萃取技术在生物样品中毒物的提取与富集中的应用

提取与富集是生物样品中毒物分析的关键步骤，本综述了各种萃取技术在此领域中的应用，分别论述了溶剂萃取，固相萃取，固相微萃取，超临界流体萃取和亲和萃取等技术的特点，局限性及应用实例，为应用及发展生物样品中毒物萃取技术提取了参考。     

分子印迹聚合物的制备及其在临床药物分析中的应用进展

本文综述了近年来以分子印迹材料为基础的药物分析新方法及其在临床样本（血浆、尿液）中的应用，详细评述了基于分子印迹技术的固相萃取、固相微萃取、磁性固相萃取、传感器和酶联免疫分析等最新进展，为我国临床药物分析新方法研究提供参考。     

固相萃取技术在体内药物分析中的应用与发展

固相萃取技术是一种发展的较快的样品预处理技术,在传统技术基础上,出现了微粒填料薄膜以及固相微萃取技术。本文综述了近几年来固相革取技术在体内药物分析中的应用与进展。     

固相微萃取在生物体液分析中的研究进展

固相微萃取是一种无溶剂样品预处理技术。固相微萃取以其无需使用溶剂、样品用量少、有一定的富集作用等特点而受到广大分析工作者的关注。本文着重综述了该方法的装置、原理、影响因素及其应用，尤其是在使用气相色谱—质谱联用、高效液相色谱—质谱联用技术分析生物体液中的应用。     

生物样品预处理技术及应用进展

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。     

几种固相萃取新技术近十年的研究进展（英文）

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。     

中药材中残留农药的检测方法

综述了近年来中药材中残留农药的常用检测方法,以及固相微萃取、超临界流体萃取、基质固相分散技术、免疫亲和技术及分子烙印聚合物技术等新的提取净化方法,以及色谱、质谱、免疫技术在中药材残留农药检测中的应用。     

固相微萃取技术在制药和生物医学分析中的当前发展和未来趋势

在分析方法学中,样品制备对于从复杂的基质中分离、浓缩需要的痕量组分是非常重要的。样品制备是劳动力最密集而且最容易出错的过程,极大地影响了分析物测定的可靠性和准确性。通过使用微萃取技术和微型设备可以有效地完成之前需要多种分析仪器才可以做到的复杂样品的制备。固相微萃取(Solid-phase microextraction,SPME)作为其中一类,既简单又有效,具有小型化,自动化和高通量的特点。此外,固相微萃取可减少分析时间,降低溶剂消耗和处置成本。本文综述了新型固相微萃取技术的当前发展状况及未来趋势,包括纤维固相微萃取,管内固相微萃取和相关的新微萃取技术。这些方法在制药和生物医学分析中至关重要。     

固相萃取技术及其在体内药物分析中的应用

目的：了解固相萃取技术进展及应用情况。方法：从萃取机制、方法建立和萃取装置等对固相萃取技术进行综述，并对近年来该技术在体内药物分析方面的应用作了介绍。结果和结论：固相萃取技术萃取回收率高、易于自动化，能有效去除样品中的杂质等，适于生物样品的预处理。     

湖北恩施厚朴顶空固相微萃取方法考察

目的优化湖北恩施厚朴顶空固相微萃取（HS SPME）技术，确定最佳萃取条件。方法进行湖北恩施厚朴顶空固相微萃取方法的样品量、萃取温度、萃取时间、解析时间和萃取头的优化实验。结果样品量1.2 g，萃取时间90 min，萃取温度90 ℃，解析时间3 min，选用PDMS/DVB萃取头。结论该实验结果为湖北恩施厚朴的HS SPME提供了优化的条件。     

Analytical methods used in conjunction with solid-phase microextraction: a review of recent bioanalytical applications

Integration of sampling and sample preparation with various analytical instruments is a highly desirable feature for any analytical method. This is most conveniently achieved by using microextraction techniques or various microdevices. Among these techniques, solid-phase microextraction (SPME) is particularly remarkable due to its simplicity and effectiveness. This review discusses the most recent applications of SPME in bioanalysis, grouped according to the analytical instrument that SPME is coupled to. It is shown that one of the most important aspects of such analytical methods is the ability of SPME to perform direct and selective extraction of analytes from complex biological samples. By far, the most popular method continues to be SPME coupled to GC. Nevertheless, the last 2 years have witnessed significant advances in other areas, such as successful automation of SPME coupled to liquid chromatography and the development of new coatings suitable for direct extraction from biological samples. Furthermore, a few bioanalytical applications based on direct coupling of SPME to MS, ion mobility spectrometry, CE and analytical chemiluminescence have been reported.     

Recent advances in SPME techniques in biomedical analysis

Biomedical analyses of drugs, metabolites, poisons, environmental and occupational pollutants, disease biomarkers and endogenous substances in body fluids and tissues are important in the development of new drugs, therapeutic monitoring, forensic toxicology, patient diagnosis, and biomonitoring of human exposure to hazardous chemicals. In these analyses, sample preparation is essential for isolation of desired components from complex biological matrices and greatly influences their reliable and accurate determination. Solid-phase microextraction (SPME) is an effective sample preparation technique that has enabled miniaturization, automation and high-throughput performance. The use of SPME has reduced assay times, as well as the costs of solvents and disposal. This review focuses on recent advances in novel SPME techniques, including fiber SPME and in-tube SPME, in biomedical analysis. We also summarize the applications of these techniques to pharmacotherapeutic, forensic, and diagnostic studies, and to determinations of environmental and occupational exposure.     

Solid-phase microextraction in the determination of methadone in human saliva by gas chromatography-mass spectrometry

Solid-phase microextraction (SPME) with a 100-microm polydimethylsiloxane film fiber was applied to the determination of methadone and 2-ethylidine-3,3-diphenylpyrrolidine (EDDP) by GC-MS in human saliva and compared with liquid-liquid extraction. A shorter extraction time of 30 min with the fiber was obtained, speeding up the total analysis time. Linearity was found for SPME from 0.05 to 2.0 microg/mL (r = 0.9976 for methadone; r = 0.9988 for EDDP) with precision between 0.7 and 4.3% for saliva spiked with 0.2 and 1.5 microg/mL of methadone and EDDP. The limit of detection using SPME was 0.04 microg/mL for methadone and 0.008 microg/mL for EDDP. Analytical recoveries of SPME and liquid-liquid extraction ranged from 98.8 to 103.6%. The use of deuterated internal standard by both methods have yielded comparable results. Thus, the SPME method is highly accurate, precise, and useful for determination of methadone and EDDP in saliva.     

固相微萃取-气相色谱-质谱联用分析白苏子挥发性化学成分

目的分析白苏子中挥发性成分的组成,为其开发利用提供科学依据。方法采用固相微萃取（SPME）法萃取白苏子中的挥发性物质,并用气相色谱-质谱（GC-MS）法对其挥发性化学成分进行分析。结果共分离出60个色谱峰,并且确定了其中47个成分,占挥发性成分总量的89.73%。其中主要化学成分是羊脂酸（8.94%）,正己醛（8.31%）,天竺葵醛（6.27%）,（E,E）-3,5-辛二烯-2-酮（5.19%）。结论白苏子中含有丰富的挥发性成分,SPME-GC-MS联用能全面快速获得其组成信息,可应用于白苏子挥发性成分的分析。     

Solid-phase microextraction for cannabinoids analysis in hair and its possible application to other drugs

This paper describes the application of solid-phase microextraction (SPME) to cannabis testing in hair. Fifty milligrams of hair was washed with petroleum ether, hydrolyzed with NaOH, neutralized, deuterated internal standard was added and directly submitted to SPME. The SPME was analyzed by GC-MS. The limit of detection was 0.1 ng/mg for cannabinol (CBN) and delta9-tetrahydrocannabinol (THC) and 0.2 ng/mg for cannabidiol (CBD). THC was detected in a range spanning from 0.1 to 0.7 ng/mg. CBD concentrations ranged from 0.7 to 14.1 ng/mg, and CBN concentrations ranged from 0.4 to 0.7 ng/mg. The effectiveness of different decontamination procedures was also studied on passively contaminated hair. The proposed method is also suitable for the analysis of methadone in hair; cocaine and cocaethylene can be detected in hair with SPME extraction after enzymatic hydrolysis.     

Automated study of ligand-receptor binding using solid-phase microextraction

An automated ligand-receptor binding study was performed for the first time using solid-phase microextraction (SPME) coupled to liquid chromatography-tandem mass spectrometry. A new multi-fibre SPME system, which relies on multi-well plate technology and allows parallel preparation of up to 96 samples was used in order to obtain all data points of the binding curve in a single experiment. The binding of diazepam to human serum albumin was used as the model system in order to evaluate the performance of automated SPME. The time required to establish equilibrium was 30 min; this was verified experimentally by constructing extraction time profiles in the presence and absence of receptor molecules. Fibre constant calibration was used to remove inter-fibre variability from the binding data. Using a simple one-site binding model, a binding constant of 9.1 x 10(5)+/-3 x 10(5)l/mol was obtained. This result is in excellent agreement with values for equilibrium dialysis and manual SPME procedures reported in the literature. The proposed method can be further extended to study plasma-protein binding or drug binding to whole blood. In comparison to other methods, SPME is simpler, faster and fully automated, can be combined with any analytical detection method, and can be used to directly study complex samples.     

Solid-phase microextraction of human plasma samples for determination of sufentanil by gas chromatography-mass spectrometry

A solid-phase microextraction (SPME) method has been developed for the quantitative analysis of sufentanil from human plasma by gas chromatography-mass spectrometry (GC-MS). The immersion SPME sampling technique was optimized for the extraction of sufentanil from plasma. The influence of the pH and the ionic strength of the sample on the extraction of the analytes by the SPME fiber were investigated. Sufentanil and fentanyl (internal standard) were extracted from plasma with a 65-microm polydimethylsiloxane-divinylbenzene (PDMS-DVB) fiber for 30 minutes using salting out agents in basic conditions. The calibration curve was linear over a concentration range of 6-50 ng/mL. Intraday and interday relative standard deviations were 3.6% and 10.6%, respectively. The limit of quantification was 6 ng/mL for a plasma volume of 1 mL. With regard to selectivity, simplicity, and low cost, the SPME method described should be useful for a rapid extraction of sufentanil from human plasma.     

蜘蛛香地上部分挥发性成分的萃取与分析

目的分析蜘蛛香地上部分的挥发性成分。方法利用固相微萃取（SPME）法和水蒸气蒸馏（SD）法提取挥发性成分，并用气相色谱-质谱联用技术进行分析。结果SPME法共分离出了37个成分，已鉴定成分占挥发油总量的82．90％；SD法共分离出了24个成分，已鉴定成分占挥发油总量的93．46％。结论SPME法比SD法得到的成分多，且方法更简便、快速。     

Development of gas chromatography-mass spectrometry with microwave distillation and simultaneous solid-phase microextraction for rapid determination of volatile constituents in ginger

In this study, gas chromatography-mass spectrometry (GC-MS) following microwave distillation and solid-phase microextraction (MD-SPME) was developed for the analysis of essential oil compounds in fresh ginger. In the proposed method, the isolation, extraction and concentration of volatile components in ginger were carried out in one single step, using the MD-SPME technique, and the analytes on the SPME fiber were analyzed by GC-MS. Some parameters, including SPME fiber coating, microwave power and irradiation time, were optimized. The optimal experiment parameters obtained were: 65 microm PDMS/DVB SPME fiber, a microwave power of 400 W and an irradiation time of 2 min. To demonstrate its feasibility, MD-SPME was compared with conventional SPME for the extraction of essential oil compounds in fresh ginger. Using MD-SPME followed by GC-MS, 54 compounds were separated and identified in ginger, which mainly included geranial (5.25%), zingiberene (15.48%), beta-sesquiphellandrene (5.54%) and beta-phellandrene (22.84%), whereas only 39 compounds were separated and identified by conventional SPME followed by GC-MS. The relative standard deviation (R.S.D.) values of less than 10% show that the proposed method has good repeatability. The result show that MD-SPME, followed by GC-MS, is a simple, rapid, solvent-free method for the determination of volatile compounds in ginger.     

Measurement of trihalomethanes and methyl tert-butyl ether in whole blood using gas chromatography with high-resolution mass spectrometry

The prevalence of disinfection by-products in drinking water supplies has raised concerns about possible adverse health effects from chronic exposure to these compounds. To support studies exploring the relation between exposure to trihalomethanes (THMs) and adverse health effects, an automated analytical method was developed using capillary gas chromatography (GC) and high-resolution mass spectrometry (MS) with selected ion mass detection and isotope-dilution techniques. This method quantified trace levels of THMs (including chloroform, bromodichloromethane, dibromochloromethane, and bromoform) and methyl tert-butyl ether (MTBE) in human blood. Analyte responses were adequate for measuring background levels after extraction of these volatile organic compounds with either purge-and-trap extraction or headspace solid-phase microextraction (SPME). The SPME method was chosen because of its ease of use and higher throughput. Detection limits for the SPME GC-MS method ranged from 0.3 to 2.4 ng/L, with linear ranges of three orders of magnitude. This method proved adequate for measuring the THMs and MTBE in most blood samples tested from a diverse U.S. reference population.