和定量分析。5种PIs在5.0～200.0 μg/L范围内的线性关系良好(R2＞0.9995),在2种浓度的添加水平下,回收率为66.7%～89.4%,相对标准偏差＜10%。方法的定量限为0.0017～0.0036 mg/dm2。该方法的样品前处理过程简单,易操作,适用于常规进出口食品接触材料表面印刷油墨中PIs的快速检测。