首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到19条相似文献,搜索用时 125 毫秒
1.
<正>固相萃取(solid phase extraction,SPF)是一种试样预处理技术,由液固萃取和柱液相色谱技术相结合发展而来,具有高效性、高选择性、高自动化程度和低耗性等优点。目前SPE技术有SPE柱、SPE盘和固相微量萃取等形式,其中使用最普遍是SPE柱。SPE柱是一种填充好固定相的短色谱柱,利用组分与吸附剂间选择性吸附与选择性洗脱的过程,达到提取分离、净化和富集的目的[1]。复方甘草口服液由甘草流浸膏、复方樟脑酊、甘油、愈创  相似文献   

2.
分子印记聚合物技术在固相萃取中的应用及影响因素   总被引:3,自引:0,他引:3  
分子印记聚合物(MIP)技术是一种具有预定选择性的新型技术,固相萃取技术(SPE)是样品分离的一种有力手段。两种技术的结合成为纯化、富集和分析样品中的待测物质的有力手段。本文讨论了MIP和SPE的原理、应用、发展及影响因素。  相似文献   

3.
郑蕊  刘铁钢 《中国药房》2007,18(10):786-788
固相萃取(Solid-phase extraction,SPE)是近20年来迅速发展起来的一种生物样本预处理技术,是以液相色谱分离机制为基础建立的分离纯化方法。由于生物样品干扰成分较多且其中药物浓度多数较低,应用高效液相色谱(HPLC)和液相色谱/质谱联用(LC/MS)法往往无法实现样品的直接测定分析。SPE与HPLC或LC/MS法联用实现了样品预处理和分离分析的优化组合,在生物样本分析方面具有广泛的适应性和优越性。核苷类逆转录酶抑制剂(NRTIs)属核苷类似物,极性较强,故此联用技术在其生物样本分析测定方面应用普遍。为此,本文介绍了近年SPE与HPLC或…  相似文献   

4.
张晓明 《辽宁医药》2004,19(3):39-41
本文综述了近几年来生物样品预处理技术的进展,包括超临界流体革取技术(SFE)。固相微革取技术(SPME),以及采用限制性介质(RAM)、微粒填粒薄膜(PLM)、分子印记固定相(MIP)填料的固相革取技术(SPE),水浴法预处理血样技术,以及这些技术的一些应用。为体内药物分析研究提供参考。  相似文献   

5.
目的采用硅胶表面分子印迹技术,制备印迹红霉素分子的聚合物材料,将其作为固相萃取介质,对自来水中添加的红霉素(erythromycin,EM)进行了富集纯化处理。方法制备中采用γ-氨丙基三甲氧基硅烷(3-aminopropyltrimethoxysilane,AMPS)作为硅胶(SiO2)改性剂,将功能单体甲基丙烯酸(methacrylic acid,MAA)接枝到AMPS-SiO2表面,形成聚甲基丙烯酸接枝硅胶(polymer methacrylic acid/SiO2,PMAA/SiO2)。最后,加入模板分子红霉素和交联剂乙二醇二甲基丙烯酸酯(2-ethanediol dimethacrylate,EDMA),聚合得到表面包被有红霉素印迹聚合物的硅胶材料(EMMIP-PMAA/SiO2)。通过电镜扫描(scanning electron microscope,SEM)和粒径测定对EM-MIPPMAA/SiO2物理性状进行了表征;通过动、静态吸附和选择性吸附试验研究了PMAA/SiO2和EMMIP-PMAA/SiO2对红霉素的结合性能和分子识别特性。结果 EM-MIP-PMAA/SiO2对红霉素显示了良好的吸附能力,最大吸附量可达104 mg·g-1,吸附约240 min达到吸附平衡;与竞争分子罗红霉素相比,表面印迹聚合物对模板分子红霉素显示了高的选择吸附能力;将其作为固相萃取介质对于生物样品中的分析物具有良好的纯化作用。结论像MIP-PMAA/SiO2这类新的印迹材料将会广泛应用于生物样品的监测分析工作,并且对于环境保护也具有一定实用意义和价值。  相似文献   

6.
固相萃取技术是一种在20世纪70年代初发展起来的样品预处理分离富集技术,具有操作简单、省时,易实现自动化等优点,广泛应用在制药、食品、环境、商检、化工等领域.固相萃取技术与高效液相色谱(HPLC)或液相色谱(LC)、质谱(MS)法等分离检测手段联用,从而实现样品在线预处理,使其在组合化学、高通量筛选等药学领域的应用日益增多.简要介绍了固相萃取技术在化学药、中药及天然药物、生物药中的应用.  相似文献   

7.
分子印记技术是制备具有预定选择性分离介质的有效途径,其应用于毛细管电色谱(CEC)手性分离具高效及独特功用。综述分子印记技术的基本原理及其在CEC中的应用模式和实例。  相似文献   

8.
固相萃取在生物样品分析中的应用   总被引:1,自引:0,他引:1  
生物样品中的药物浓度与药物的疗效有很大的相关性,尤其是血浆(或血清)药物浓度直接与药效相关。尿液中常常含有丰富的药物代谢产物,也被经常使用。唾液由于采集方便且有时和血浆游离药物浓度具有相关性而有时使用。其他脏器组织,除特别需要,较少用。生物样品的药物分析因其复杂多样性而对样品的预处理技术提出了较高的要求。在各种处理方法中,固相萃取由于其适用性广,实用性强而越来越受到广大科研工作者的重视。本文综述了固相萃取技术(SPE)及其在生物样品分析中应用的相关报道,以期对相关研究者提供理论指导和技术支持。  相似文献   

9.
生物样品预处理技术及应用进展   总被引:2,自引:0,他引:2  
张颖 《天津药学》2006,18(1):56-58
分析生物样品中的药物,因其复杂多样性而对样品的预处理技术提出了更高的要求。本文综述了相关文献报道的几种较新型生物样品预处理技术:固相萃取技术、超临界流体萃取技术、固相微萃取技术及其在生物样品分析中的应用。  相似文献   

10.
黄美霞  胡娟 《海峡药学》2008,20(5):18-20
目的利用分子印迹技术,合成阿司匹林分子印迹聚合物,并探讨以此为固定相的液相色谱柱行为,为研究中草药中阿司匹林及其结构类似物的直接提取奠定理论和实验基础,以供进一步开发和应用。方法以阿司匹林为模板分子,丙烯酰胺(AM)为功能单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂,封管聚合法制备阿司匹林分子印迹聚合物。通过高效液相色谱方法研究MIP对阿司匹林的识别机理。结果与同样化学组成的非模板聚合物相比,阿司匹林分子模板聚合物对阿司匹林有较大的吸附性能。结论封管聚合法制备所得的阿司匹林分子模板聚合物对阿司匹林具有较大的选择性作用,这种选择性取决于模板聚合物的立体孔穴中的功能基团与模板分子功能基之间的作用,以及孔穴的立体选择性,显示了分子印迹效果。  相似文献   

11.
Yu JC  Lai EP 《Toxins》2010,2(6):1536-1553
Molecularly imprinted polymers (MIPs) are considered as polymeric materials that mimic the functionality of antibodies. MIPs have been utilized for a wide variety of applications in chromatography, solid phase extraction, immunoassays, and sensor recognition. In this article, recent advances of MIPs for the extraction and analysis of ochratoxins are discussed. Selection of functional monomers to bind ochratoxin A (OTA) with high affinities, optimization of extraction procedures, and limitations of MIPs are compared from different reports. The most relevant examples in the literature are described to clearly show how useful these materials are. Strategies on MIP preparation and schemes of analytical methods are also reviewed in order to suggest the next step that would make better use of MIPs in the field of ochratoxin research. The review ends by outlining the remaining issues and impediments.  相似文献   

12.
Synthetic cathinones are a type of drug belonging to group of new psychoactive substances (NPSs). The illicit market for these substances is characterized by the continuous introduction to the market of new analogs to evade legislation and to avoid detection. New screening and confirmation assays are therefore needed, mainly in forensic/clinical samples. In the current development, a porous membrane‐protected, micro‐solid‐phase extraction (μ‐SPE) has been developed for the assessment of several cathinones in urine. The μ‐SPE device consisted of a cone‐shaped polypropylene (PP) porous membrane containing the adsorbent (molecularly imprinted polymers, MIPs, synthesized for the first time for this class of drugs). MIPs were prepared using ethylone and 3‐methylmethcathinone (3‐MMC) as templates, ethylene glycol dimethacrylate (EGDMA) as a functional monomer, divinylbenzene (DVB) as a cross‐linker, and 2,2´‐azobisisobutyronitrile (AIBN) as an initiator. The prepared ethylone‐based MIP and 3‐MMC‐based MIP have been fully characterized and evaluated as new selective adsorbents for μ‐SPE. Cathinones separation/determination was performed by high performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS). Optimum loading conditions (pH 5.0, loading for 4.0 minutes under orbital‐horizontal shaking at 200 rpm) and elution conditions [2.0 mL of 75:20:5 heptane/2‐propanol/ammonium hydroxide and ultrasounds assistance (37 kHz, 325 W) for 4.0 minutes] were found for ethylone‐based MIP. Validation (intra‐day and inter‐day precision and analytical recovery) showed RSD values lower than 9 and 10% for intra‐day and inter‐day precision, and within the 88%–101% range for intra‐day and inter‐day analytical recovery.  相似文献   

13.
几种固相萃取新技术近十年的研究进展(英文)   总被引:1,自引:0,他引:1       下载免费PDF全文
固相萃取技术是近年来发展较快并得到广泛应用的一种样品前处理方法 (分离、纯化、富集), 具有节省时间、溶剂消耗少, 富集倍数高, 准确度高等优点。随着科学技术的不断发展及研究的不断深入, 多种优于传统固相萃取技术的新型固相萃取新技术如分子印迹固相萃取、磁性固相萃取、固相微萃取等不断出现并广泛应用到食品、药品、生物及环境监测等领域。本文对几种固相萃取新技术的基本原理、方法及近十年来在不同研究领域的研究应用进行综述。  相似文献   

14.
Stir bar sorptive extraction is a technique used for extracting target substances from various aqueous matrixes such as environmental water, food, and biological samples. This type of extraction is carried out by rotating a coated stir bar is rotated in the sample solution. In particular, Twister bar is a commercial stir bar that is coated with polydimethylsiloxane (PDMS) and used to perform sorptive extraction. In this study, we developed a method for simultaneous detection of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, and a Δ(9)-tetrahydrocannabiniol (THC) metabolite in human urine. For extracting the target analytes, the Twister bar was simply stirred in the sample in the presence of a derivatizing agent. Using this technique, phenethylamines and the acidic THC metabolite can be simultaneously extracted from human urine. This method also enables the extraction of trace amounts of these substances with good reproducibility and high selectivity. The proposed method offers many advantages over other extraction-based approaches and is therefore well suited for screening psychoactive substances in urine specimens.  相似文献   

15.
Bioanalysis is a relevant area of analytical chemistry for clinical studies. Biological samples are complex and diverse, so sample preparation represents a challenge when chromatographic methods are developed. According to the principles of green analytical chemistry (GAC), recent trends in sample preparation include miniaturization, automation (online coupling to the analytical instrument), and high-throughput performance. In this context, column switching liquid chromatography stands out as a multidimensional chromatographic method in which an extraction column is directly coupled to high-performance liquid chromatography (HPLC) systems. This online method consists of two steps and involves two columns, the extraction and the chromatographic columns. In the former column, the analytes are isolated from the sample and preconcentrated; in the latter column, the analytes are separated. Online systems improve the sensitivity and accuracy of analytical methods, consume lower amounts of organic solvents, and minimize sample handling. This review summarizes state-of-the-art column switching liquid chromatography and focuses on selective stationary phases for preconcentration of analytes (first dimension), including reversed phases, monolithic phases, restricted access materials (RAMs), and molecularly imprinted polymers (MIP). Principles, instrumental aspects, applications in bioanalysis, and future trends in column switching liquid chromatography are also discussed.  相似文献   

16.
Stir bar sorptive extraction (SBSE) is sample preparation technique that involves the extraction and enrichment of organic compounds from a liquid sample. The technique is based on the principle of sorptive extraction. A large amount of extraction phase is coated on a stir bar. An analyte is extracted into the extraction phase, based on its octanol-water partitioning coefficient and the phase ratio. Recently, various methods involving SBSE were developed in order to further facilitate analysis and improve sensitivity. In this review, we focused on the novel methods that involve SBSE with in situ derivatization, SBSE with in situ de-conjugation, thermal desorption (TD) in the multi-shot mode and TD with in tube derivatization method. Those methods were applied successfully to the trace analysis of environmental and biological samples and extremely low detection limits were achieved.  相似文献   

17.
目的:建立了分子印迹固相萃取-高效液相色谱法检测食品中2种三唑类杀菌剂残留的方法。方法:分别以三唑醇、烯唑醇为模板分子,α-甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,采用本体聚合法合成分子印迹聚合物。将制得的三唑醇、烯唑醇聚合物按质量比1:1混合,制成固相萃取柱用于样品的前处理,并采用高效液相色谱法检测。结果:在低和高浓度添加水平下,平均回收率在78.7%~94.3%之间,RSD在1.8%~2.4%之间(n=5)。结论:该方法灵敏度高,精密度好,适合于同时检测食品中三唑醇和烯唑醇2种三唑类杀菌剂残留。  相似文献   

18.
Non-covalent molecularly imprinted polymers (MIPs) of cholesterol were prepared by UV initiated polymerization. A polymer that had the highest binding selectivity and capability was used as solid-phase extraction (SPE) sorbents for direct extraction of cholesterol from different biological samples (human serum, cow milk, yolk, shrimp, pork and beef). The extraction conditions of molecularly imprinted SPE (MISPE) were optimized and the optimum protocol was: conditioning MISPE cartridges with n-hexane, loading with n-hexane, washing with n-hexane and n-hexane:toluene = 9:1, respectively, then eluting with chloroform:ethanol:acetic acid = 3:1:1. Cholesterol MISPE selectively recognized, effectively trapped and pre-concentrated cholesterol over a concentration range of 10–80 μg/mL. Recoveries ranged from 80.6% to 92.7%, with R.S.D. lower than 9.8%. Under the optimal condition, MISPE recoveries of spiked human serum, yolk, cow milk, shrimp, pork and beef were 91.1%, 80.4%, 86.6%, 78.2%, 81.4% and 80.1%, respectively. Compared with C18 SPE, almost all of the matrix interferences were removed after MISPE, and better baselines and higher selectivity were achieved.  相似文献   

19.
Detection of the cyanobacterial hepatotoxins microcystins   总被引:7,自引:0,他引:7  
Concern regarding the presence of microcystins in drinking water and their possible contamination in food (e.g., salad vegetables, fish, shellfish) has resulted in the need for reliable methods for the detection and accurate quantification of this class of toxins. Currently, routine analysis of microcystins is most commonly carried out using high-performance liquid chromatography with photodiode array detection (HPLC-PDA), although more sensitive biological assays such as antibody-based ELISAs and protein phosphatase inhibition assays have also proven useful. However, many of these methods have been hindered by the availability of a wide range of purified microcystins. Although over 60 variants have now been reported, only a very small number are commercially available and calibrated standards are not yet obtainable. This has led to the common practice of reporting microcystin-LR equivalence regardless of which variant is present. The increased availability of HPLC with online mass spectral analysis (HPLC-MS) may facilitate more accurate detection of toxin variants but as several microcystins share the same molecular mass, definitive identification can be difficult. A further difficulty in analyzing microcystins is the requirement for sample processing before analysis. Solid phase extraction (SPE) is typically used to enrich environmental concentrations of microcystins, or to eliminate contaminants from complex samples such as animal and plant tissues. Recently, new technologies employing recombinant antibodies and molecularly imprinted polymers have been exploited to develop assays and biosensors for microcystins. These novel detection systems are highly sensitive, often do not require sample processing, and offer a simpler, less expensive alternative to analytical techniques. They have also been successfully employed in solid phase extraction formats for the concentration and clean up of environmental samples before HPLC analysis.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号