除草剂阿特拉津气质联用色谱的测定

阿特拉津又名莠去津,是由瑞士Basel Geigy化学公司开发的一种广泛使用的均三嗪类除草剂,用于玉米、高粱、甘蔗、果园、草皮场和林地等的阔叶杂草和禾草的防除。农田中大量投放的水溶性较强的阿特拉津也是在各国河流、小溪等水体中检出率最高的除草剂。实验表明,长期低剂量的阿特拉津作用有诱发人类染色体破裂与生殖系统疾病的危险,也是水生动物种类大量减少的主要原因。     

SPME-GC/MS方法分析水样中偏二甲肼降解产物

本文使用SPME-GC/MS技术分析不同时间水中偏二甲肼降解产物浓度变化规律,并得到SPME对偏二甲肼降解产物的最佳萃取条件。该方法快速、便捷,具有时间短、灵敏度高、操作简便等优点。     

气质联用技术在水环境突发性污染事件中的应用

本文对气质联用技术在水环境突发性污染事件中的应急监测进行了研究,具体讨论了水中挥发性和半挥发性有机污染物的快速检测方法,结果为：以吹扫捕集-气质联用对水中62种挥发性有机物的检测时间小于25min,检测限在0.16～0.63μg/L,回收率在74.1%～115.9%;以液液微萃取-气质联用对水中63种半挥发性有机物的检测时间小于50min,方法检测限在0.073～3.1μg/L,回收率在34.2%～135.5%。此外还讨论了气质联用技术在应用中的局限性。     

气质联用法监测三氯蔗糖的合成

采用单酯化法合成三氯蔗糖,并建立了气相色谱-质谱(GC/MS)检测合成过程中各重要组分的方法。采用HP-5毛细管气相色谱柱(30 m×0.25 mm×0.25μm),以电子轰击为电离方式,选取最佳实验条件对蔗糖、蔗糖-6-乙酯、三氯蔗糖进行硅烷化衍生,并对其进行定性、定量检测。该检测方法用于监测单酯化法合成三氯蔗糖的工艺过程,取得了理想效果。     

气质联用法测定花色蛤中扑草净残留量

本文研究建立了花色蛤中扑草净含量的气质联用测定方法。样品用正己烷提取后,经硅藻土固相萃取柱净化后,注入气质联用仪中进行检测。经弱极性色谱柱分离,EI源离子化,以及sim方式对样品中的扑草净残留量进行定性与定量分析。该方法测定结果的相对标准偏差小于6％（n=6）,平均回收率大于74％,线性范围为0．05—1μg／ml,最低检出限为0．00022mg／kg。     

气相色谱和质谱联用测定原始细菌Natronobacterium ma gadii中不活泼极性甘油脂的结构

本文报导了气相色谱和质谱联用利用电子电离 (EI)和化学电离 (CI)两种模式测定Natronobacteriummagadii中主要类脂的全甲基化衍生物的方法。实验数据显示 ,Natronobacteriummagadii和一般的原始细菌不一样 ,除含有传统的C2 0-C2 0 类脂甘油醚外 ,还存在一种不太常见的C2 0 -C2 5的类脂甘油醚。EI给出的碎片峰和CI给出的准分子离子峰使我们确证了C2 0 -C2 2 和C2 0 -C2 5结构的存在。质谱电子轰击法和化学电离法已成功地应用于测定原始细菌中主要不活泼类脂的烷基链结构 ,特别是电子轰击法的硬电离 ,获得了众多的烷基碎片峰 ,从而弥补了软电离ESI和APCI未能出现烷基碎片峰的不足。值得注意的是EI质谱显示出烷基是以直链 ,而并非有规律地按叔碳原子排列的支链 ,尽管这种说法尚需进一步确证     

偏二甲肼中颗粒物的分析表征

采用热重与差热分析、裂解质谱分析、元素分析、X射线衍射分析等多种分析手段 ,对偏二甲肼中的颗粒物和絮状物的成分与结构进行分析表征 ,并对颗粒物和絮状物的来源进行分析     

顶空-气质联用法测定潲水油中的挥发性有机化合物

为了寻找煎炸油、潲水油和正常食用植物油的成分差别,采用静态顶空与气质联用法分析潲水油样品和食用植物油样品中的挥发性成分。结果表明,食用植物油氧化变质的二级产物为醛类物质,脂肪酸小分子是由植物油二级氧化产物进一步氧化而得;潲水油中已存在大量的氧化产物脂肪酸小分子,说明潲水油已过度氧化。采用顶空-气质联用法找到了潲水油与正常食用植物油主要差别成分：乙酸、丙酸、丁酸、戊酸、己酸小分子脂肪酸中一种、两种或者多种。其中丁酸是最重要的特征性指标,在丁酸检出而其他脂肪酸未检出的情况下也可以判定待测油样为地沟油。     

固相微萃取气质联用法测定地表水中四乙基铅

本研究优化了地表水中四乙基铅的固相微萃取(SPME)气质联用法,在30 ℃顶空萃取温度、100 μm聚二甲基硅氧烷（PDMS）萃取头等SPME条件下,提高了方法的检出限,缩短了前处理时间。在3 min萃取时间内,四乙基铅的检出限可达1.24 ng/L,精密度在3.4%以下。实际地表水样品加标回收率在84.2%~98.8%之间,废水样品加标回收率在66.0%~102%之间。该方法操作简便、环境友好,能满足集中式生活饮用水源地水质监测的要求,也可用于部分废水样品的测定。     

气质联用仪测定汽油中含氧化合物、苯和甲苯的含量

利用选择离子法（SIM）对汽油中含氧化合物、苯和甲苯进行定量分析,可以简化分析步骤,缩短分析时间,有效消除汽油中复杂成分对目标组分分析结果的影响,提高了分析结果的准确性。15种组分标准曲线的线性相关系数均大于0.998 8,最低检测限为2~5 μg•g^-1,回收率为90%~103%,保留时间相对标准偏差小于0.5%,峰面积相对标准偏差小于11.05%。     

采用裂解气相色谱/质谱法剖析船用沥青

采用裂解气相色谱/质谱联用方法对三种不同类型的沥青进行分析研究,选择在550℃裂解,其裂解产物通过SE-54高效毛细管柱分离和质谱鉴定,提供了有关这三种沥青各自结构的特征信息。通过碎片峰相对峰面积的比较,可区分不同产地的石油沥青样品。具有样品无需前处理,用量少,谱图直观,对应性强,灵敏度高等特点。     

热裂解气相色谱/质谱联用快速分析聚合物中添加剂

热裂解气相色谱/质谱(Py-GC/MS)联用技术可以省去复杂的前处理,直接对聚合物中有机添加剂进行分析。本文分别对Py-GC/MS在易挥发性小分子添加剂,难挥发性大分子添加剂定性分析及添加剂定量分析中的应用进行了介绍。     

Liquid chromatography combined with mass spectrometry for 13C isotopic analysis in life science research

Among the different disciplines covered by mass spectrometry, measurement of (13)C/(12)C isotopic ratio crosses a large section of disciplines from a tool revealing the origin of compounds to more recent approaches such as metabolomics and proteomics. Isotope ratio mass spectrometry (IRMS) and molecular mass spectrometry (MS) are the two most mature techniques for (13)C isotopic analysis of compounds, respectively, for high and low-isotopic precision. For the sample introduction, the coupling of gas chromatography (GC) to either IRMS or MS is state of the art technique for targeted isotopic analysis of volatile analytes. However, liquid chromatography (LC) also needs to be considered as a tool for the sample introduction into IRMS or MS for (13)C isotopic analyses of non-volatile analytes at natural abundance as well as for (13)C-labeled compounds. This review presents the past and the current processes used to perform (13)C isotopic analysis in combination with LC. It gives particular attention to the combination of LC with IRMS which started in the 1990's with the moving wire transport, then subsequently moved to the chemical reaction interface (CRI) and was made commercially available in 2004 with the wet chemical oxidation interface (LC-IRMS). The LC-IRMS method development is also discussed in this review, including the possible approaches for increasing selectivity and efficiency, for example, using a 100% aqueous mobile phase for the LC separation. In addition, applications for measuring (13)C isotopic enrichments using atmospheric pressure LC-MS instruments with a quadrupole, a time-of-flight, and an ion trap analyzer are also discussed as well as a LC-ICPMS using a prototype instrument with two quadrupoles.     

Multiclass mycotoxin analysis in food, environmental and biological matrices with chromatography/mass spectrometry

Mold metabolites that can elicit deleterious effects on other organisms are classified as mycotoxins. Human exposure to mycotoxins occurs mostly through the intake of contaminated agricultural products or residues due to carry over or metabolite products in foods of animal origin such as milk and eggs, but can also occur by dermal contact and inhalation. Mycotoxins contained in moldy foods, but also in damp interiors, can cause diseases in humans and animals. Nephropathy, various types of cancer, alimentary toxic aleukia, hepatic diseases, various hemorrhagic syndromes, and immune and neurological disorders are the most common diseases that can be related to mycotoxicosis. The absence or presence of mold infestation and its propagation are seldom correlated with mycotoxin presence. Mycotoxins must be determined directly, and suitable analytical methods are necessary. Hundreds of mycotoxins have been recognized, but only for a few of them, and in a restricted number of utilities, a maximum acceptable level has been regulated by law. However, mycotoxins seldom develop alone; more often various types and/or classes form in the same substrate. The co-occurrence might render the individual mycotoxin tolerance dose irrelevant, and therefore the mere presence of multiple mycotoxins should be considered a risk factor. The advantage of chromatography/mass spectrometry (MS) is that many compounds can be determined and confirmed in one analysis. This review illustrates the state-of-the-art of mycotoxin MS-based analytical methods for multiclass, multianalyte determination in all the matrices in which they appear. A chapter is devoted to the history of the long-standing coexistence and interaction among humans, domestic animals and mycotoxicosis, and the history of the discovery of mycotoxins. Quality assurance, although this topic relates to analytical chemistry in general, has been also examined for mycotoxin analysis as a preliminary to the systematic literature excursus. Sample handling is a crucial step to devise a multiclass analytical method; so when possible, it has been treated separately for a better comparison before tackling the instrumental part of the whole analytical method. This structure has resulted sometimes in unavoidable redundancies, because it was also important to underline the interconnection. Most reviews do not deal with all the possible mycotoxin sources, including the environmental ones. The focus of this review is the analytical methods based on MS for multimycotoxin class determination. Because the final purpose to devise multimycotoxin analysis should be the assessment of the danger to health of exposition to multitoxicants of natural origin (and possibly also the interaction with anthropogenic contaminants), therefore also the analytical methods for environmental relevant mycotoxins have been thoroughly reviewed. Finally, because the best way to shed light on actual risk assessment could be the individuation of exposure biomarkers, the review covers also the scarce literature on biological fluids.     

VTMS等离子体聚合物的裂解色谱—质谱分析

本文应用裂解色谱-质谱(PGC/MS)分析和鉴定了乙烯基三甲基硅烷(VTMS)分别与Ar、N_2苯(Bz)混合体系等离子体聚合物的裂解碎片。质谱分析结果表明VTMS/Ar、VTMS/N_2以及VTMS/Bz三体系等离子体聚合物的裂解产物分别由8个、10个和16个主要碎片组成。根据PGC-MS结果讨论了VTMS等离子体聚合物的化学结构,并提出了VTMS等离子体聚合机理。     

Matrix-free methods for laser desorption/ionization mass spectrometry

Matrix assisted laser desorption/ionization (MALDI) is a soft ionization mass spectrometric method that has become a preeminent technique in the analysis of a wide variety of compounds including polymers and proteins. The main drawback of MALDI is that it is difficult to analyze low molecular weight compounds (<1,000 m/z) because the matrix that allows MALDI to work interferes in this mass range. In recent years there has been considerable interest in developing laser desorption/ionization (LDI) techniques for the analysis of small molecules. This review examines the approaches to matrix-free LDI mass spectrometry including desorption/ionization on silicon (DIOS), sol-gels, and carbon-based microstructures. For the purposes of this review matrix-free methods are defined as those that do not require matrix to be mixed with the analyte and therefore does not require co-crystallization. The review will also examine mechanisms of ionization and applications of matrix-free LDI-MS.     

鱼油中二十二碳六烯酸的气相色谱-质谱分析

建立了用毛细管柱气相色谱-质谱方法（GC—MS）分析鱼油中二十二碳六烯酸（DHA）的分析方法。鱼油中的DHA用质谱进行定性确证分析,同时通过总离子流色谱图对鱼油中的DHA含量进行定量分析。GC—MS定量分析鱼油中的DHA在30-4000μg／mL浓度范围内有较好的线性关系,线性方程为Y=36188X-106,相关系数为R^2=0．9984。本方法DHA添加水平为1．0％时回收率为85．0％～102．0％,方法可靠实用,结果准确。本文介绍了在方法的实际操作过程中的注意事项。使用该方法分析一种市售鱼油中DHA含量为19．7％。     

Collagen analysis with mass spectrometry

Mass spectrometry-based techniques can be applied to investigate collagen with respect to identification, quantification, supramolecular organization, and various post-translational modifications. The continuous interest in collagen research has led to a shift from techniques to analyze the physical characteristics of collagen to methods to study collagen abundance and modifications. In this review, we illustrate the potential of mass spectrometry for in-depth analyses of collagen.     

吹扫捕集-气相色谱/质谱法测定不同饼干中挥发性成分

本研究将吹扫捕集进样技术与气相色谱/质谱法相结合应用于5种市售饼干样品中挥发性组分的分析,分离并鉴定39种挥发性化合物。所鉴定出的物质中,要包括醇类、醛类、酮类、烷烃类、酯类及杂环类等化合物。在5种饼干样品定性分析化合物中,TIC图峰面积比均较大的化合物主要为2-甲基丁醛、异戊醛、苯甲醛、己醛等芳香醛类物质。     

Tandem mass spectrometry strategies for phosphoproteome analysis

Protein phosphorylation is involved in nearly all essential biochemical pathways and the deregulation of phosphorylation events has been associated with the onset of numerous diseases. A multitude of tandem mass spectrometry (MS/MS) and multistage MS/MS (i.e., MSⁿ) strategies have been developed in recent years and have been applied toward comprehensive phosphoproteomic analysis, based on the interrogation of proteolytically derived phosphopeptides. However, the utility of each of these MS/MS and MSⁿ approaches for phosphopeptide identification and characterization, including phosphorylation site localization, is critically dependant on the properties of the precursor ion (e.g., polarity and charge state), the specific ion activation method that is employed, and the underlying gas‐phase ion chemistries, mechanisms and other factors that influence the gas‐phase fragmentation behavior of phosphopeptide ions. This review therefore provides an overview of recent studies aimed at developing an improved understanding of these issues, and highlights the advantages and limitations of both established (e.g., CID) and newly maturing (e.g., ECD, ETD, photodissociation, etc.) yet complementary, ion activation techniques. This understanding is expected to facilitate the continued refinement of existing MS/MS strategies, and the development of novel MS/MS techniques for phosphopeptide analysis, with great promise in providing new insights into the role of protein phosphorylation on normal biological function, and in the onset and progression of disease. © 2011 Wiley Periodicals, Inc., Mass Spec Rev 30:600–625, 2011