液相色谱-串联质谱技术在临床检验中的应用研究进展

液相色谱-串联质谱(LC-MS/MS)技术具有高灵敏度、高特异性、高分辨率和高效率的优点。近年来随着仪器灵敏度的提高,LC-MS/MS在常规临床检验中显示出极大的潜力,并在疾病早期预防和诊断中发挥着不可替代的作用。本文对LC-MS/MS在新生儿疾病筛查、维生素D检测、内分泌激素检测、肽类和蛋白质定量分析等临床检验方面的研究进展进行综述,并讨论了未来面临的挑战。     

基于液相色谱-质谱联用技术的蛋白质类肿瘤标志物定量方法研究进展

液相色谱-质谱（LC-MS）联用技术因具有高通量、高灵敏度等优点而成为发现、验证生物标志物及对生物标志物进行定量分析的有力工具。近年来,LC-MS在临床应用中,特别是在定量肿瘤生物标志物方面做出了重要贡献。研究人员通过不同的设计原理开发出多种定量方法,逐步实现了对高度复杂样品中蛋白质类肿瘤标志物的准确定量。本文从用于定量蛋白质类肿瘤标志物的样品前处理方法及LC-MS分析中的质谱扫描策略两个方面,对近年来的主要定量方法进行总结。     

液相色谱-质谱联用技术在中药农药残留分析中的应用进展

液相色谱-质谱联用(LC-MS/MS)技术在农药残留分析领域的研究已经显示出极大的发展潜力。本文阐述LC-MS/MS法在农残分析中的研究进展,特别强调了该技术在中药农残分析中的应用现状和发展前景。由于样品前处理是农残分析中耗时最多、最易引起误差的关键环节,本文也讨论了最近发展和广泛应用的前处理技术,分析了不同方法的特点,从而为我国中药行业在农药残留方面的监测工作提供参考。     

基于LC-MS/MS测定人体类固醇激素的研究进展

类固醇激素是一类具有环戊烷多氢菲结构的化合物,由细胞色素P450酶催化形成,在调节机体代谢、促进性器官发育等方面起着重要作用。临床上将类固醇激素水平作为肾上腺疾病、精神类疾病等的诊断指标。液相色谱-串联质谱(LC-MS/MS)联用技术因具有高灵敏度、高通量和高专属性的特点,已成为类固醇临床测定的首选方法。本文综述了LC-MS/MS在内源性类固醇激素测定中的应用,特别是在样品前处理、色谱条件和质谱条件优化等方面的研究进展,为临床上类固醇激素的诊断检测提供参考。     

毛细管电泳-质谱联用中的若干关键技术问题及解决方案

自二十世纪八十年代以来,毛细管电泳-质谱联用技术（CE-MS）取得了长足发展。本文立足前人的研究成果,对CE-MS发展与应用过程中遇到的技术问题（如接口技术,背景电解质兼容性,迁移时间重现性等问题）及相应的解决方案进行了分析总结。与气相色谱-质谱联用（GC-MS）和液相色谱-质谱联用（LC-MS）相比,CE-MS有其独特的技术特点和优势,已经成为一种重要的分离检测模式,解决了许多分析科学难题,日益发挥更重要的作用。     

使用高场非对称波形离子迁移谱（FAIMS）技术提高液相色谱-质谱（LC-MS）分析的选择性

对一些审查严格的应用领域,如制药工业等,方法的选择性至关重要.高场非对称波形离子迁移谱(FAIMS)技术可以有效提高方法的选择性.本文描述了这种与色谱和质谱正交的技术,并显示了在LC-MS流程中它能够显著提高实验室的产出率.     

LC-MS/MS和荧光偏振法监测环孢素A血药浓度的相关性研究

建立液相色谱-质谱（LC-MS/MS）监测环孢素A(CsA)血药浓度的方法,并与荧光偏振法（TDx）监测结果比较,进行统计学分析,考察2种方法的相关性。LC-MS/MS方法测定CsA血药浓度平均为（99.9±62.7） μg/L,小于TDx法测定的浓度平均值（199.7±129.1） μg/L,2种监测方法测定结果相关系数r平均为0.929,相关性较好,LC-MS/MS法和TDx法自身配对比值平均为（51.6±9.3）%,因此推测LC-MS/MS法可用于CsA血药浓度监测的治疗窗。LC-MS/MS法测定的浓度为CsA原型药物浓度,能更准确的反映原型药物在体内的准确浓度,更适用于日常血药浓度监测工作。     

高效液相色谱仪串联三重四级杆质谱法快速测定姜茶中的姜黄素

建立了高效液相色谱串联三重四级杆质谱法(LC-MS/MS)测定姜茶中的姜黄素的方法。对样品的前处理方法及LC-MS/MS分析条件进行了优化,样品以甲醇为提取溶剂,超声提取,LC-MS/MS多反应监测模式(MRM)进行测定。姜黄素在0.005~0.1μg/mL范围内均呈良好的线性关系,相关系数为0.999;检出限为1.0μg/kg。标准加标回收试验,姜黄素添加浓度分别为5.0,10.0,20.0μg/kg,平均回收率为92.5%~102.5%,相对标准偏差(RSD)2.0%~2.5%。方法简便、快速、溶剂用量少,可消除姜油带来的干扰,结果准确可靠,适合进行批量样品的测定。     

液相色谱-串联质谱生物分析方法的基质效应和对策

液相色谱-串联质谱（LC-MS/MS）法具有高灵敏度、高选择性、高通量等特点,已经成为生物分析的主流方法,广泛应用于新药发现和开发过程中新化学实体及其代谢物的定量分析。然而,由于生物样品基质成分复杂,共洗脱物质会影响分析物的离子化,使分析物的质谱响应增加或降低,从而影响LC-MS/MS分析方法的准确度和精密度。一般而言,离子抑制较离子增强更为常见。因此,在建立LC-MS/MS法时,需要对离子抑制进行评估和校正,并采用不同的策略消除或减少基质效应的影响。本文综述了生物样品分析中基质效应的来源和评估方法,重点介绍了克服基质效应的策略。引起基质效应的物质包括磷脂、盐类、尿素、代谢物等内源性物质和赋形剂、抗凝剂、固定相释放物质及降解产物等外源性物质。目前基质效应的评价方法主要有提取后加入法和柱后灌注法。克服基质效应的策略主要有使用稳定同位素内标,将极性药物衍生化,沉淀蛋白后稀释上清液,优化样品预处理方法、色谱和质谱条件等。结合本课题组的应用实例,重点阐述了建立LC-MS/MS生物分析方法时,为减少基质效应遇到的困难及解决方法。     

亲和超滤质谱技术在中药活性成分筛选中的研究进展

亲和超滤质谱技术是20世纪90年代中期发展起来的一种快速、简单、有效的药物小分子发现模式。该技术利用配体与受体之间特异性结合,通过超滤装置快速筛选活性小分子化合物,再结合液相色谱 质谱联用技术（LC-MS）,鉴定活性成分结构。亲和超滤质谱技术集药物活性成分筛选、结构鉴定于一体,尤其适用于从复杂体系中筛选潜在的活性小分子化合物。近年来,针对中药发挥药理作用具有多组分、多靶点的重要特点,亲和超滤质谱技术已被广泛用于从中药提取物中筛选与特定蛋白靶点相结合的小分子活性物质,对阐明中药药效的物质基础和以活性成分作为先导化合物的新药开发具有重要意义,是对传统药物发现方法的有利补充。本工作综述了该技术在中药活性成分筛选中的原理、特点、应用进展,以及对未来的展望。     

现代分析技术在中药质量控制中的应用

介绍色谱法、光谱法、核磁共振波谱、质谱及其联用技术、DNA分子诊断技术、X射线衍射法等几种现代分析方法在中药质量控制中的应用。     

Mass spectrometry in grape and wine chemistry. Part I: polyphenols

Mass spectrometry, had and still has, a very important role for research and quality control in the viticulture and enology field, and its analytical power is relevant for structural studies on aroma and polyphenolic compounds. Polyphenols are responsible for the taste and color of wine, and confer astringency and structure to the beverage. The knowledge of the anthocyanic structure is very important to predict the aging attitude of wine, and to attempt to resolve problems about color stability. Moreover, polyphenols are the main compounds related to the benefits of wine consumption in the diet, because of their properties in the treatment of circulatory disorders such as capillary fragility, peripheral chronic venous insufficiency, and microangiopathy of the retina. Liquid Chromatography-Mass Spectrometry (LC-MS) techniques are nowadays the best analytical approach to study polyphenols in grape extracts and wine, and are the most effective tool in the study of the structure of anthocyanins. The MS/MS approach is a very powerful tool that permits anthocyanin aglycone and sugar moiety characterization. LC-MS allows the characterization of complex structures of grape polyphenols, such as procyanidins, proanthocyanidins, prodelphinidins, and tannins, and provides experimental evidence for structures that were previously only hypothesized. The matrix-assisted-laser-desorption-ionization-time-of-flight (MALDI-TOF) technique is suitable to determine the presence of molecules of higher molecular weight with high accuracy, and it has been applied with success to study procyanidin oligomers up to heptamers in the reflectron mode, and up to nonamers in the linear mode. The levels of resveratrol in wine, an important polyphenol well-known for its beneficial effects, have been determined by SPME and LC-MS, and the former approach led to the best results in terms of sensitivity.     

Residue analysis of 500 high priority pesticides: Better by GC–MS or LC–MS/MS?

This overview evaluates the capabilities of mass spectrometry (MS) in combination with gas chromatography (GC) and liquid chromatography (LC) for the determination of a multitude of pesticides. The selection of pesticides for this assessment is based on the status of production, the existence of regulations on maximum residue levels in food, and the frequency of residue detection. GC-MS with electron impact (EI) ionization and the combination of LC with tandem mass spectrometers (LC-MS/MS) using electrospray ionization (ESI) are identified as techniques most often applied in multi-residue methods for pesticides at present. Therefore, applicability and sensitivity obtained with GC-EI-MS and LC-ESI-MS/MS is individually compared for each of the selected pesticides. Only for one substance class only, the organochlorine pesticides, GC-MS achieves better performance. For all other classes of pesticides, the assessment shows a wider scope and better sensitivity if detection is based on LC-MS.     

液相色谱-串联质谱检测兽药残留中的基质效应研究进展

液相色谱-串联质谱技术作为强有力的分析工具已被广泛应用于多个领域,但其检测中的基质效应对测定结果准确性的影响需引起重视。本文综述了液相色谱-串联质谱分析测定中基质效应的来源、重要性、产生的可能机制、影响因素、评价及消除和（或）补偿基质效应的方法,重点概括了典型兽药残留检测中应对基质效应的方法进展。     

Control of pesticide residues by liquid chromatography-mass spectrometry to ensure food safety

Liquid chromatography-mass spectrometry (LC-MS) has become an invaluable technique for the control of pesticide residues to ensure food safety. After an introduction about the regulations that highlights its importance to meet the official requirements on analytical performance, the different mass spectrometers used in this field of research, as well as the LC-MS interfaces and the difficulties associated with quantitative LC-MS determination, are discussed. The ability to use practical data for quantifying pesticides together with the option of obtaining structural information to identify target and non-target parent compounds and metabolites are discussed. Special attention is paid to the impact of sample preparation and chromatography on the ionization efficiency of pesticides from food. The last section is devoted to applications from a food safety point of view. (c) 2006 Wiley Periodicals, Inc.     

液相色谱-质谱/质谱联用技术新进展及应用

简介了液相色谱-质谱/质谱联用技术的新进展,综述了近年来该技术的应用及其发展前景。     

Time of flight mass spectrometry applied to the liquid chromatographic analysis of pesticides in water and food

Liquid chromatography coupled to mass spectrometry (LC-MS) is an excellent technique to determine trace levels of polar and thermolabile pesticides and their degradation products in complex matrices. LC-MS can be equipped with several mass analyzers, each of which provides unique features capable to identify, quantify, and resolve ambiguities by selecting appropriate ionization and acquisition parameters. We discuss in this review the use of LC coupled to (quadrupole) time-of-flight mass spectrometry (LC-(Q)ToF-MS) to determine the presence of target and non-target pesticides in water and food. This technique is characterized by operating at a resolving power of 10,000 or more. Therefore, it gives accurate masses for both parent and fragment ions and enables the measurement of the elemental formula of a compound achieving compound identification. In addition, the combination of quadrupole-ToF permits tandem mass spectrometry, provides more structural information, and enhances selectivity. The purpose of this article is to provide an overview on the state of art and applicability of liquid chromatography time-of-flight mass spectrometry (LC-ToF-MS), and liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QToF-MS) for the analysis of pesticides in environmental matrices and food. The performance of such techniques is depicted in terms of accurate mass measurement, fragmentation, and selectivity. The final section is devoted to describing the applicability of LC-(Q)ToF-MS to routine analysis of pesticides in food matrices, indicating those operational conditions and criteria used to screen, quantify, and identify target and "suspected" pesticides and their degradation products in water, fruits, and vegetables. The potential and future trends as well as limitations of LC-(Q)ToF-MS for pesticide monitoring are highlighted.