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脂质作为细胞膜和亚细胞膜的主要结构成分,在能量来源、细胞信号传导等多种生物学过程中发挥着重要作用。近年来,脂质分析受到越来越多的关注,其中色谱-质谱联用技术在脂质分析中占据主导地位。由于样品基质复杂,样品前处理有富集痕量物质和减少基质干扰的作用,成为脂质分析中的一个关键步骤。该文综述了近年来基于色谱-质谱联用技术的脂质分析中样品前处理技术的研究进展和应用,对各种样品前处理技术进行了阐述和总结。基于液相的萃取方法有液-液萃取和单一有机溶剂萃取。基于固相的萃取方法包括固相萃取和固相微萃取。场辅助萃取方法包括超临界流体萃取、加压流体萃取、微波辅助萃取和超声辅助萃取。此外,还介绍了在线联用样品前处理方法和用于活体分析的样品前处理方法。最后,对基于色谱-质谱联用的脂质分析样品前处理技术存在的问题及发展趋势进行了探讨。样品前处理技术的发展将提高脂质分析的灵敏度、选择性和分析速度。 相似文献
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《色谱》2020,(1)
脂质作为细胞膜和亚细胞膜的主要结构成分,在能量来源、细胞信号传导等多种生物学过程中发挥着重要作用。近年来,脂质分析受到越来越多的关注,其中色谱-质谱联用技术在脂质分析中占据主导地位。由于样品基质复杂,样品前处理有富集痕量物质和减少基质干扰的作用,成为脂质分析中的一个关键步骤。该文综述了近年来基于色谱-质谱联用技术的脂质分析中样品前处理技术的研究进展和应用,对各种样品前处理技术进行了阐述和总结。基于液相的萃取方法有液-液萃取和单一有机溶剂萃取。基于固相的萃取方法包括固相萃取和固相微萃取。场辅助萃取方法包括超临界流体萃取、加压流体萃取、微波辅助萃取和超声辅助萃取。此外,还介绍了在线联用样品前处理方法和用于活体分析的样品前处理方法。最后,对基于色谱-质谱联用的脂质分析样品前处理技术存在的问题及发展趋势进行了探讨。样品前处理技术的发展将提高脂质分析的灵敏度、选择性和分析速度。 相似文献
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作为一种常见的溴代阻燃剂,六溴环十二烷(HBCDs)因具备持久性、长距离迁移性、生物蓄积性和高毒性,于2013年被列入《斯德哥尔摩公约》。因此,环境样品中HBCDs污染水平的准确分析和严格控制对完善环境监管长效机制至关重要。然而,实际样品中HBCDs的定性定量分析正面临着基质复杂、目标物含量低等问题。尤其,HBCDs在高温环境及特定有机溶剂中易降解,会产生异构体,提高了分析难度。该综述简述了HBCDs的理化性质、毒性危害和标准限制,重点围绕不同基质中HBCDs的样品前处理和仪器检测两方面进行了总结。论文内容引用2000~2022年的70余篇源于科学引文索引(SCI)与中文核心期刊中的相关论文。总结归纳了固体和液体样品中HBCDs分析的前处理技术,包括索式提取、超声辅助萃取、加速溶剂萃取、超临界流体萃取、液液萃取、分散液液微萃取、固相萃取、分散固相萃取和固相微萃取等,介绍了气相色谱、液相色谱和色谱-质谱联用技术等仪器检测方法在HBCDs分析中的应用。通过综述近期相关研究,侧面表明HBCDs的分析方法研究发展迅速,但也面临一些挑战,如样品前处理步骤繁琐、耗时长、样品量和有机溶剂用量大等问题。最后,对新型样品前处理技术在HBCDs分析中的应用进行了展望。 相似文献
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卤代阻燃剂被广泛用作油漆、纺织品、电子器件的添加剂,由于其具有挥发性,能渗入并长久存在于环境中,在环境和食物链中积累,对人类和其他生物健康造成危害,现已被禁止或限制使用。因此,急需建立更加灵敏、准确的卤代阻燃剂残留分析方法。本文系统介绍了卤代阻燃剂的污染途径,以及近年来关于卤代阻燃剂残留样品前处理方法和检测技术,污染途径包括:土壤、水体、空气、灰尘和生物样品污染途径等;样品前处理方法包括:固相萃取、搅拌棒萃取、分子印迹萃取、磁性固相萃取、超临界流体萃取、加压液体萃取等;检测技术包括:气相色谱-质谱检测法、液相色谱-质谱检测法、免疫分析检测法、X射线荧光法等,并对卤代阻燃剂的分析检测技术进行了总结和展望。 相似文献
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水产品含有丰富的蛋白、维生素和多种微量元素,是人们摄取动物性蛋白质的重要来源之一,我国是世界上最大的水产品消费国,其质量安全问题一直备受关注。但水产样品基质复杂,有害物质的含量低,须对其进行分离富集后才能进行检测,传统的液-液萃取、固相萃取和快速固相分散萃取等样品前处理技术在水产品分析中得到广泛应用,同时针对一些挥发性和超痕量有害物质检测时,固相微萃取同样体现出巨大优势。这些样品前处理技术可以有效去除基体对分析对象的干扰,提高检测方法的灵敏度和准确度。根据目标分析物性质的不同,选择合适的样品前处理技术,是水产品中有害物质分析的关键步骤。该文以水产品中有害物的来源不同,将其分为3类:(1)水产品中环境污染物的分析;(2)养殖运输和加工过程中有害物的分析;(3)水产品中生物毒素的分析。以这3类有害物质的分析为主线,综述了近10年水产品中有害物质分析的样品前处理技术,包括液-液萃取、固相萃取、固相微萃取、快速固相分散萃取和磁性固相萃取等。此外,还对各种技术的优缺点进行了探讨,并对其未来发展方向进行了展望。 相似文献
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Turbulent flow chromatography coupled to tandem mass spectrometry (TFC-MS-MS) has been widely used within bioanalysis, because of the ability to inject directly neat biological samples with no prior pretreatment. TFC-MS-MS removes the need for time consuming sample preparation procedures such as protein precipitation, liquid-liquid extraction or solid-phase extraction. There are two standard configurations that are commonly adopted for the use of TFC, namely fast elute and focus mode. In this paper, a new micro TFC column which has the advantages of reducing solvent consumption and improving mass sensitivity, was used to develop a fast elute method. A wide range of pharmaceutical compounds with various physicochemical properties was used to assess the system performance. Carry-over has often been identified as a potential source of inaccuracy in a fast elute mode. This paper shows how by using a systematic approach, carryover was eliminated. The parameters influencing the robustness of the micro TFC column are also discussed. This method was fully validated for a Pfizer development compound in human plasma using a new TFC parallel platform allowing two systems to be operated in parallel. Multiplexing the sample analysis allowed a 2-fold increase in throughput and provided an efficient use of the mass spectrometer. 相似文献
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R C Williams 《International journal of environmental analytical chemistry》1984,18(1-2):37-49
The Du Pont PREP automated sample processor is a centrifugally based, microprocessor controlled instrument that was designed for extraction of samples from biological fluids. Extraction takes place in cartridges containing either organic resins or bonded silica packings as extraction sorbants. This paper will discuss the application of several lipophilic and ion exchange sorbants to the extraction of biological samples from body fluids. The advantages of these different types of sorbants will be compared and their performance with automated sample preparation will be shown. A variety of applications including the extraction of benzodiazepine, barbiturate, aminoglycoside and anticonvulsant drugs and their metabolites from serum, urine, and tissue homogenates will be discussed. 相似文献
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Abstract The Du Pont PREPTM automated sample processor is a centrifugally based, microprocessor controlled instrument that was designed for extraction of samples from biological fluids. Extraction takes place in cartridges containing either organic resins or bonded silica packings as extraction sorbants. This paper will discuss the application of several lipophilic and ion exchange sorbants to the extraction of biological samples from body fluids. The advantages of these different types of sorbants will be compared and their performance with automated sample preparation will be shown. A variety of applications including the extraction of benzodiazepine, barbiturate, aminoglycoside and anticonvulsant drugs and their metabolites from serum, urine, and tissue homogenates will be discussed. 相似文献
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This review attempts to provide an updated overview (including works published till June 2006) on the latest applications of compressed fluids as sample preparation techniques for food analysis. After a general review of the principles of supercritical fluid extraction (SFE) and pressurized liquid extraction (PLE; also called accelerated solvent extraction, ASE or subcritical water extraction, SWE, when water is employed as extraction solvent), the principal applications of such techniques in the mentioned fields of food and natural products are described, discussing their main advantages and drawbacks. 相似文献
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State-of-the-art methods of the extraction, preconcentration, and determination of quercetin and other flavonoids are described.
Different methods of sample preparation of real samples are compared, including solvent extraction from solid matrices and
liquid-liquid, supercritical fluid, and solid-phase extraction. The following main determination methods are discussed: HPLC,
thin-layer chromatography, capillary electrophoresis, spectrophotometry, luminescence, and electrochemical methods. Some examples
of quercetin determination in biological fluids, food products, biologically active food supplements, pharmaceutical preparations,
and plant samples are given. 相似文献
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Stir bar sorptive extraction based on restricted access material for the direct extraction of caffeine and metabolites in biological fluids 总被引:2,自引:0,他引:2
A biocompatible stir bar sorptive extraction (SBSE) device was prepared using an alkyl-diol-silica (ADS) restricted access material (RAM) as the SBSE coating. The RAM-SBSE bar was able to simultaneously fractionate the protein component from a biological sample, while directly extracting caffeine and its metabolites, overcoming the present disadvantages of direct sampling in biological matrices by SBSE, such as fouling of the extraction coating by proteins. Desorption of the analytes was performed by stirring the bar in a water/ACN mixture (3/1, v/v) and subsequently reconcentrating the sample solution in water to enable HPLC-UV analysis to be performed. The limit of detection, based on a signal to noise ratio of 3, for caffeine was 25 ng/mL in plasma. The method was confirmed to be linear over the range of 0.5-100 microg/mL of caffeine with an average linear coefficient (R2) value of 0.9981. The injection repeatability and intra-assay precision of the method were evaluated over ten injections, resulting in a %RSD of approximately 8%. The RAM-SBSE device was robust (>50 extraction in plasma without significant signal loss) and simple to use, providing many direct extractions and subsequent determination of caffeine and its metabolites in biological fluids. In contrast to existing sample preparation methods for the analysis of caffeine and selected metabolites in biological fluids, this feasibility study using a biocompatible SBSE approach was advantageous in terms of simplifying the sample preparation procedures. 相似文献
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磁性固相萃取(Magnetic solid-phase extraction,MSPE)是一种采用磁性材料作为吸附剂的新型样品前处理技术,发展新型的磁性材料作为吸附剂是MSPE领域的研究热点。用离子液体(Ionic liquid,IL)修饰磁性材料作为吸附剂既具有MSPE操作简单、萃取快速、基质干扰小的优点,又兼具IL结构的可设计性和易功能化的优点,在样品前处理领域引起了广泛关注。该文综述了IL修饰磁性吸附剂的制备方法(物理涂敷、化学键合和包埋法),IL-MSPE的萃取方式(传统的MSPE,混合半胶束-MSPE和分散液液微萃取-MSPE),以及IL-MSPE在有机污染物、金属离子和生物活性物质萃取分离中的应用,并对该技术的发展趋势进行了展望。 相似文献
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Paula Berton Nerina B. Lana Juan M. Ríos Juan F. García-Reyes Jorgelina C. Altamirano 《Analytica chimica acta》2016
Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003–2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed. 相似文献
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Electro-assisted extraction of ionic drugs from biological fluids through a supported liquid membrane (SLM) and into an aqueous acceptor solution was recently introduced as a new sample preparation technique termed electromembrane extraction (EME). The applied electrical potential across the SLM has typically been in the range of 1-300 V. Successful extractions have been demonstrated even with common batteries (9 V) instead of a power supply. The chemical composition of the SLM has been crucial for the selectivity and for the recoveries of the extraction. Compared to other liquid-phase microextraction techniques (LPME), extraction times have been reduced by a factor of 6-17, and successful extractions have been obtained at extraction times of 1-5 min, and even down to a few seconds with online microfluidic EME devices. The technique has provided very efficient sample clean-up and has been found well suited for the extraction of sample sizes in the low μL range. Extractions have been performed with both rod-shaped hydrophobic porous fibers and with flat hydrophobic porous sheets as SLM support. The technique has been successfully downscaled into the micro-chip format. The nature of the SLM has been tuned for extraction of drugs with different polarity allowing extractions to be tailored for specific applications depending on the analyte of interest. The technique has been found to be compatible with a wide range of biological fluids and extraction of drugs directly from untreated human plasma and whole blood has been demonstrated. EME selectively extracts the compounds from the complex biological sample matrix as well as allowing concentration of the drugs. With home-built equipment fully acceptable validation results have been obtained. 相似文献
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A review of sample preparation methods for organic acids in biological fluids, in particular serum and urine, is presented. It covers techniques on organic acid determination without sample preparation, release of organic acids from binding locations, removal of proteins by protein precipitation and ultrafiltration, isolation of the organic acids by liquid-liquid and liquid-solid extraction, purification of the extract, derivatization and pre-fractionation. The various alternative sample preparation steps are compared and critically discussed. Examples of applications including profile analysis of organic acids by gas chromatography (GC), determination of particular organic acids by GC or liquid chromatography and determination of fatty acids as a distinct chemical class of acids demonstrate that the kind of sample preparation chosen depends strongly on the analytical aims. 相似文献