固相萃取

近１０多年来,固相萃取作为试样预处理技术得到迅速的发展。评述了该技术的特点、装置、方法的建立,应用和前景。文中强调固相萃取在环境分析、药物分析等方面有广泛的应用前景,并总结了近年来固相萃取在药物分析中的应用。     

样品制备与处理的进展——无溶剂萃取技术

本文讨论了现代分析化学的重要领域之一, 样品制备及前处理技术的进展--无溶剂萃取技术。包括气相萃取、超临界流体萃取、膜萃取、固相萃取、固相微萃取等方法。简述了这些方法的原理及其应用, 探讨了样品制备与前处理技术的发展动向。     

Fabric Phase Sorptive Extraction: A Paradigm Shift Approach in Analytical and Bioanalytical Sample Preparation

Fabric phase sorptive extraction (FPSE) is an evolutionary sample preparation approach which was introduced in 2014, meeting all green analytical chemistry (GAC) requirements by implementing a natural or synthetic permeable and flexible fabric substrate to host a chemically coated sol–gel organic–inorganic hybrid sorbent in the form of an ultra-thin coating. This construction results in a versatile, fast, and sensitive micro-extraction device. The user-friendly FPSE membrane allows direct extraction of analytes with no sample modification, thus eliminating/minimizing the sample pre-treatment steps, which are not only time consuming, but are also considered the primary source of major analyte loss. Sol–gel sorbent-coated FPSE membranes possess high chemical, solvent, and thermal stability due to the strong covalent bonding between the fabric substrate and the sol–gel sorbent coating. Subsequent to the extraction on FPSE membrane, a wide range of organic solvents can be used in a small volume to exhaustively back-extract the analytes after FPSE process, leading to a high preconcentration factor. In most cases, no solvent evaporation and sample reconstitution are necessary. In addition to the extensive simplification of the sample preparation workflow, FPSE has also innovatively combined the extraction principle of two major, yet competing sample preparation techniques: solid phase extraction (SPE) with its characteristic exhaustive extraction, and solid phase microextraction (SPME) with its characteristic equilibrium driven extraction mechanism. Furthermore, FPSE has offered the most comprehensive cache of sorbent chemistry by successfully combining almost all of the sorbents traditionally used exclusively in either SPE or in SPME. FPSE is the first sample preparation technique to exploit the substrate surface chemistry that complements the overall selectivity and the extraction efficiency of the device. As such, FPSE indeed represents a paradigm shift approach in analytical/bioanalytical sample preparation. Furthermore, an FPSE membrane can be used as an SPME fiber or as an SPE disk for sample preparation, owing to its special geometric advantage. So far, FPSE has overwhelmingly attracted the interest of the separation scientist community, and many analytical scientists have been developing new methodologies by implementing this cutting-edge technique for the extraction and determination of many analytes at their trace and ultra-trace level concentrations in environmental samples as well as in food, pharmaceutical, and biological samples. FPSE offers a total sample preparation solution by providing neutral, cation exchanger, anion exchanger, mixed mode cation exchanger, mixed mode anion exchanger, zwitterionic, and mixed mode zwitterionic sorbents to deal with any analyte regardless of its polarity, ionic state, or the sample matrix where it resides. Herein we present the theoretical background, synthesis, mechanisms of extraction and desorption, the types of sorbents, and the main applications of FPSE so far according to different sample categories, and to briefly show the progress, advantages, and the main principles of the proposed technique.     

C18固相萃取圆盘与聚氨酯泡沫(PUF)萃取水体中二噁英的对比性研究

水体样品经玻璃纤维膜过滤富集颗粒物后使用C18膜或聚氨酯泡沫固相萃取水相中二噁英,冷冻干燥后索氏抽提,抽提液依次经多段混合硅胶柱、氧化铝柱净化后,采用13C同位素稀释法对其中的17个2,3,7,8-氯取代二噁英(PCDD/Fs)同系物进行测定.研究结果表明,用该法分析二噁英标准溶液、C18膜或聚氨酯泡沫各4次,分析结果的平均值和标准偏差都符合EPA1613规定值,回收率分别为74%～130%和61%～110%;标准参考样的分析结果(n=3)符合标准参考值范围.实验表明在大水量(大于100 L)样品前处理阶段使用聚氨酯泡沫替代C18膜是合理、可行的.     

Miniaturized Salting-Out Assisted Liquid-Liquid Extraction Combined with Disposable Pipette Extraction for Fast Sample Preparation of Neonicotinoid Pesticides in Bee Pollen

As the main source of nutrients for the important pollinator honeybee, bee pollen is crucial for the health of the honeybee and the agro-ecosystem. In the present study, a new sample preparation procedure has been developed for the determination of neonicotinoid pesticides in bee pollen. The neonicotinoid pesticides were extracted using miniaturized salting-out assisted liquid-liquid extraction (mini-SALLE), followed by disposable pipette extraction (DPX) for the clean-up of analytes. Effects of DPX parameters on the clean-up performance were systematically investigated, including sorbent types (PSA, C18, and silica gel), mass of sorbent, loading modes, and elution conditions. In addition, the clean-up effect of classical dispersive solid-phase extraction (d-SPE) was compared with that of the DPX method. Results indicated that PSA-based DPX showed excellent clean-up ability for the high performance liquid chromatography (HPLC) analysis of neonicotinoid pesticides in bee pollen. The proposed DPX method was fully validated and demonstrated to provide the advantage of simple and rapid clean-up with low consumption of solvent. This is the first report of DPX method applied in bee pollen matrix, and would be valuable for the development of a fast sample preparation method for this challenging and important matrix.     

在线离子对固相萃取预富集系统分析水样中的烷基苯磺酸盐

采用在线离子对固相萃取法富集测定生活废水中阴离子表面活性剂十二烷基苯磺酸钠。电动分析系统由1个电渗泵和5个电磁切换阀组成,计算机控制泵运作和阀切换。在萃取柱和检测器之闯用改进的气液分离器除去洗脱液中气泡。实验对离子对试剂和固相萃取条件进行了优化。结果表明,在样品溶液中加入0．5mmol／L四丁基溴化铵、采样体积15mL、用0．80mL／min萃取保留,2．0mL／min吸入80％乙腈洗脱液15s,再以1．65mL／min洗脱时,结果最佳。方法检出限为10彬L,线性范围0．030—1．00mg／L,富集倍数65,相对标准偏差3．7％,回收率90．6％-98．0％。     

固相萃取分离铀

铀是重要的核工业原料,也是一种有较强化学和生物毒性的重金属。从各类含铀水体系中分离和回收铀对缓解铀资源短缺,保护人类健康和生态环境安全都具有重要的科学和实际意义。本文简要回顾和评述了近15年来具有代表性的新型固相萃取材料及其在铀分离方面的应用研究,并对相关材料在铀分离领域的应用前景进行了分析和展望。     

固相萃取-气相色谱法测定动物组织中盐酸克伦特罗残留量

建立了固相萃取-气相色谱分析动物组织中盐酸克伦特罗残留量的方法．采用固相萃取,分离富集动物组织中的盐酸克伦特罗．肉样的加标回收率在70％～80％;最低检出限为1μg／kg．盐酸克伦特罗的硅烷化衍生产物,采用气相色谱(ECD检测器)检测,其衍生物的峰面积与样品浓度在0．005～1．0μg／mL范围内呈良好的线性关系,线性回归系数大于0．999．     

固相萃取新技术研究

固相萃取技术是一种用于样品分离、纯化、浓缩的重要的样品前处理手段。近年来,高分子材料合成技术、分子印迹技术等新技术与传统固相萃取技术相结合,衍生出众多技术改进和创新。主要对各种固相萃取新技术进行评述。     

限进介质固相萃取及其应用

系统地介绍了限进介质固相萃取的原理、特点、发展现状及其发展趋势,并对该技术在生物和环境样品前处理中的应用作了较详细的综述。引用文献58篇。     

Microfluidic Chip-Based Induced Phase Separation Extraction as a Fast and Efficient Miniaturized Sample Preparation Method

Induced phase separation extraction (IPSE) is an efficient sample clean-up technique that can replace liquid-liquid extraction (LLE). The purpose of this study was to miniaturize IPSE by carrying it out in a microfluidic chip. An IPSE chip was designed and evaluated for its ability to separate and purify samples on a microscale. The 5 × 2 cm chip was fed with a solution of polar to non-polar model compounds in acetonitrile-water (1:1). In the 100 µm wide and 40 µm deep microchannels, the sample solution was efficiently separated into two immiscible phases by adding a hydrophobic solvent as inducer. Analytes present in the sample solution each migrated to their own favorable phase upon phase separation. After optimization, extraction and fractionation were easily and efficiently achieved. The behavior of analytes with a pH-dependent partitioning could be influenced by adjusting the pH of the sample solution. Scutellaria baicalensis extract, used in Traditional Chinese Medicine (TCM), was successfully separated in aglycones and glycosides. In this microscale system, the sample and solvent consumption is reduced to microliters, while the time needed for the sample pretreatment is less than one minute. Additionally, the extraction efficiency can reach up to 98.8%, and emulsion formation is avoided.     

固相萃取技术及固定相络合法富集环境水样中微量金属离子的思路

固相萃取（Solid Phase Extraction SPE）是一种处于迅速发展中的样品前处理新技术,SPE技术在液体试样制备中以突出的优点已成为优先考虑的方法。本文旨在介绍SPE技术,并从配合物基本理论出发,首次提出“固定相络合法”富集环境水样中微量金属离子的思路。     

固相萃取材料在食品真菌毒素检测中的研究进展

被真菌毒素污染的食品可引发严重的健康问题,如癌症和畸形等,已成为全球公共卫生关注的焦点.因此,精准检测食品中痕量真菌毒素对保障人类健康具有重要意义.真菌毒素在食品中的浓度水平较低且易与复杂的食品基质成分结合,基质干扰严重影响检测的灵敏度,需采用有效的样品前处理技术进行富集和净化.固相萃取作为一种高效的样品前处理技术,其...     

微波辅助萃取/样品前处理联用技术的研究进展

微波辅助萃取是近年来新发展的一种样品前处理技术,随着微波辅助萃取的发展和成熟,它与其它样品前处理技术的联用得到了迅速发展。与传统前处理方法相比,这些联用方法具有快速、高效、操作简便、节省溶剂、选择性好、应用范围广的特点。该文综述了微波辅助萃取及其与其它样品前处理技术联用的特点及适用性,并对近年来微波辅助萃取与其它前处理方法联用的发展概况及在分析领域中的应用情况进行了详细总结。     

固相萃取-气相色谱-质谱分析肉样中盐酸克伦特罗的残留量

建立了固相萃取 气相色谱 质谱联机分析肉样中盐酸克伦特罗残留量的方法。对盐酸克伦特罗在C1 8和离子交换固相萃取柱上的保留行为进行了研究 ,发现不同浓度盐酸克伦特罗的固相萃取回收率在 75 %～ 95 %之间 ;肉样中的加标回收率在 70 %～ 83 % ;相对标准偏差在 4 .95 %～ 1 3 .4 % ;最低检出限为 1 μg kg。盐酸克伦特罗的硅烷化产物 ,采用选择离子的模式进行检测 ( 86、2 4 3、2 62、2 77) ,衍生物的峰面积与样品浓度在0 .0 0 2 5 2～ 2 .0 2mg L范围内呈良好的线性关系 ,线性回归系数大于 0 .9999。     

固相萃取真空装置的设计与应用

目前常用的样品预处理方法——固相萃取（ＳＰＥ）,具有高效、快速、方便和高选择性等特点。国家色谱研究分析中心新近开发成功的ＳＰＥ真空装置是ＳＰＥ方法的重要组成部分,能同时处理１２个样品,利用其独特的转动上盖,可方便地在ＳＰＥ各步骤间任意切换,以收取所需要的组分。给出了利用ＳＰＥ真空装置并结合高效液相色谱法（ＨＰＬＣ）分离人血清中胆汁酸的应用实例。     

溶胶凝胶法制备固相微萃取搅拌棒

采用溶胶凝胶法制备了一种新型PDMS固定相，键合于固相微萃取搅拌棒玻璃表面作为固相萃取固定相。PDMS的一部分以键合的方式与凝胶网络结合，而另外一部分则是被凝胶网络所包埋。由于萃取固定相涂层的厚度在30μm以上，采用多阶程序升温方式对固定相进行老化避免涂层龟裂，制备的萃取固定相耐温达到300℃。     

罗丹明B分子印迹固相萃取小柱的研制及应用

研制一种对罗丹明B具有特异性识别性能的分子印迹固相萃取小柱。用沉淀聚合法制备罗丹明B分子印迹聚合物,通过静态平衡吸附实验及固相萃取实验表征其性能,并对市售辣椒样品中的罗丹明B进行测量。罗丹明B模板聚合物的吸附能力明显优于空白聚合物;印迹固相萃取小柱对罗丹明B标准溶液(0.05 mmol/L)一次性萃取率为98.24%,实际样品测量的回收率为90.0%~95.0%,测定结果的相对标准偏差为0.9%~1.7%(n=3)。罗丹明B分子印迹固相萃取小柱选择性好、萃取率高,可应用于食品、化妆品检测等相关领域。     

葡萄糖苷特异性固相萃取固定相的合成、表征及应用

以马来酰亚胺基修饰凝胶载体,通过β-葡萄糖胺和2-亚氨基硫代烷盐酸盐将作为配基的β-葡萄糖脒连接到载体上,合成了一种葡萄糖苷特异性固相萃取固定相,并对其固相萃取性能进行了表征.该固定相对葡萄糖苷具有特异性识别,并成功用于固相萃取分离葡萄糖苷.     

基质固相分散法与固相萃取法在检测水产品中己烯雌酚残留中的应用

分别建立了基质固相分散（MSPD）法、固相萃取（SPE）法与气相色谱/质谱联用（GC-MS）测定水产品中己烯雌酚（DES）残留量的分析方法,并对MSPD与SPE 2种样品前处理方法的效果进行了比较。MSPD法中样品以弗罗里硅土（Florisil）作为固相分散剂,经乙酸乙酯提取,再用Florisil净化;SPE法中样品经乙酸乙酯超声提取,过Florisil小柱进行净化,最后经GC-MS在选择离子监测模式下测定水产品中DES。在优化的色谱条件下,方法的线性范围为1-300 μg/L,相关系数为0.9985。M