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Vinyl chloride analysis with Solid Phase Microextraction (SPME)/GC/MS applied to analysis in materials and aqueous samples 固相微萃取(SPME)/气相色谱/质谱法分析氯乙烯,适用于材料和水样的分析
Pub Date : 2000-12-01 DOI: 10.1051/ANALUSIS:2000165
R. Charvet, C. Cun, P. Leroy
The increasing use of plastics in our society makes the vinyl chloride a potential source of pollution for environment. Related to its toxicity and presence in the environment, the new European Directive for drinking water quality includes now a limit for its concentration in drinking water. Currently a government needs new analytical methods to analyse this pollutant. T his study concerns the optimization of the headspace solid-phase microextraction (HS-SPME) combined with gas chromatography- ion trap mass spectrometry for the vinyl chloride analysis in liquid and solid samples. The Carboxen PDMS (Polydimethylsiloxane) 75 µm fibre allows a limit of detection of 50 ppt and 100 ppt as a limit of quan- tification in linearity and repeatability conditions useful for control analysis. Moreover, the excellent affinity between this fibre and the molecule of interest makes the use of little volumes of samples possible. Each parameter had been optimized to obtain the best sensibility. This method has also been applied to materials.
在我们的社会中塑料的使用越来越多,使得氯乙烯成为一个潜在的环境污染源。与它的毒性和在环境中的存在有关,新的欧洲饮用水质量指令现在包括了饮用水中它的浓度限制。目前,政府需要新的分析方法来分析这种污染物。本研究对顶空固相微萃取(HS-SPME)结合气相色谱-离子阱质谱法分析液体和固体样品中的氯乙烯进行了优化。Carboxen PDMS(聚二甲基硅氧烷)75µm纤维允许检测限为50 ppt和100 ppt,作为线性和可重复性条件下的全化限制,对控制分析有用。此外,这种纤维和感兴趣的分子之间的良好亲和力使得使用小体积的样品成为可能。对各参数进行了优化,以获得最佳的灵敏度。这种方法也被应用于材料。
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引用次数: 9
Determination of volatile organic compounds in coal, fly ash and slag samples by direct thermal desorption/GC/ms 直接热解吸/GC/ms法测定煤、粉煤灰和矿渣样品中的挥发性有机物
Pub Date : 2000-12-01 DOI: 10.1051/ANALUSIS:2000161
G. Fernández-Martínez, P. López‐Mahía, S. Muniategui-Lorenzo, D. Prada-Rodríguez
This work proposes a method for quantifying volatile organic compounds (VOCs) in coal, fly ash and slag, coming from coal-fired power stations, using direct thermal desorption coupled with gas chromatography (GC) and mass spectrometry (MS) detection. The described method requires practically no sample handling and is precise and sensitive. Aromatic and aliphat ic hydrocarbons (benzene, toluene, alkylbenzes, heptane and octane) are the most abundant compounds in these solid samples, coal samples presenting higher levels than fly ash and slag. Other compounds (acids, ketones, aldehydes, limonene, etc.) were identi- fied by mass spectrometry.
本文提出了一种利用直接热解吸-气相色谱(GC)和质谱(MS)相结合的方法来定量测定燃煤电厂煤、粉煤灰和炉渣中的挥发性有机化合物(VOCs)。所描述的方法几乎不需要处理样品,并且精确和敏感。芳香烃和脂肪烃(苯、甲苯、烷基苯、庚烷和辛烷)是这些固体样品中含量最多的化合物,煤样品的含量高于粉煤灰和矿渣。其他化合物(酸类、酮类、醛类、柠檬烯等)用质谱法鉴定。
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引用次数: 5
Simultaneous determination of fluorine, chlorine and sulfur in incinerator residues by oxidative high pressure digestion and ion chromatography 氧化高压消解-离子色谱法同时测定焚化炉残留物中的氟、氯和硫
Pub Date : 2000-12-01 DOI: 10.1051/ANALUSIS:2000166
H. Belevi, H. Mönch
An oxidative high pressure digestion method is presented to dissolve fluorine, chlorine and sulfur components of munic- ipal solid waste incinerator residues. It is a combination of the classical high pressure digestion technique with the combusti on in a closed system. The concentration determination is carried out by ion chromatography. The results are compared with those obtained by other digestion and extraction methods combined also with ion chromatography. A CNS-analyzer is used as a fur- ther method to compare the sulfur concentrations. Based on the obtained data, the accuracy of the fluorine, chlorine and sulfur concentrations is estimated as better than 85 %. It is concluded, that the oxidative high pressure digestion combined with ion chromatography is an appropriate method to determine fluorine, chlorine and sulfur concentrations in incinerator residues. Its main advantage is the simultaneous analysis of these three elements. However, it is a time consuming method.
提出了一种氧化高压消解法,用于溶解市政垃圾焚烧炉废渣中的氟、氯、硫组分。它是经典的高压消化技术与封闭系统内燃烧的结合。浓度测定采用离子色谱法。并与其它溶出提取方法及离子色谱法所得结果进行了比较。使用cns分析仪作为比较硫浓度的另一种方法。根据所获得的数据,估计氟、氯和硫浓度的准确度优于85%。结果表明,氧化高压消解与离子色谱法相结合是测定焚烧炉废渣中氟、氯、硫浓度的一种合适的方法。它的主要优点是同时分析这三个元素。然而,这是一个耗时的方法。
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引用次数: 5
Evaluation of Q-TOF-MS/MS and multiple stage IT-MSn for the dereplication of flavonoids and related compounds in crude plant extracts Q-TOF-MS/MS和多级IT-MSn对植物粗提取物中黄酮类化合物分离的评价
Pub Date : 2000-12-01 DOI: 10.1051/ANALUSIS:2000280895
J. Wolfender, P. Waridel, K. Ndjoko, K. Hobby, H. Major, K. Hostettmann
LC/MS/MS is becoming a very important tool for the on-line identification of natural products in crude plant extracts. For an efficient use of this technique in the dereplication of natural products, a careful study of the parameters used to generate informative MS/MS spectra is needed. In this paper the CID MS/MS spectra of ubiquitous flavonoids and related plant constituents have been systematically studied using hybrid quadrupole time of flight (Q-TOF) and ion trap (IT) mass analysers under various CID energy conditions. The results demonstrate that, if for hydroxylated flavonoids the CID MS/MS spectra generated on both instruments are similar, for partially methoxylated derivatives, important differences are observed hampering the creation of MS/MS databases exchangeable between instruments. Generally, fragments issued from C-ring cleavage, corresponding to those classically reported, were recorded but they were more easily observed on a Q-TOF instrument while losses of small molecules were favoured in IT-MS. MS/MS spectra recorded in the positive ion mode were more informative than those obtained from negative ions. For the assignment of flavonoids product ion spectra, on-line accurate mass measurement of all MS/MS fragments was obtained on the Q-TOF, while the multiple stage MSn capability of the ion trap was used to prove fragmentation pathways
LC/MS/MS正成为植物粗提取物中天然产物在线鉴定的重要工具。为了在天然产物的分离中有效地利用该技术,需要仔细研究用于生成信息丰富的MS/MS谱的参数。本文采用混合四极杆飞行时间(Q-TOF)和离子阱(IT)质谱仪,系统地研究了不同CID能量条件下植物中普遍存在的黄酮类化合物及其相关成分的CID MS/MS光谱。结果表明,对于羟基化的类黄酮,在两种仪器上生成的CID MS/MS光谱是相似的,对于部分甲氧基化的衍生物,观察到重要的差异,阻碍了在仪器之间可交换的MS/MS数据库的创建。通常,记录了c环裂解产生的片段,与经典报道的片段相对应,但在Q-TOF仪器上更容易观察到它们,而在IT-MS中更容易观察到小分子的损失。在正离子模式下记录的MS/MS谱比在负离子模式下获得的谱信息更丰富。对于类黄酮产物离子谱的分配,在Q-TOF上获得了所有MS/MS片段的在线精确质量测量,并利用离子阱的多级MSn能力证明了碎片化途径
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引用次数: 89
Use of LC-MS/MS for xenobiotic metabolism studies in animals LC-MS/MS用于动物异种代谢研究
Pub Date : 2000-12-01 DOI: 10.1051/ANALUSIS:2000280914
L. Debrauwer
The use of LC-MS/MS in the identification of xenobic metabolism pathawys in animals is described, on the basis of selected examples in the field of toxixologically relevant growth promoting agents. The structural elucidation of xenobiotic metabollites in complex biological matrices is archieved using various analytical methods and strategies using LC-MS with ESI or APCI ionisation techniques in combination with in-source CAD or MS/MS experiments. The use of some particular analytical tools (e.g. H/D exchange or MSn multisequential experiments) for solving specific structural ambiguities is also discussed.
基于在毒理学相关生长促进剂领域的选定实例,描述了LC-MS/MS在动物异种代谢途径鉴定中的应用。复杂生物基质中外源代谢物的结构阐明使用各种分析方法和策略,使用LC-MS与ESI或APCI电离技术,结合内部CAD或MS/MS实验。使用一些特殊的分析工具(例如H/D交换或MSn多序列实验)来解决特定的结构歧义也进行了讨论。
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引用次数: 6
UV spectrophotometry for monitoring toxic gases 有毒气体监测用紫外分光光度法
Pub Date : 2000-12-01 DOI: 10.1051/ANALUSIS:2000163
E. Dupuit, A. Dandrieux, P. Kvapil, J. Ollivier, G. Dusserre, O. Thomas
The need for gas compound measurement concerns overall three domains: environmental monitoring, emission mea- surement and risk assessment. These fields are different because of concentration range (from 10 -3 to thousands mg.m-3). A fast technique has been developed based on UV spectrophotometry. Simple robust optics and absence of interference from water vapour and carbon dioxide are two of the main benefits of this method. All measurements are performed with a quartz flow cell of 10 cm pathlength. In this condition, the detection limits of various compounds (ammonia, hydrogen sulphide, sulphur dioxide, benzene, toluene, ethylbenzene and p-xylene) vary between 30 and 100 mg.m-3. This UV spectrometry system has been tested with success in two applications. The first one is during gaseous ammonia dispersion, simulating a chemical accident. The sec- ond one is BTEX monitoring measurement in a process control of soil remediation. In this case, UV is associated with spectral data treatment software. All results are compared with reference methods (Nessler reagent for ammonia, gas chromatography for BTEX). An acceptable agreement was found.
对气体化合物测量的需求涉及三个领域:环境监测、排放测量和风险评估。这些场的浓度范围不同(从10 -3毫克到数千毫克)。建立了一种基于紫外分光光度法的快速检测技术。该方法的两个主要优点是光学简单,不受水蒸气和二氧化碳的干扰。所有的测量都是用10厘米路径长度的石英流池进行的。在这种条件下,各种化合物(氨、硫化氢、二氧化硫、苯、甲苯、乙苯和对二甲苯)的检出限在30至100毫克/立方米之间。该紫外光谱系统已在两个应用中测试成功。第一个是气态氨分散,模拟化学事故。二是土壤修复过程控制中BTEX的监测测量。在这种情况下,UV与光谱数据处理软件相关联。所有结果与参考方法(奈斯勒试剂测定氨,气相色谱法测定BTEX)进行比较。达成了一个可接受的协议。
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引用次数: 11
Individual, species and geographic origin influence on cooperage oak extractible content (Quercus robur L. and Quercus petraea Liebl.) 个体、树种和地理来源对栎(栎)和栎(栎)提取物含量的影响
Pub Date : 2000-12-01 DOI: 10.1051/ANALUSIS:2000162
F. Doussot, P. Pardon, J. Dedier, B. Jeso
Dry extract, ellagitanins, free ellagic acid, whisky-lactone, eugenol and vanillin have been quantified for a sample set of 61 pedunculate oaks (Quercus robur L.) and 72 sessile oaks (Quercus petraea Liebl.) originating from 6 different forests. Despite a very high interindividual variability, pedunculate oak shows higher level of dry extract, ellagitanins and free ellagic acid but lower level in volatil compounds compared to sessile oak. Inside a same species, differences between forests are less marked . Extractible compounds level is poorly correlated to the grain (ring width). Regarding cambial age, it might have its significanc e but lack of scientific data could not permit to conclude in that sense. Our results suggest that cooperage oak selection should be based on a species-provenance combination rather than on the grain or the provenance solely.
对来自6个不同森林的61株有梗栎树(Quercus robur L.)和72株无梗栎树(Quercus petaea Liebl.)的干提取物、鞣花单宁、游离鞣花酸、威士忌内酯、丁香酚和香兰素进行了定量分析。尽管个体间差异很大,但与无梗橡木相比,有梗橡木的干提取物、鞣花单宁和游离鞣花酸含量较高,但挥发物含量较低。在同一物种内部,森林之间的差异不太明显。可提取化合物水平与颗粒(环宽)相关性较差。关于形成层年龄,它可能有其意义,但由于缺乏科学数据,不能在这个意义上得出结论。我们的研究结果表明,合作橡木的选择应基于品种-种源组合,而不是仅仅基于籽粒或种源。
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引用次数: 43
MS/MS-libraries with triple quadrupole-tandem mass spectrometers for drug identification and drug screening MS/MS-文库与三重四极杆串联质谱用于药物鉴定和药物筛选
Pub Date : 2000-12-01 DOI: 10.1051/ANALUSIS:2000280934
W. Weinmann, M. Gergov, M. Goerner
Two MS/MS libraries of drugs created by electroscopy ionisation (ESI) and collision-induced dissociation (CID) of the quasimolecular ions have been developed with triple-quadrupole ion-spray mass spectrometers. for both libraries three and four different collision energies were used, rezspectively, to ontain a variety of CID spectra, which were all included separately into the MS/MS librarie. The MS/MS product ion spectraof more than 400 drugs were acquired in positive or negative mode in two labrories independetly. recently, on of these MS/MS libraries was applied successfully for the identification of drug metabolites and the other has been used for qualitative analysis of drugs in urine samples with data dependent experiments (DDE). In this work, the reproducibility of CID spectra has been tested with three instruments (including two different instruments) in three laboratories. For comparision of CID-spectra, library searching with a combination of the two libraries was performed and fit values were compared. With regard to libary fit values CID-spectra were found to be highly reproducible between the instruments, when similar CID gas pressure and collision energy were applied. In addition, the long-time reproducibility of CIS over 30 months with the API 365 was demonstrated. Furthermore, comparisions of in-source CID and CID by MS/MS was given. It can be concluded, that both MS/MS libraries created with APIs 365 can be used with both types of triple-quadrupole instruments from Sciex (API 365 and 2000) for drug identification. Two applications of these MS/MS spectra libraries in combination with data dependent experiments are summarised.
利用三-四极杆离子喷雾质谱仪建立了两个准分子离子的电子电离(ESI)和碰撞诱导解离(CID)建立的药物MS/MS文库。两个库分别使用3种和4种不同的碰撞能来包含各种CID谱,并分别纳入MS/MS库。在两个实验室分别以阳性或阴性模式获得了400多种药物的MS/MS产物离子谱。最近,其中一个MS/MS文库成功应用于药物代谢物的鉴定,另一个已用于数据依赖实验(data dependent experiments, DDE)对尿样中的药物进行定性分析。在本工作中,在三个实验室用三种仪器(包括两种不同的仪器)测试了CID光谱的再现性。为了比较cid光谱,将两个库组合进行库搜索,并比较拟合值。当使用相似的CID气体压力和碰撞能量时,两种仪器之间的CID光谱具有较高的重现性。此外,证明了API 365的CIS在30个月以上的长时间重复性。并用MS/MS法比较了内源CID和内源CID的差异。由此可见,用API 365创建的两种MS/MS文库均可用于Sciex的两种类型的三四极杆仪器(API 365和2000)进行药物鉴定。结合数据依赖实验,总结了这些MS/MS谱库的两种应用。
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引用次数: 44
Tandem mass spectral strategies for the structural characterization of flavonoid glycosides 类黄酮苷结构表征的串联质谱策略
Pub Date : 2000-12-01 DOI: 10.1051/ANALUSIS:2000280888
F. Cuyckens, Y. Ma, G. Pocsfalvi, M. Claeys
In this article we review tandem mass spectral approaches to the structural characterization of flavonoid glycosides wich are ubiquitous secondary plant metabolites. It is demonstrated how structural information on O-diglycosides can be obtained on (i) the carboydrate sequence, (ii) the aglycone part, and (iii) the linkage in the diglycosidic part. Both the positive and negative ion modes have been employed.
本文综述了用串联质谱方法研究植物次生代谢产物黄酮类苷的结构特征。它演示了如何从(i)碳酸酯序列,(ii)苷元部分和(iii)二糖苷部分的连接上获得o -二糖苷的结构信息。正离子模式和负离子模式都被采用。
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引用次数: 107
Ion-Trap Multiple Mass Spectrometry in Pesticide Analysis. 离子阱多重质谱法在农药分析中的应用。
Pub Date : 2000-12-01 DOI: 10.1051/ANALUSIS:2000280941
B. Larsen
Liquid chromatography pultiple mass spectrometry with atmospheric pressure ionisation and ion-trap instruments is a potentially useful technique for structure elucidation of polar pestcides and their degradation products. The major drawback today is the lack of spectral libraries and our limited knowledge on collision induced dissociation processes. The present paper gives an introduction to this area of research and presents interesting examples of fragmentation pathaways for protonated and deprotonated ions obtained by atmospheric pressure chemical ionisation (APCI) and electrospray ionisation (ESI).
液相色谱-多重质谱联用常压电离和离子阱仪器是一种极具潜力的极性农药及其降解产物结构分析技术。目前的主要缺点是缺乏谱库和我们对碰撞诱导解离过程的有限知识。本文介绍了这一研究领域,并介绍了通过大气压化学电离(APCI)和电喷雾电离(ESI)获得的质子化和去质子化离子的裂解途径的有趣例子。
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引用次数: 12
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