共查询到19条相似文献,搜索用时 93 毫秒
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固相萃取/离子阱气相色谱质谱联用对血液中多种安眠药物的同时测定 总被引:3,自引:1,他引:3
建立了气相色谱-质谱联用测定血液中多种安眠药物的分析方法,通过固相萃取提取并富集血液样品中的9种常见巴比妥类、吩噻嗪类和苯二氮杂类安眠药物,采用离子阱二级质谱检测其含量。通过优化萃取溶液pH值及气相色谱-质谱联用分析条件,对9种安眠药物进行了定量分析。采用离子阱串联质谱(MS/MS)技术消除基底干扰,给出被测物结构信息。9种安眠药物的检出限为0.04~0.10 mg/L,回收率为78%~93%。方法用于人心血中安眠药物的检测,检出安定0.6 mg/L。该方法高效、简单、灵敏度高,可用于血液中巴比妥类、吩噻嗪类和苯二氮杂类安眠药物的同时测定。 相似文献
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对当前法庭科学领域中有机炸药的实验室和现场常用的检验技术如:气相色谱、液相色谱等色谱技术,原位电离质谱、同位素比质谱等质谱技术,气相色谱-质谱、液相色谱-质谱等色谱-质谱联用技术,毛细管电泳技术,离子迁移谱技术,红外光谱、拉曼光谱、太赫兹等光谱技术,荧光、电化学、表面等离子体共振等传感器技术进行了归类和总结,并对有机炸... 相似文献
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《理化检验(化学分册)》2010,(11)
综述了从1968-2010年间质谱及色谱-质谱联用分析法在多糖结构分析中的应用,包括电子轰击质谱、化学电离质谱、快原子轰击质谱、电喷雾质谱、基质辅助激光解吸离子化质谱、气相色谱-质谱、液相色谱-质谱和毛细管电泳-质谱法(引用文献42篇)。 相似文献
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建立了同时筛查测定猪肉组织中氟喹诺酮类、磺胺类、有机磷类、β-激动剂类、四环素类5类26种药物残留的液相色谱-四极杆飞行时间质谱分析方法。试样采用QuEChERS前处理方法,样品经酸化乙腈-甲醇(1%乙酸,10%甲醇)提取。提取液以C18分散剂和正己烷净化,氮吹浓缩、定容后过滤膜上机检测。液相色谱以甲醇-水(0.1%甲酸)作为流动相梯度洗脱,C18色谱柱分离;高分辨质谱采用正离子模式检测,以二级质谱特征离子定性,以分子离子精确质量数提取色谱峰面积定量。结果表明26种药物的定量下限为0.4~10μg/kg;加标回收率为56.7%~106.2%,相对标准偏差(RSD)为7.7%~15.8%。方法操作简单、快速、高效,可作为猪肉中26种药物残留的快速筛查检测方法。 相似文献
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Mass spectrometry for identifying pharmaceutical biotransformation products in the environment 总被引:1,自引:0,他引:1
T. Kosjek E. Heath M. Petrovi D. Barcel 《Trends in analytical chemistry : TRAC》2007,26(11):1076-1085
Many classes of pharmaceuticals have been detected in wastewaters and surface waters around Europe, but little is known about their occurrence, fate and potential harmful effects on the environment, and that makes them an important group among those compounds considered to be new emerging contaminants. To understand the cycling of pharmaceuticals and their metabolites, it is essential to possess qualitative and quantitative information on their presence in the environment. This review covers the current status and future prospects of advanced hyphenated mass spectrometric (MS) techniques (gas chromatography-MS (GC-MS) and liquid chromatography-MS (LC-MS)) in elucidating the structures of trace contaminants, namely pharmaceutical biodegradation products in complex environmental matrices. The article is oriented towards technique and method and discusses capabilities, potential and limitations of different GC and LC mass analyzers (quadrupole, ion trap, time-of-flight and hybrid techniques) in dealing with analytical challenges of complex matrices and trace contaminants. We also give practical examples of their applications. The main scope of this article is to support and to facilitate the on-going research on pharmaceutical biodegradation products in environmental samples. 相似文献
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Frommberger M Hertkorn N Englmann M Jakoby S Hartmann A Kettrup A Schmitt-Kopplin P 《Electrophoresis》2005,26(7-8):1523-1532
A quantitative, specific, and sensitive method for the determination of N-acylhomoserine lactones (HSLs - a group of bacterial semiochemicals) in the form of their hydrolysis products (N-acylhomoserines, HSs) is presented. Real samples were analyzed by capillary zone electrophoresis-mass spectrometry (CZE-MS) after alkaline lactonolysis and extraction by mixed-mode anion-exchange solid-phase extraction. The presented cleanup significantly speeds up the HSL extraction procedure, strongly reduces sample consumption, and is more selective compared to the commonly used liquid/liquid extraction. Completeness of the hydrolysis reaction was examined by nuclear magnetic resonance spectroscopy. This CZE-MS method complements recently published capillary separation techniques (nano liquid chromatography-MS, partial-filling micellar electrokinetic chromatography-MS, gas chromatography-MS) and provides a possibility to differentiate quantitatively between the homoserines (as naturally occurring degradation products) besides the intact homoserine lactones. The method was found to be quantitative down to a concentration of 0.05 microg/mL (limit of quantification), while the limit of detection was determined with 0.01 microg/mL - sufficient for the analysis of culture supernatants. 相似文献
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Tang K Page JS Marginean I Kelly RT Smith RD 《Journal of the American Society for Mass Spectrometry》2011,22(8):1318-1325
In this work, the subambient pressure ionization with nanoelectrospray (SPIN) ion source and interface, which operates at
~15–30 Torr, is demonstrated to be compatible with gradient reversed-phase liquid chromatography-MS applications, exemplified
here with the analysis of complex samples (a protein tryptic digest and a whole cell lysate). A low liquid chromatographic
flow rate (100–400 nL/min) allowed stable electrospray to be established while avoiding electrical breakdown. Efforts to increase
the operating pressure of the SPIN source relative to previously reported designs prevented solvent freezing and enhanced
charged cluster/droplet desolvation. A 5- to 12-fold improvement in sensitivity relative to a conventional atmospheric pressure
nanoelectrospray ionization (ESI) source was obtained for detected peptides. 相似文献
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Demetrio De la Calle García Manfred Reichenbcher Klaus Danzer Christian Hurlbeck Christine Bartzsch Karl-Heinz Feller 《Journal of separation science》1997,20(12):665-668
The extraction of wine bouquet components with solid-phase microextraction (SPME) using different fibers was studied. Polyacrylate fibers (PA-85) achieve the most complete bouquet profiles. About ninety substances were identified by capillary gas chromatography-MS and their retention factors were calculated to allow peak identification in capillary-GC-FID chromatograms. The terpene profiles of different wines were recorded by SPME (PA-85)-CGC-FID. 相似文献
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Heegaard NH Hansen MZ Sen JW Christiansen M Westermark P 《Journal of separation science》2006,29(3):371-377
Transthyretin (TTR) is a small serum protein that is involved in distinct phenotypes of amyloidosis with different tissue localization, age of onset, and rate of progression. Some types of TTR-amyloidosis (such as familial amyloid polyneuropathy) are associated with various amino acid point mutations, while cardiac amyloid myopathy may also be associated with precipitation of the wild-type molecules, e.g., in senile systemic amyloidosis. Because of the unsettled relationship between circulating and precipitated TTR we here explore on-line immunoaffinity (IA) chromatography-MS and immunoprecipitation (IP)-MS methods for characterizing the circulating TTR population in normal individuals and in patients with known TTR-amyloidosis. It was found necessary to reduce the samples, e.g., with DTT, prior to ESI-TOF-MS. This reversed oxidative modifications to sufficiently resolve the two mass peaks isolated from sera of heterozygous patients. A simple IP technique without the use of centrifugal filtration was found to be convenient for the assessment of the TTR population in serum as demonstrated for both normal and variant (the Met111Leu mutation) TTR. This approach also readily allowed the identification of oxidation, S-sulfation, and S-cysteinylation in unreduced samples, while these modifications were less well resolved in the on-line IA chromatography-MS approach. 相似文献
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《Trends in analytical chemistry : TRAC》1988,7(6):202-208
New procedures in quantitative mass spectrometry (MS) continue to follow very closely the development of qualitative methods. The burgeoning of MS techniques appropriate to the analysis of polar and non-volatile compounds has produced a corresponding increase in the scope of quantitative MS. In general, quantitative procedures based on the newer methods (such as fast-atom bombardment, liquid chromatography-MS, MS-MS) have not yet reached the point of quantitative refinement that may be expected of gas chromatography. Nevertheless, with increased understanding of the newer methods, significant improvements in quantification may be confidently anticipated. 相似文献
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The analytical data for identifying an unknown substance that was found in a nutrition supplement is presented. The unknown substance is purified using thin-layer chromatography and then measured using high-resolution mass spectrometry (HRMS) giving the exact mass from which the structure of the unknown substance was proposed. The procedure for synthesizing N-nitrosofenfluramine from fenfluramine is described. The extracted, synthesized, and standard N-nitrosofenfluramine are compared using HRMS, high-performance liquid chromatography (HPLC)-MS, HPLC-UV, Fourier transform IR spectroscopy, gas chromatography-MS, TLC, and NMR (1H NMR and 13C NMR). All analytical data obtained confirm that the unknown peak in the nutrition supplement is N-nitrosofenfluramine and that the synthetic procedure described can easily provide the N-nitrosofenfluramine reference substance for identification. 相似文献