液相微萃取技术及其在生物样品预处理中的应用进展

液相微萃取是在液相萃取技术基础上发展起来的新型生物样品前处理技术,具有简便、快速、经济、环保等特点,已在血液、尿液、唾液等生物基质样品分析中广泛应用。本文通过查阅近5年文献,对液相微萃取技术的主要模式,即单液滴微萃取、分散液-液微萃取和中空纤维液相微萃取的基本原理,以及其在生物样品预处理中的应用进展进行综述,以期为体内药物分析、药代动力学研究以及新药研发等领域样品前处理提供技术支撑和参考。     

分散液相微萃取技术在药物分析中的应用

目的综述分散液相微萃取(dispersive liquid-liquid microextraction,DLLME)的研究进展及其在药物分析中的应用。方法查阅国内外文献,并进行分析和总结。结果 DLLME是一种新型样品前处理方法,具有操作简单、快速、有机溶剂消耗量少、富集倍数高等优点,受到研究者的重视。该技术发展迅速、应用广泛。结论 DLLME在药物快速分析中的应用前景广阔。     

中空纤维膜液相微萃取技术及其应用进展

中空纤维膜液相微萃取技术是一种集采样、萃取和浓缩于一体,环境友好的样品前处理技术。本文介绍了多孔中空纤维膜的结构特点、微萃取装置以及萃取模式,对影响其萃取效果的因素加以分析,同时介绍了中空纤维膜液相微萃取技术在环境和生物体液等样品中的应用。     

中空纤维液相微萃取技术的应用研究

近年来,随着人们对食品和环境安全的重视度不断提高,单纯的检测分析不能对复杂样品中痕量组分进行定量分析,也使传统的样品前处理面临新的挑战,因此,寻求一种高富集、绿色环保、快速净化的样品前处理新技术,已成为目前检测分析研究的热点之一.基于这一问题,提出了中空纤维的液相微萃取(HF-LPME),其具有高浓缩、快速友好的样品前处理功能.本文重点对HF-LPME的模式及原理、仪器装置、影响因素、应用领域以及发展前景作了综述.     

固相微萃取技术及其在药物分析中的应用

固相微萃取(SPME)技术作为一种样品前处理方法,能够对样品中的痕量分析物进行富集,具有操作简单、高通量、有机溶剂用量少、易自动化的特点。该技术集提取、浓缩、进样于一体,大幅提高了萃取效率。该研究在介绍SPME技术的基础上,综述了近年来SPME在药物分析领域的应用,并简要探讨其局限性与发展前景,为复杂基质中的痕量组分检测提供了参考。     

萃取技术在药物分析中的应用

简要介绍几种色谱分析样品处理技术中萃取技术的原理和特点,以及在天然药物有效成分的提取、鉴定、含量测定及生物样品中药物的检测和药物有机残留溶剂残留量测定等方面的应用。     

一种新型固相萃取技术——固相微萃取

固相微萃取技术是９０年代初新发展起来的集采样,萃取,浓集,进样于一体的分析技术,具有操作简单易行,不必使用大量有机溶剂,且易实现自动化等优点。本文对该技术的实验方法,原理及其在药物分析、环境保护等领域中的应用进行了综述。     

固相微萃取技术的原理,应用及发展

固相微萃取是近年来发展起来的集采样、萃取、浓缩、进样于一体综合技术，具有不使用有毒有机溶剂、操作简单快速、适用范围广等优点。它采用一相聚合物涂层的熔融石英纤维从样品基南中或样品上方的顶空气体中直接吸附萃取待测物，然后在色谱进样口解吸，分析。本文综述了技术的原理、应用以及近期发展。     

生物样品中苯丙胺类药物的检测进展

苯丙胺类化合物是一类人工合成的有机胺类兴奋剂,又称作苯丙胺类兴奋剂(amphetamine-type stinmulants,ATS).     

中空纤维液相微萃取及其在生物碱解离常数测定中的应用

目的探讨中空纤维液相微萃取(HFLPME)对药根碱、黄连碱、巴马汀、小檗碱的萃取行为;揭示供相OH-(H+)浓度对碱(酸)性分析物HFLPME浓缩倍数的影响规律,利用此规律测定弱碱性分析物的解离常数(pKb)。方法液相微萃取以聚丙烯中空纤维为溶剂载体,正辛醇作为萃取溶剂,供相为10-4mol/L的氢氧化钠溶液,接受相为10-2mol/L盐酸溶液,搅拌速度1200r/min,萃取时间60min。结果在优化的HFLPME条件下,4种分析物药根碱、黄连碱、巴马汀、小檗碱的的富集倍数在12.9～64.6倍;pKb分别为6.95,3.30,3.40和4.08。结论 HFLPME的成功应用为碱性化合物的pKb的测定提供了理论依据和实验方法。     

Application of hollow fiber liquid phase microextraction and dispersive liquid–liquid microextraction techniques in analytical toxicology

The recent developments in hollow fiber liquid phase microextraction and dispersive liquid –liquid microextraction are reviewed. Applications of these newly emerging developments in extraction and preconcentration of a vast category of compounds including heavy metals, pesticides, pharmaceuticals and abused drugs in complex matrices (environmental and biological matrices) are reviewed and discussed. The new developments in these techniques including the use of solvents lighter than water, ionic liquids and supramolecular solvents are also considered. Applications of these new solvents reduce the use of toxic solvents and eliminate the centrifugation step, which reduces the extraction time.     

用中空纤维液相微萃取-HPLC法测定人血浆中酒石酸美托洛尔的浓度

目的:建立中空纤维液相微萃取-HPLC法测定人血浆中酒石酸美托洛尔的浓度.方法:优化酒石酸美托洛尔液相微萃取法供给相和接受相的浓度、萃取时间、萃取温度、萃取转速和离子强度,血浆样品经中空纤维液相微萃取法萃取后,用HPLC法测定酒石酸美托洛尔的浓度.色谱柱:Agilent Zorbax Eclipse XDB-C18柱,流动相:甲醇-0.1％磷酸(40∶60),流速:1 ml/min,激发波长:227 nm,发射波长:305 nm,柱温:30℃.结果:酒石酸美托洛尔在2～ 125 ng/ml线性关系良好,低、中、高三种浓度(5、20、100 ng/ml)的日内、日间精密度均＜10％,回收率分别为(87.1±7.3)％、(92.6±5.8)％和(89.1±2.5)％.结论:中空纤维液相微萃取-HPLC法适用于测定血浆样品中酒石酸美托洛尔的浓度.     

Miniaturized hollow fibre assisted liquid‐phase microextraction and gas chromatography for determination of trace concentration of sufentanil and alfentanil in biological samples

A simple and highly sensitive method that involves miniaturized hollow fibre assisted liquid‐phase microextraction with gas chromatography‐flame ionization detector was developed for the determination of trace concentration of sufentanil and alfentanil in biological samples. These drugs were extracted from 5 ml of aqueous solution with pH 10.0 into an organic extracting solvent (1‐octanol) impregnated in the pores and lumen of a hollow fibre. After extraction for a prescribed time, 2.0 µl of the extraction solvent was injected directly in to the GC injection port. Under the optimized conditions, (1‐octanol as extracting solvent, stirring rate of 700 rpm, 15% (w/v) salt addition, pH 10.0 and 25 min sampling time at 50 °C) large enrichment factors of 535 and 420 were achieved for sufentanil and alfentanil, respectively. Dynamic linear ranges were in the range of 0.05 to 500 ng/ml for sufentanil and 0.1 to 500 ng/ml for alfentanil. Limits of detection 0.01 and 0.02 ng/ml were obtained for sufentanil and alfentanil, respectively. The percent relative intra‐day and inter‐day standard deviations were found to be less than 8.4% (n = 5). Finally, this method was successfully applied for the separation, preconcentration and determination of trace concentration of sufentanil and alfentanil in plasma and urine samples. Copyright © 2012 John Wiley & Sons, Ltd.     

A guide to recent trends in green applications of liquid phase microextraction for bioanalytical sample preparations

Liquid phase microextraction (LPME) techniques have become increasingly important components for bio-analytical sample preparation methods due to the versatility, adaptability, sensitivity, and conformity to green analytical chemistry (GAC) principles that they provide for the analyses of complex biological matrices. Despite having been used for sample preparations for some 25 years, LPME is not a static sample preparation field, but is continuously undergoing innovation and improvements and new research and applications for bio-analytical sample preparation are being published constantly. This review is meant to serve not only as a listing of recent literature, but as a guide to current trends in LPME. In order to fully understand the trends, advantages and limitations of this field in bio-analytical sample analyses, LPME based methods are compared with traditional sample preparation methods, the limitations and advantages of each LPME mode examined, and a variety of reviews and successful applications papers for LPME are included. To simplify searching for appropriate LPME methods these reviews and applications have been categorized to aid in searching for a needed application technique or publication. Following sections briefly cover the trends in LPME development, concentrating on bioanalytical sample preparation applications. The review continues with an examination of the trends for the use use of non-traditional green solvents for LPME based methods, and concludes with a discussion of recent innovations which have the potential for commercialization of high throughput automation for LPME based bio-analytical sample preparation and analysis methods.     

Hollow fiber-based liquid phase microextraction (HF-LPME) as a new approach for the HPLC determination of fluoroquinolones in biological and environmental matrices

In this paper, a three phase hollow fiber-based liquid phase microextraction (HF-LPME) combined with a HPLC procedure using diode array (DAD) and fluorescence detection (FLD) has been developed for the determination of eight widely used fluoroquinolones: marbofloxacin (MRB), norfloxacin (NRF), ciprofloxacin (CPR), danofloxacin (DNF), enrofloxacin (ENR), gatifloxacin (GTF), grepafloxacin (GRP) and flumequine (FLM). A Q3/2 Accurel PP polypropylene hollow fiber supporting 1-octanol was used between a 2 M Na2SO4 aqueous solution (pH 7) as donor phase and aqueous solution (pH 12) as acceptor phase. The microextraction parameters were optimised from an experimental central composite design. The procedure allows very low detection and quantitation limits of 0.3-16 ng L(-1) and 1-50 ng L(-1), respectively. The proposed method was applied to the determination of the analytes in bovine urine and in environmental water samples (surface, tap and wastewater).     

液相微萃取光化学荧光高效液相色谱法测定生物样品中枸橼酸氯米芬顺反异构体的含量

目的:建立液相微萃取光化学荧光高效液相色谱法测定生物样品中枸橼酸氯米芬顺反异构体的含量。方法:应用自制的液相微萃取装置,对生物样品中的枸橼酸氯米芬顺反异构体萃取后,分离采用 Sinochrom ODS—BP C_(18)色谱柱(200 mm×4.6mm,5μm);流动相为甲醇-水(70∶30,每1L 水含0.25 mL 磷酸、50μL三乙胺);流速为0.8 mL·min~(-1);荧光检测器的激发波长和发射波长分别为255 nm 和378 nm;柱温20℃。结果:利用该方法可以将血浆、尿液和肝脏组织匀浆中的枸橼酸氯米芬顺反异构体同时提取分离,浓缩倍数可达5～7倍;枸橼酸氯米芬在血浆、尿液和肝脏中的线性范围分别为0.05～20μg·mL~(-1),0.02～20μg·mL~(-1),0.04～40μg·g~(-1);检出限分别为20 ng·mL~(-1),10μg·mL~(-1),20 ng·g~(-1);精密度试验的 RSD 小于11.7%。结论:本文将液相微萃取技术应用于生物样品中枸橼酸氯米芬顺反异构体的提取分离,利用高效液相色谱法荧光检测,获得了较好的效果。     

Three-phase hollow fiber liquid-phase microextraction based on two immiscible organic solvents for determination of tramadol in urine and plasma samples

Recently, the new concept of three-phase liquid microextraction was introduced based on applying two immiscible organic solvents in lumen and wall pores of hollow fiber. In the present work, this novel microextraction technique combined with gas chromatography-mass spectrometry has been developed for determination of tramadol, an analgesic agent, in plasma and urine samples. A systematic investigation of the proposed method was applied to find optimal extraction conditions and evaluate the interaction effects between the factors by designing experiments according to the methodology of Box-Behnken response surface design. Analysis of variance (ANOVA) revealed that the important factors contributing to extraction efficiency are extraction time, stirring rate and hollow fiber length. Under the optimum conditions, the developed method provided a preconcentration factor of 546, good repeatability (RSD % = 6.4), and good linearity (r² = 0.995) for spiked plasma and urine real samples. The linear dynamic range from 0.1 to 400 μg L⁻¹ and limit of detection (LOD) of 0.08 μg L⁻¹ were obtained under selected ion monitoring mode. The results demonstrated that three-phase hollow fiber microextraction based on two immiscible solvents is a simple and accurate technique with very good preconcentration factor and clean-up for extraction of tramadol from biological samples.     

Extraction and determination of trace amounts of chlorpromazine in biological fluids using hollow fiber liquid phase microextraction followed by high-performance liquid chromatography

In the present work, hollow fiber liquid phase microextraction (HF-LPME) in conjunction with reversed-phase HPLC/UV was developed for extraction and determination of trace amounts of chlorpromazine in biological fluids. The drug was extracted from an 11 ml aqueous sample (source phase; SP) into an organic phase impregnated in the pores of the hollow fiber (membrane phase; MP) followed by the back-extraction into a second aqueous solution (receiving phase; RP) located in the lumen of the hollow fiber. The effects of several factors such as the nature of organic solvent, compositions of SP and RP solutions, extraction time, ionic strength and stirring rate on the extraction efficiency of the drug were examined and optimized. Under the optimal conditions, enrichment factor of 250, dynamic linear range of 1–500 μg l⁻¹, and limit of detection of 0.5 μg l⁻¹ were obtained for the drug. The percent relative intra-day and inter-day standard deviation (R.S.D.%) based on three replicate determinations were 6.7 and 10.3%, respectively. The method was applied to drug level monitoring in the biological fluids and satisfactory results were obtained.