一种新的绿色化学技术:超临界萃取作为样品制备技术在痕量药检分析中的应用

综述了超临界萃取作为样品制备技术在痕量药检分析中的应用.研究了生物基质对有效萃取目标检测物的影响及提高萃取率的途径.并重点评述了减少类脂杂质、选择性的分离目标检测物的非在线吸附剂收集与在线吸附剂收集技术.从而展示了SFE作为绿色化学技术具有萃取率高、使用溶剂少,分离步骤少,环境无害等明显优于传统方法的特点.     

分子印迹固相萃取技术在食品安全检测中的应用进展

分子印迹固相萃取技术(MISPE)是一种高效的样品前处理技术,能从复杂的样品中选择性分离目标物及其结构类似物。分子印迹技术(MIT)在食品中农药和兽药残留检测中的应用得到快速发展。综述了近两年国内外分子印迹固相萃取技术在食品安全检测中农药、兽药残留检测的应用及进展,讨论了当前分子印迹固相萃取技术在食品安全检测应用中存在的问题,并对其发展趋势进行了展望。     

超临界CO2流体萃取中的在线检测技术

综述了超临界CO2流体萃取中的在线检测技术,介绍了超临界CO2流体萃取与超临界流体色谱、气相色谱、高效液相色谱、核磁共振、近红外光谱等技术的联用在线检测,阐述了在线检测技术的优越性,提出了如何发展超临界CO2流体萃取中的在线检测技术。     

分离技术的进展

本文概述了基于生物技术的发展、超纯材料的制备等对发展分离科学和技术的需求,特别是从大量基体物或稀溶液中提取、分离、纯化和检测低含量物质要求发展高选择性的分离技术和相应的分离体系。在发展和完善原有分离技术(如萃取、离子交换、吸附、吸收等)的同时,超临界萃取和膜分离技术具有引入的应用前景。还应注意两种或多种分离技术相结合的分离方法和技术的研究。     

分散液液微萃取技术萃取剂的改进研究

分散液液微萃取技术是建立在三相溶剂体系基础之上的萃取技术,是一种简单、易操作、环境友好、富集倍数高的分离富集技术。该方法大大增加了有机萃取相和水相之间的接触面积,加快了目标分析物在有机相和水相间的萃取平衡。对该技术中的萃取剂进行针对性的改进,使得目标化合物迅速萃入到萃取剂微滴内,可进一步提高该技术的萃取效率及富集倍数。     

双水相萃取技术研究进展及应用

双水相萃取技术作为一种新型的分离技术日益受到重视，它与传统的萃取方法相比有独特的优点。总结了双水相萃取形成的原理，萃取过程的基本理论、萃取体系的特点以及热力学模型的发展，综述了双水相萃取技术在生化工业、分析检测、稀有金属分离等方面的应用，介绍了该技术的最新进展，指出了该技术工业存在的问题并对今后的发展作了展望。     

替代生物样品的绿色样品制备技术在法医毒物学中的研究应用

法医毒物学是研究死亡案件、药物检测、运动兴奋剂等的重要学科，主要是结合现代仪器分析技术，对体内外未知毒物如安非他命、苯二氮卓类、大麻和阿片类等进行定性、定量分析。替代生物样品如头发、指甲、唾液、汗液、脑脊液等是法医毒物分析主要对象，与常规血液和尿液样品相比，它们具有易于收集、相对稳定和不易变质等优点。在样品制备过程中，为了达到消除基质干扰并进行预富集的目的，目标分析物与分析仪器应相互兼容。测定法医毒物目标分析物的常用仪器有气相色谱仪和液相色谱仪结合质量检测器。目前被广泛应用的是固相萃取技术和液-液萃取技术。此外，随着绿色分析化学的发展，至今已开发了大量的微萃取和微型萃取技术。简要综述了法医毒物学中替代生物样品的绿色样品制备技术的研究应用。     

基于分子印迹固相萃取填料的合成及其在微流控芯片中的应用

分子印迹技术,是基于模拟酶-底物或抗体-抗原之间的相互作用,对印迹分子(也称模板分子)进行专一识别的技术,因其能够对目标分子具有特异性的识别能力,目前被广泛用于生物传感和样品分离。本工作基于离子液体印迹聚合物,作为固相萃取技术填料,并联用微流控芯片毛细管电泳技术,实现对目标物的选择性分离检测。     

萃取精馏技术及其在分离过程中的应用

对萃取精馏技术及其在分离过程中的研究与应用进行了讨论。从萃取精馏的基本原理与操作类型、溶剂的物理特性与筛选方法等方面进行了介绍,同时列举了萃取精馏技术在一些物系分离中的应用。最后指出了萃取精馏技术的研究方向。     

医药化工中溶剂萃取技术进展

本文讨论了医药化工中８０年代以来特别是近１０年来溶剂萑取技术的研究进展，包括化学反应萃取、液膜技术、在线萃取中化反应过程，异构体的分离和预分散萃取等新工艺的发展趋向和应用前景。     

Use of crosslinked poly(ferric acrylate) as a sorbent in solid‐phase extraction

A sample‐preparation step, before chromatographic analysis, is frequently performed to enrich the components of interest from a complex matrix. This step is also needed to purify and concentrate the analyte present in a highly dilute medium. Solid‐phase extraction (SPE) with a specific sorbent is one of the most widely used techniques for extracting trace components from aqueous or nonaqueous media. In this method, analytes are extracted by the passage of the medium through a cartridge containing a solid matrix. The recovery of the analytes from the medium considerably depends on the extent of the interactions between the analytes and the sorbent. Through the enhancement of these interactions, the extent of the uptake of the analytes can be improved. Poly(acrylic acid) is commonly employed as the sorbent in SPE for the isolation of polar analytes. This article discusses the use of the metal‐containing polymer poly(ferric acrylate) as the sorbent for the isolation of a few phenols as representative components from water. The results indicate that the metal‐containing polymer has an enhanced adsorption capacity in comparison with the capacity of the widely used sorbent poly(acrylic acid). © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 2184–2187, 2002     

Microwave-Assisted Extraction and Solid-Phase Separation of Quercetin from Solid Onion (Allium cepa L.)

The challenge of extraction of natural product in the twenty-first century is to achieve 100% selectivity of the desired product and develop renewable energy based processes. An object of the present work is to provide a method for producing specific bioactive compounds from agricultural products. A simple protocol was used to obtain the conditions of microwave-assisted extraction (MWAE) and ultrasound-assisted extraction (USAE). Total quercetin content under microwave irradiation for 150 sec at pH 6.25 (209 mg/ 100 gm F. wt). The effects of operating conditions, such as extraction time and pH on the extraction yield of quercetin were studied. Microwave-assisted ionic liquid-based silica sorbent (ILSis) was developed by a process involving surface chemical modification of commercial silica using a synthesized ionic liquid and characterized by FTIR. The obtained particles were successfully used as a special sorbent in a solid-phase separation process to isolate quercetin and its glycosides from solid onion. Different washing and elution solvents, such as water, water/methanol (v/v), and pure methanol were evaluated. Ionic liquid-based silica sorbent was compared with traditional C18 sorbent and it exhibited higher selectivity. The target compounds in solid onion containing quercetin and its glycosides were determined.     

萃取剂对GC-MS法测定天麻茎秆化学组分的影响

采用常见极性溶剂和非极性溶剂作为萃取试剂,在超声波辅助下,对干燥天麻茎秆粉末进行萃取,然后分别用GC-MS法对极性溶剂和非极性溶剂的提取浓缩液进行化学成分分析,比较其中化学组分的差别。结果表明:甲醇作萃取溶剂时,38种化学组分可被鉴别确认;四氯化碳作萃取溶剂时,43种化学组分可别鉴别确认,其中有24种化合物在甲醇提取浸膏中同样被检出,且可识别的化学组分中烷烃等极性较小的化合物明显增多。此结果有助于天麻茎秆化学组分的研究,可以根据所需分析目标的不同选用合适的提取溶剂。     

Investigating the Potential Use of Chemical Biopsy Devices to Characterize Brain Tumor Lipidomes

The development of a fast and accurate intraoperative method that enables the differentiation and stratification of cancerous lesions is still a challenging problem in laboratory medicine. Therefore, it is important to find and optimize a simple and effective analytical method of enabling the selection of distinctive metabolites. This study aims to assess the usefulness of solid-phase microextraction (SPME) probes as a sampling method for the lipidomic analysis of brain tumors. To this end, SPME was applied to sample brain tumors immediately after excision, followed by lipidomic analysis via liquid chromatography-high resolution mass spectrometry (LC-HRMS). The results showed that long fibers were a good option for extracting analytes from an entire lesion to obtain an average lipidomic profile. Moreover, significant differences between tumors of different histological origin were observed. In-depth investigation of the glioma samples revealed that malignancy grade and isocitrate dehydrogenase (IDH) mutation status impact the lipidomic composition of the tumor, whereas 1p/19q co-deletion did not appear to alter the lipid profile. This first on-site lipidomic analysis of intact tumors proved that chemical biopsy with SPME is a promising tool for the simple and fast extraction of lipid markers in neurooncology.     

苯基键合硅胶萃取黄酮化合物的性能研究

以苯基三氯硅烷和硅胶为原料制得苯基键合硅胶固相萃取材料,采用扫描电镜、元素分析、比表面积/孔径分析、红外光谱等对其进行了结构表征。装填固相萃取小柱,以4个黄酮模型化合物为目标分析物,研究苯基键合硅胶的萃取性能。对上样体积、上样速度、上样pH、洗脱剂类型、洗脱体积、洗脱速度等萃取参数进行了优化,并建立了苯基键合硅胶富集萃取黄酮化合物的高效液相色谱分析检测方法。实验证实该方法具有宽的线性范围(1~200μg/L)、低的检出限(0.25μg/L),并成功应用于2种实际样品中黄酮化合物的富集检测。上述结果说明苯基键合硅胶是一种对黄酮化合物具有良好萃取性能的固相萃取材料。     

燃煤电厂吸附剂喷射脱汞技术的研究进展

燃煤汞污染已引起广泛关注。燃煤电厂控制汞排放最成熟可行的技术是烟道活性炭喷射技术,但该技术在我国燃煤电厂的广泛应用还存在较多的科学问题,因为活性炭对烟气汞的脱除是包含吸附、扩散、传质及化学反应在内的多元化过程,因此,针对燃煤电厂吸附剂喷射脱汞技术的研究已成为当前的热点课题。本文从吸附剂喷射脱汞技术原理、脱汞吸附剂的评价方法、汞吸附机理研究以及吸附剂喷射脱汞数学模型方面评述了燃煤电厂吸附剂喷射脱汞技术近些年取得的研究进展,并在此基础上提出了开发廉价高效、可再生的脱汞吸附剂,全面深入研究吸附剂的脱汞机理以及开发简单、精确的吸附剂喷射脱汞数学模型等后续研究方向,可为我国燃煤电厂吸附剂喷射脱汞技术的开发提供一定指导。     

CO2捕集的研究现状及钙基吸收剂的应用

温室气体CO2是当今世界环境恶化的主要原因之一,近年来针对CO2的捕集技术也相继被研究.磷石膏是湿法冶炼磷酸的副产物,具有产量大、微辐射性等特点,严重危害自然环境和人类健康.本文阐述二氧化碳捕集与封存(CCS)以及燃烧后捕集的三大方法的具体技术原理与特点,着重分析利用钙基吸收剂捕集CO2的技术特点和优势,提出CO2捕集技术的探索方向并指出利用磷石膏分解渣作钙基吸收剂矿化捕集CO2的思路.当前对CO2捕集的研究多停留在吸收剂捕集方面,单纯吸收剂虽吸收效果较好,但其成本较高.磷石膏分解渣作钙基吸收剂不仅有着良好的捕集效果,且解决了成本问题,实现了"以废制废"的思路.     

Graphene oxide modified expanded perlite as a new sorbent for Cu(II) and Pb(II) prior to determination by high-resolution continuum source flame atomic absorption spectrometry

Graphene oxide (GO) modified expanded perlite (EP) was prepared as a new sorbent for solid phase extraction of Cu(II) and Pb(II) prior to determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS-FAAS). Characterization of the synthesized sorbent was proved by Fourier transform infrared spectroscopy (FT-IR); X-ray diffraction (XRD); Brunaer, Emmet, and Teller (BET); specific surface area; and scanning electron microscopy (SEM) techniques. Several parameters such as pH, eluent type and concentration, flow rate, sample volume, interfering ions, adsorption capacity of sorbent were investigated and optimized. The proposed method was successfully applied for spiked analysis of Cu(II) and Pb(II) ions in tap water and fruity sodas sample, and fine recoveries (relative error <10%) were obtained.     

MSPD-GC法测定苹果和蔬菜中腐霉利农药残留

建立了基质固相分散萃取-气相色谱法(MSPD-GC)测定农产品中腐霉利农药残留的方法。研究了萃取及色谱条件对测定结果的影响,确定了最佳萃取条件:以弗罗里硅土作分散剂,样品与佛罗里硅土的比例为1∶4,以8 mL正己烷+丙酮(1∶1)作为洗脱剂。结果表明,该方法的相对标准偏差(RSD)为5.2%～6.8%;最低检出限为0.05μg/g;加标回收率为87.3%～104.3%。该法简单、准确、灵敏、重现性好,能满足农产品中腐霉利残留的分析测定要求。