1-0-烯丙基-a-L-鼠李糖苷类化合物的快原子轰击质谱研究

快原子轰击质谱技术,在分析极性、难挥发化合物方面有很强的优越性,广泛应用于糖类化合物的分析、检测。我们对一系列1-0-烯丙基-a-L-鼠李糖及其它糖类化合物进行质谱检测后,发现1-0-烯丙基-a-L-鼠李糖类合物的快原子轰击质谱中易出现[M-H]^ 离子峰,而与一般化合物在FAB谱中易出现[M H]^ 离子峰不同。我们对此提出一质谱裂解机理,并总结了此类化合物的FAB质谱规律。     

毛细管电泳-质谱联用技术及其在药物和生物分析中的应用

毛细管电泳-质谱（CE-MS）联用技术是在液相色谱-质谱联用技术基础上发展起来的一项新型分析技术,它结合了毛细管电泳具有的分离效率高、分离速度快、样品消耗量少以及质谱检测具有的高灵敏度和强结构解析能力等优点,现已成为倍受分析化学工作者关注的新型微量分析技术。目前,CE-MS联用技术是中药有效成分分析,体内药物分析以及生物样品,如氨基酸、多肽、蛋白质和多糖等分析的重要手段。本文对CE-MS联用技术中同轴鞘流及无鞘流纳流电喷雾等几种接口装置的研究进展,CE-MS技术在中药活性成分分析及多级质谱结构解析以及氨基酸、多肽及蛋白质等生物样品分析中的应用研究进行了综述,并对该技术的发展进行了展望。     

基质辅助激光解吸电离-飞行时间质谱在高分子研究中的应用

在质谱学的发展过程中,如何获得大分子物质的质谱信息一直是最具有挑战性的课题。在过去的20年里,大分子的质谱研究取得了很大进展,发展出快原子轰击（FAB）、液质联用（LC-MS）、基质辅助激光解吸电离-飞行时间质谱（MALDI-TOF）以及质谱/质谱串联（MALDI-TOF/TOF）等技术,并在生物大分子的结构测定、高聚物的结构及端基测定、共聚物的序列结构及组成等方面对高分子科学的发展作出了突出贡献。本文结合具体实例着重介绍了MALDI-TOF MS在大分子分析中的技术优势及应用     

MassWorksTM与气相色谱-质谱联用分析洋甘菊精油成分

采用气相色谱-质谱联用(GC/MS)技术,结合MassWorks^TM质谱解析软件,对产自甘肃省永登县的洋甘菊(Chamomila recutita L.)精油成分进行分析。对两种不同极性的色谱柱进行分离比较实验,确定了适合于洋甘菊精油分离分析的色谱条件和质谱条件,解析并确定出精油中的35种化合物。MassWorks软件在低分辨率质谱上可对化合物分子质量实现精确测量,为低分辨四极杆质谱确定化合物的元素组成和解析化合物结构提供重要依据,同时也为植物精油的成分分析提供新的技术手段。     

芬太尼类新精神活性物质的质谱特征研究

采用气相色谱-质谱(GC/MS)法和超高效液相色谱-串联四极杆飞行时间质谱(UPLC-Q-TOF MS)法对2015~2016年国内检测发现的8种芬太尼类新精神活性物质进行分析。GC/MS分析采用电子轰击源(EI)模式采集数据,UPLC-Q-TOF MS分析采用电喷雾正离子碰撞诱导解离（CID）模式采集数据。通过总结该类物质在两种模式下获得的碎片离子与分子结构的关系,推测其可能的碎裂途径,并归纳了通过谱图推导未知芬太尼类新精神活性物质结构的方法,结果可为该类物质的鉴定提供参考。     

基于特征性离子快速筛查和识别色胺类新精神活性物质

采用气相色谱-质谱(GC-MS)法和超高效液相色谱-串联四极杆飞行时间质谱(UPLC-QTOF MS)法分析2015~2019年国内检测发现的11种色胺类新精神活性物质。GC-MS在电子轰击源(EI)模式下采集数据,UPLC-QTOF MS在电喷雾正离子(ESI⁺)-碰撞诱导解离(CID)模式下采集数据。通过对目标物质谱裂解产生的特征性离子进行分析,推测了色胺类新精神活性物质可能的碎裂途径,建立了一种快速、便捷筛查和识别色胺类新精神活性物质的方法。     

脂肪醇聚氧乙烯醚类非离子表面活性剂的质谱解析及色谱分离研究

采用液相色谱-四极杆串联质谱技术分离检测非表面活性剂十二醇聚氧乙烯醚类、十六醇聚氧乙烯醚类和十八醇聚氧乙烯醚类物质。本实验通过对7种脂肪醇聚氧乙烯醚标准品的质谱解析,得出此类物质的质谱解析规律,并推断出标准品中所包含的41种脂肪醇聚氧乙烯醚的组分。通过中性丢失、母离子扫描和子离子扫描对质谱规律进行验证。在电喷雾正离子(ESI)扫描模式下,对此类物质的质谱解析和裂解规律进行了研究。本研究建立了简便、快速的分离方法,并鉴定出不同碳链数和不同加成数的混合脂肪醇聚氧乙烯醚类非离子表面活性剂的单个组分的检测方法,为环境水体中此类物质的检测提供了依据。     

用毛细管色谱—化学电离质谱法分析塑料添加剂

在塑料中加入少量的添加剂就能大大地改善塑料的性能。因此,在许多未知塑料试样的剖析中,微量添加剂的分离和鉴定是十分重要的。目前,在多组份有机混合物的微量分析方面,色谱——质谱联用是最有用的方法之一。然而,许多常用的塑料添加剂都是长链的脂肪族酯类和胺类化合物;在它们的电子轰击质谱上,分子离子峰不但不出现,而且高质量端的离子峰也很少。因此,仅靠电子轰击质谱,难于确定它们的结构。     

全氟甲基乙烯基醚的杂质分析

本文采用色谱分离、质谱检定的方法,对全氟甲基乙烯基醚在其制备过程中产生的微量杂质,进行了定性研究,确定了它们的化学组成,它们分别为氮、二氧化碳、四氟乙烯、双-三氟甲基过氧化物和一氯三氟乙烯,此外尚有微量的全氟甲醚。实验所用仪器,大量的色谱工作是在北京分析仪器厂的产品SP-2305(全型)上进行。色-质检定是用西德Varian公司产品MaT 112型小型双聚焦电子轰击源色谱-质谱计,该仪器配套的数据处理系统是该公司的SS 101MS型。色谱-质谱试验所选用的条件为;色谱柱长:3m,φ=4mm;担体:GDX-104 60—80     

色质联用技术的进步与农药多残留分析方法的发展（之一）

气相色谱-质谱联用技术是农药多类多残留检测分析方法发展的起点,液相色谱-质谱联用技术的发展给极性农药、热不稳定性农药及其代谢物的检测创造了条件,高选择性、高灵敏度、高通量的色谱-串联质谱技术创建了农药的多残留检测方法。本文回顾了色质联用技术的进步及其在农药多残留分析方法发展过程中的重要作用。     

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.     

色谱-质谱法在水环境监测中的应用

本文综述色谱和质谱联用技术在水环境检测中的应用,作为一种检测手段,其灵敏度高,定性的专一性强,定量再现性好,能够给出被测物质许多结构和含量的信息,解决环境监测中背景复杂、干扰多、被测物质浓度小等问题。     

美国应用生物系统公司串联液质系统--食品安全的卫士

高效液相色谱-串联质谱联用技术在近几年发展迅猛，已成为在复杂体系中进行微量组分的筛选、定性和定量极其可靠、快速和准确的分析手段。受到了学术界和分析测试行业的普遍青睐，并在生命科学、药学、医学、环境与健康等领域得到广泛应用。本文论述了美国应用生物系统公司串联液质系统用于食品安全领域关键的技术要点，比如三级四极杆质谱技术擅长快速定量分析，就好比是“长了眼睛的分析检测技术”，不需要液相色谱的完全分离，提高了方法建立与分析检测的速度，并拓展了分析测试的检测下限；同时。线性离子阱技术可提供高质量的化合物碎片离子全扫描图谱以及多级串联质谱功能，大大增强了系统的定性功能。而两种技术的完美组合即“串联四极杆-线性离子阱融合质谱技术”不仅出色地完成高灵敏度、高选择性的定量分析，同时可以获得增强性化和物结构碎片图谱，使定性、定量工作一次完成，大大提高了食品安全中分析检测的通量．本文介绍了这种新技术的基本原理及其在食品安全中的经典应用。     

Direct-EI in LC-MS: towards a universal detector for small-molecule applications

This review article will give an up-to-date and exhaustive overview on the efficient use of electron ionization (EI) to couple liquid chromatography and mass spectrometry (LC-MS) with an innovative interface called Direct-EI. EI is based on the gas-phase ionization of the analytes, and it is suitable for many applications in a wide range of LC-amenable compounds. In addition, thanks to its operating principles, it prevents unwelcome matrix effects (ME). In fact, although atmospheric pressure ionization (API) methodologies have boosted the use of LC-MS, the related analytical methods are sometime affected by inaccurate quantitative results, due to unavoidable and unpredictable ME. In addition, API's soft ionization spectra always demand for costly and complex tandem mass spectrometry (MS/MS) instruments, which are essential to acquire an "information-rich" spectrum and to obtain accurate quantitative information. In EI a one-stage analyzer is sufficient for a qualitative investigation and MS/MS detection is only used to improve sensitivity and to cut chemical noise. The technology illustrated here provides a robust and straightforward access to classical, well-characterized EI data for a variety of LC applications, and readily interpretable spectra for a wide range of areas of research. The Direct-EI interface can represent the basis for a forthcoming universal LC-MS detector for small molecules.     

敞开式离子化质谱技术研究进展

军事、公共安全和应急救援等对现场、实时、准确、快速检测技术提出了迫切需求。敞开式离子化质谱技术可以现场直接分析样品,具有简单、快速、无需样品前处理、可分析多种相态物质的特点。本文总结了基于激光、等离子体和电喷雾原理的敞开式离子化技术的研究进展,介绍了敞开式离子化质谱技术在化学战剂、生物和爆炸物检测领域的应用,并对敞开式离子化质谱技术面临的问题和未来研究方向进行了总结与展望。     

Mass spectrometry for the study of protein glycation in disease

The structural elucidation of advanced glycation end-product (AGE)-modified proteins and quantitative analysis of free AGEs have been successfully performed, by use of mass spectrometry (MS) in plasma and tissues of patients with AGE-related diseases, such as diabetes mellitus, uremia, cataract, and liver cirrhosis. Matrix-assisted laser desorption/ionization (MALDI)-MS made it possible to directly analyze the AGE-modified proteins such as albumin and IgG. However, because the direct structural analysis of intact AGE-modified proteins is often not easy due to the formation of broad and poorly resolved peaks, peptide mapping after enzymatic hydrolysis was introduced into the analysis of AGE-modified proteins and the site-specific analysis of defined AGEs by MALDI-MS. Liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS) has been employed not only for the structural elucidation of enzymatically hydrolyzed AGEs-modified peptides but also for simultaneous quantification of free AGEs in plasma and tissues of patients. Based on many studies that use MS for the analysis of AGEs, there is no doubt as to the important role of protein-linked AGEs in several diseases.     

中药多成分药代动力学分析技术研究进展

中药多成分药代动力学是中医药理论和作用机制阐明的重要研究内容。如何全面、准确地描述中药复杂成分在体内的药代动力学过程，诠释中药多成分、多靶标、多途径的特点，需要强有力的分析技术支撑。近年来，多种高通量、快速、自动化的前处理技术显著提升了中药体内外多成分的分离提取效率；色谱、质谱分析技术蓬勃发展，推动了中药体内外多成分的快速鉴别和全面、准确定量；质谱成像等新兴技术不断涌现，为中药多成分药代动力学研究提供了新的分析平台和研究手段。本文综述了近10年来中药多成分药代动力学研究分析技术的进展和应用，并对其前景进行展望。     

食品中三聚氰胺检测方法的研究进展

本文综述了近年来食品中三聚氰胺的检测方法,主要包括气相色谱一质谱联用检测方法（GC—MS）、超高效液相色谱与质谱联用、固相萃取与高效液相色谱联用等,并指出气质联用（GC-MS）技术利用了色谱的高分离能力和质谱的高鉴别特性,可以对比较复杂的混合样品进行分离、定性、定量分析一次完成,是一种比较完美的现代分析方法。超高液相色谱一串联质谱法具有更快的分析速度、更高的分离能力和灵敏度,可以满足食品中三聚氰胺残留量的快速检测要求。     

铀材料分析中的无机与同位素质谱法研究进展

综述了近年来中国工程物理研究院材料研究所应用无机与同位素质谱法进行铀材料分析的相关研究工作。在痕量铀同位素测量方面,发展了一种以氧化石墨烯作为电离增强剂的热电离质谱制样技术,显著增强了电离效率。在铀材料中杂质元素分析方面,开发了基于微流控芯片与电感耦合等离子体质谱联用的在线分离、分析方法,提高了分析的自动化程度。在金属铀中杂质元素的辉光放电质谱直接测定方面,基于相对灵敏度因子影响因素的研究基础,获得了一套普适性的相对灵敏度因子,实现了缺乏基体匹配标准物质时的准确测定。利用飞行时间-二次离子质谱法研究了铀及铀合金的偏析行为、夹杂物的表征、氢化/氧化腐蚀行为,为铀材料研究提供了表征手段。最后,对无机与同位素质谱法用于铀材料分析的发展前景进行了展望。     

Mass spectrometry-based methods for the advanced characterization and structural analysis of lignin: A review

Lignin is currently one of the most promising biologically derived resources, due to its abundance and application in biofuels, materials and conversion to value aromatic chemicals. The need to better characterize and understand this complex biopolymer has led to the development of many different analytical approaches, several of which involve mass spectrometry and subsequent data analysis. This review surveys the most important analytical methods for lignin involving mass spectrometry, first looking at methods involving gas chromatography, liquid chromatography and then continuing with more contemporary methods such as matrix assisted laser desorption ionization and time-of-flight-secondary ion mass spectrometry. Following that will be techniques that directly ionize lignin mixtures—without chromatographic separation—using softer atmospheric ionization techniques that leave the lignin oligomers intact. Finally, ultra-high resolution mass analyzers such as FT-ICR have enabled lignin analysis without major sample preparation and chromatography steps. Concurrent with an increase in the resolution of mass spectrometers, there have been a wealth of complementary data analyses and visualization methods that have allowed researchers to probe deeper into the “lignome” than ever before. These approaches extract trends such as compound series and even important analytical information about lignin substructures without performing lignin degradation either chemically or during MS analysis. These innovative methods are paving the way for a more comprehensive understanding of this important biopolymer, as we seek more sustainable solutions for our human species’ energy and materials needs.