基于色谱-质谱联用的脂质分析样品前处理技术研究进展（英文）

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。     

可卡因及代谢物的分析检测研究进展

综述了近十年来生物检材中可卡因及其代谢物分析常用的样品前处理技术和检测方法,比较了液-液萃取、固相萃取、固相微萃取等提取方法的可行性和局限性及气相色谱、气相色谱-质谱联用、液相色谱-质谱联用等检测方法的应用进展。     

分散液液微萃取技术的研究进展

分散液液微萃取是一种基于传统液液萃取的新型样品前处理技术。该文以分散液液微萃取技术中萃取剂的筛选为出发点,综述了低密度萃取剂、辅助萃取剂、反萃取剂和离子液体等低毒性萃取剂在该技术中的应用,以及应用自制装置、溶剂去乳化、悬浮萃取剂固化,辅助萃取,反萃取和离子液体-分散液液微萃取等萃取模式;并简要评述了该技术与液液萃取、固相萃取、固相微萃取、分散固相萃取、基质固相分散萃取、超临界流体萃取、超声辅助萃取等其他样品前处理技术的联用特性。     

六溴环十二烷的样品前处理和检测方法研究进展北大核心CSCD

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。     

兽药残留分析中样品前处理技术研究进展

样品前处理是兽药残留分析中的关键步骤,直接影响检测的结果.近年来,出现了一些新的样品前处理技术,如固相萃取、基质固相分散萃取、固相微萃取、搅拌棒吸附萃取、膜萃取、液相微萃取、超临界流体萃取、加速溶剂萃取、分子印迹、微波辅助萃取.这些技术能够有效地减少分析过程中由样品前处理过程带来的误差,具有前处理快速、简便的优点,同时可与分析仪器联用,实现分析的自动化.本文对这些新技术的基本原理、特点及在兽药残留分析中的应用进行了综述,并对样品前处理的前景进行了展望.     

样品前处理-色谱在线分析农药残留的研究进展

农药残留分析的样品来源多样、基体复杂,而传统的离线样品前处理中,萃取、转移、净化、浓缩等步骤分步进行,繁琐费时、样品损失较大、精密度和重现性差,因此,发展样品前处理-色谱在线分析技术可望解决这些问题。本文综述了近年来固相萃取、固相微萃取、基质固相分散萃取、膜萃取、微波辅助萃取、加速溶剂萃取和超临界萃取等样品前处理-色谱在线分析农药残留的研究进展,并展望了其应用前景和发展方向。引用文献54篇。     

食品中邻苯二甲酸酯类化合物的分析方法研究进展

邻苯二甲酸酯是应用最广泛的增塑剂,具有生殖、发育毒性及致癌性,是近年来食品污染的一个重要来源。该类化合物种类多、同系物和同分异构体性质接近、在基体中含量范围宽,高效样品前处理、高选择性分离和高灵敏检测、降低本底干扰等技术是食品中邻苯二甲酸酯类化合物准确测定面临的挑战。本文综述了液液萃取、液液微萃取、固相萃取、固相微萃取、基质固相萃取等传统及新型的提取与净化技术在食品样品分析中的应用,比较分析了气相色谱、液相色谱、串联质谱、高分辨质谱以及酶联免疫、离子迁移谱等快速检测技术的特点,并展望了发展趋势。     

鸡肉中兽药残留检测技术研究进展

鸡肉中兽药残留检测是食品安全检测关注的热点,作为目前普遍发展的样品前处理技术,超临界流体萃取、加速溶剂萃取、毛细管固相微萃取及其与色谱质谱联用检测兽药残留受到广泛关注。以鸡肉为主要检测基质对这些新技术的基本原理、特点及在兽药残留分析中的应用进行了综述,同时对兽药残留分析的研究方向进行了展望。     

油料油脂酚类化合物测定中样品前处理技术的研究进展

该文主要综述了油料油脂酚类化合物测定中的样品前处理技术研究进展,包括液液萃取、超声波辅助萃取、微波辅助萃取、超临界流体萃取、固相萃取以及磁固相萃取等。比较了不同前处理技术的优缺点,并对油料油脂酚类化合物测定中样品前处理技术研究趋势进行了展望。     

脂质组学分析中样品前处理技术的研究进展

脂质不仅是细胞膜的主要组成部分,还参与一些生命活动如能量存储、信号传导等,在生命体中发挥着重要作用。近年来,越来越多的研究表明脂质的变化与一些重大疾病的发生发展密切相关,脂质组学研究对理解疾病的发生机制及过程具有重要意义。在脂质分析过程中,由于样品基质的干扰或被分析物浓度的限制,通常需要对样品进行前处理,以得到最佳的分析性能。该文综述了脂质组学分析中的样品前处理技术,包括脂质的提取方法（如液液萃取、固相萃取等）和针对不同类脂质的化学衍生化技术在各领域,尤其是生命分析和代谢组学中的应用,并对脂质组学分析中的样品前处理技术的发展进行了展望。     

Advances in sample preparation in chromatography for organic environmental pollutants analyses

Many pollutants are present at trace level in our environment, which are beyond the scope of the detection by advance instruments too. Therefore, there is urgent need to develop advance sample preparation methods to determine the concentrations of the pollutants even at trace levels. Keeping this into consideration, many extraction techniques have been developed and applied for the analysis of organic pollutants in environmental samples. This review presents the sate-of-the-art of sample preparation methods in environmental samples. The extraction techniques discussed are headspace, liquid based extraction, supported liquid, homogeneous liquid–liquid, homogeneous liquid–liquid, single drop micro-extraction, membrane assisted solvent, solid-phase, molecularly imprinted solid-phase, monolithic spin column, matrix solid-phase, dispersive solid-phase, disposable pipette, magnetic solid-phase, solid-phase micro-extraction, micro-extraction by packed sorbent and stir bar sorptive. The article will be highly useful for environmental chromatographers.     

肉类食品中杂环胺检测的样品前处理及分析方法的研究进展

杂环胺是畜禽、鱼肉等食品在高温烹饪过程中生成的一类致癌、致突变化合物,高效、高选择性的样品前处理方法和高灵敏的分析方法是食品中痕量杂环胺分析检测的关键。本文综述了近年来溶剂萃取、固相萃取和固相微萃取等样品前处理方法,以及液相色谱、液相色谱-质谱等分析方法在食品中痕量杂环胺检测中的应用,结合现有研究对其发展趋势进行了展望。共引用文献51篇。     

Sample treatment and determination of pesticide residues in fatty vegetable matrices: A review

A demanding task in pesticide residue analysis is yet the development of multi-residue methods for the determination of pesticides in vegetables with relatively high fat content (i.e. edible oils and fatty vegetables). The separation of pesticides and other chemical contaminants from high-fat food samples prior to subsequent steps in the analytical process is yet a challenging issue to which much effort in method development has being applied. This review addresses the main sample treatment methodologies for pesticide residue analysis in fatty vegetable matrices. Even with the advent of advanced hyphenated techniques based on mass spectrometry these complex fatty matrices usually require extensive sample extraction and purification. Current methods involve the use of one or the combination of some of the following techniques for both the sample extraction and clean-up steps: liquid-liquid partitioning, solid-phase extraction (SPE), gel-permeation chromatography (GPC), matrix solid-phase dispersion (MSPD), etc. An overview of methods developed for these contaminants in fatty vegetables matrices is presented. Sample extraction and purification techniques are discussed and their most recent applications are highlighted. This review emphasizes that sample preparation is a critical step, but also the determination method is, and cannot be treated separately from sample treatment. In recent years, the appearance and use of new, more polar pesticides has fostered the development of liquid chromatography/mass spectrometry (LC-MS) besides gas chromatography. The main features of LC-MS for the analysis of multi-class pesticides in fatty vegetable samples will be also underlined, with an emphasis on the multi-class, multi-residue strategy and the difficulties associated.     

Analytical methods for the assessment of endocrine disrupting chemical exposure during human fetal and lactation stages: A review

In the present work, a review of the analytical methods developed in the last 15 years for the determination of endocrine disrupting chemicals (EDCs) in human samples related with children, including placenta, cord blood, amniotic fluid, maternal blood, maternal urine and breast milk, is proposed. Children are highly vulnerable to toxic chemicals in the environment. Among these environmental contaminants to which children are at risk of exposure are EDCs —substances able to alter the normal hormone function of wildlife and humans—. The work focuses mainly on sample preparation and instrumental techniques used for the detection and quantification of the analytes. The sample preparation techniques include, not only liquid–liquid extraction (LLE) and solid-phase extraction (SPE), but also modern microextraction techniques such as extraction with molecular imprinted polymers (MIPs), stir-bar sorptive extraction (SBSE), hollow-fiber liquid-phase microextraction (HF-LPME), dispersive liquid–liquid microextraction (DLLME), matrix solid phase dispersion (MSPD) or ultrasound-assisted extraction (UAE), which are becoming alternatives in the analysis of human samples. Most studies focus on minimizing the number of steps and using the lowest solvent amounts in the sample treatment. The usual instrumental techniques employed include liquid chromatography (LC), gas chromatography (GC) mainly coupled to tandem mass spectrometry. Multiresidue methods are being developed for the determination of several families of EDCs with one extraction step and limited sample preparation.     

Recent advances and trends in miniaturized sample preparation techniques

Advances in the area of sample preparation are significant and have been growing significantly in recent years. This initial step of the analysis is essential and must be carried out properly, consisting of a complicated procedure with multiple stages. Consequently, it corresponds to a potential source of errors and will determine, at the end of the process, either a satisfactory result or a fail. One of the advances in this field includes the miniaturization of extraction techniques based on the conventional sample preparation procedures such as liquid‐liquid extraction and solid‐phase extraction. These modern techniques have gained prominence in the face of traditional methods since they minimize the consumption of organic solvents and the sample volume. As another feature, it is possible to reuse the sorbents, and its coupling to chromatographic systems might be automated. The review will emphasize the main techniques based on liquid‐phase microextraction, as well as those based upon the use of sorbents. The first group includes currently popular techniques such as single drop microextraction, hollow fiber liquid‐phase microextraction, and dispersive liquid‐liquid microextraction. In the second group, solid‐phase microextraction techniques such as in‐tube solid‐phase microextraction, stir bar sorptive extraction, dispersive solid‐phase extraction, dispersive micro solid‐phase microextraction, and microextraction by packed sorbent are highlighted. These approaches, in common, aim the determination of analytes at low concentrations in complex matrices. This article describes some characteristics, recent advances, and trends on miniaturized sample preparation techniques, as well as their current applications in food, environmental, and bioanalysis fields.     

Reproducibility of serum protein profiling by systematic assessment using solid-phase extraction and matrix-assisted laser desorption/ionization mass spectrometry

Protein profiling of human serum by matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS) is potentially a new diagnostic tool for early detection of human diseases, including cancer. Sample preparation is a key issue in MALDI MS and the analysis of complex samples such as serum requires optimized, reproducible methods for handling and deposition of protein samples. Data acquisition in MALDI MS is also a critical issue, since heterogeneity of sample deposits leads to attenuation of ion signals in MALDI MS. In order to improve the robustness and reproducibility of MALDI MS for serum protein profiling we investigated a range of sample preparation techniques and developed a statistical method based on repeated analyses for evaluation of protein-profiling performance of MALDI MS. Two different solid-phase extraction (SPE) methods were investigated, namely custom-made microcolumns and commercially available magnetic beads. Using these two methods, nineteen different sample preparation methods for serum profiling by MALDI MS were systematically tested with regard to matrix selection, stationary phase, selectivity, and reproducibility. Microcolumns were tested with regard to chromatographic properties; reversed phase (C8, C18, SDB-XC), ion-exchange (anion, weak cation, mixed-phase (SDB-RPS)) and magnetic beads were tested with regard to chromatographic properties; reversed phase (C8) or affinity chromatography (Cu-IMAC). The reproducibility of each sample preparation method was determined by enumeration and analysis of protein signals that were detected in at least six out of nine spectra obtained by three triplicate analyses of one serum sample.A candidate for best overall performance as evaluated by the number of peaks generated and the reproducibility of mass spectra was found among the tested methods. Up to 418 reproducible peaks were detected in one cancer serum sample. These protein peaks can be part of a possible diagnostic profile, suggesting that this sample preparation method and data acquisition approach is suitable for large-scale analysis of serum samples for protein profiling.     

Determination of major aroma impact compounds in fermented cucumbers by solid-phase microextraction--gas chromatography--mass spectrometry--olfactometry detection

Purge-and-trap, solid-phase extraction, and solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) sample preparation techniques for the analysis of odor impact chemicals in fermented cucumber brine are compared. SPME-GC-MS is coupled with detection frequency olfactometry experiments to determine key impact odor compounds in the brine. The most potent odorants that define the typical characteristic brine aroma are trans-4-hexenoic acid and cis-4-hexenoic acid. Confirmation of key impact odorants in brine is confirmed by recombination experiments.     

Automated sample preparation using in-tube solid-phase microextraction and its application -- a review

Sample preparation, such as extraction, concentration, and isolation of analytes, greatly influences their reliable and accurate analysis. In-tube solid-phase microextraction (SPME) is a new effective sample preparation technique using an open tubular fused-silica capillary column as an extraction device. Organic compounds in aqueous samples are directly extracted and concentrated into the stationary phase of capillary columns by repeated draw/eject cycles of sample solution, and they can be directly transferred to the liquid chromatographic column. In-tube SPME is an ideal sample preparation technique because it is fast to operate, easy to automate, solvent-free, and inexpensive. On-line in-tube SPME-performed continuous extraction, concentration, desorption, and injection using an autosampler, is usually used in combination with high performance liquid chromatography and liquid chromatography-mass spectrometry. This technique has successfully been applied to the determination of various compounds such as pesticides, drugs, environmental pollutants, and food contaminants. In this review, an overview of the development of in-tube SPME technique and its applications to environmental, clinical, forensic, and food analyses are described.     

Applications of solid‐phase micro‐extraction with mass spectrometry in pesticide analysis

Pesticides, widely applied in agriculture, can produce a variety of transformation products and their continuous use causes deleterious effects to ecosystem. Efficient and sensitive analytical techniques for enrichment and analysis of pesticides samples are highly required. Compared with other extraction methods, solid‐phase micro extraction is a solvent free, cost effective, robust, versatile, and high throughput sample preparation technique, especially for the analysis of pesticides from complicated matrices. Coupling of solid‐phase micro extraction with gas chromatography and mass spectrometry and liquid chromatography–mass spectrometry has been extensively applied in pesticide analysis. On the other hand, in recent years, combination of fast separation using solid‐phase micro extraction and rapid detection using ambient mass spectrometry is providing highly efficient pesticide screening. This article summarizes the applications of solid‐phase micro extraction coupled to mass spectrometry for pesticides analysis.