Liquid Chromatography Particle Beam Mass Research Articles

Particle beam liquid chromatography-mass spectrometry of triphenylmethane dyes: application to confirmation of malachite green in incurred catfish tissue.

Eight triphenylmethane dyes (malachite green, leucomalachite green, gentian violet, leucogentian violet, brilliant green, pentamethyl gentian violet, N',N'-tetramethyl gentian violet and N',N"-tetramethyl gentian violet) have been characterized by particle beam liquid chromatography-mass spectrometry. The electron ionization spectra obtained of these dyes by this technique exhibit similar fragmentation, with the formation of phenyl and substituted phenyl radicals, and loss of alkyl groups from the amines. It was observed that the six cationic dyes are reduced in the mass spectrometer source to form the corresponding leuco compounds. This technique was evaluated for the confirmation of malachite green and leucomalachite green in incurred catfish (Ictalurus punctatus) muscle tissue.

Identification and characterization of nitrogen compounds in Brazilian diesel oil by particle beam l.c.-m.s.

A simple procedure has been developed to isolate the basic and neutral nitrogen compounds from a Brazilian diesel distillate through acid partition and open column chromatography using alumina. With minimum sample preparation and clean-up, isolated fractions were analysed by particle beam liquid chromatography-mass spectrometry (l.c.-m.s.) using both reversed phase and normal phase chromatography. The basic fraction was found to contain mostly alkyl benzoquinolines (C 2C 4). The neutral fraction contained mostly alkyl carbazoles (C 1C 5). The identification was based upon electron impact mass spectra of each class of nitrogen compounds, and confirmed by ultraviolet (u.v.) spectral characteristics obtained using online photodiode array detection. Reversed phase chromatography was found to be more appropriate for resolving each class of carbazoles and benzoquinolines, while normal phase chromatography was superior for separating individual isomers. The quantitation of each class of carbazoles and benzoquinolines was obtained by high performance liquid chromatography-ultraviolet (h.p.l.c.-u.v.) analysis at 254 nm using carbazole and benzo[ h]quinoline as calibration standards. Comparison of the Brazilian diesel distillate to diesels having other origins indicated that they were nearly identical in terms of the nitrogen compounds present.

Analysis of coumarins by micro high-performance liquid chromatography—mass spectrometry with a particle beam interface

Coumarins are a large group of compounds that are naturally present in plant tissues and that exhibit a wide range of pharmacological properties. Analytical methods based on chromatographic techniques and conventional detectors are inadequate to accurately analyze coumarins in complex matrices such as plant extracts. In this article a new method based on a modified particle beam liquid chromatography-mass spectrometry interface is described. The method allows specific and accurate determination of several coumarins in biological matrices. An application regarding the analysis of 18 coumarins in the extract of Smyrnium perfoliatum L. is also reported.

Characterization of anthraquinone-2-carbonyl chloride as an alcohol derivatization reagent for negative ion chemical ionization mass spectrometry

Anthraquinone-2-carbonyl chloride has been utilized as a derivatization reagent for alcohols to impart electron affinity and aid in transport via a particle beam liquid chromatography-mass spectrometry (LC/MS) interface. In addition, the gas chromatographic-mass spectrometry, UV, fluorescence, and electrochemical characteristics of the derivatives were determined. A series of model compounds, 2-phenylethanol (phenethyl alcohol), 1-phenyl-2-propanol, 2-methyl-l-phenyl-2-propanol, hexanol, and methyl 2-methylglycerate, were used as analytes.The particle beam LC/MS properties of the resultant anthraquinone carboxylate esters were determined in electron impact (EI) and negative ion chemical ionization (NCI) modes. The NCI responses of these anthraquinone carboxylate esters were compared with the corresponding 3,5-dinitrobenzoate esters. The anthraquinone carboxylate esters exhibited an NCI to EI sensitivity enhancement of 113 and were detected in NCI at a tenfold lower concentration than the corresponding 3,5-dinitrobenzoate esters. A detection limit of 26 pg injected on column was achieved for phenethyl anthraquinone carboxylate in NCI by using selected ion monitoring.

Identification of vitamins A, D and E by particle beam liquid chromatography-mass spectrometry

Particle beam (PB) high performance liquid chromatography (HPLC)-mass spectrometry (MS) has been studied to investigate its suitability for the analysis of fat-soluble vitamins, as an example of thermally labile substances. The PB LC-MS system has been used to detect and identify vitamins A, D and E in foods and multi-vitamin preparations. The qualitative performance of the PB interface has been evaluated by an examination of the working parameters. A rapid elution of the vitamins was obtained on a C8 reversed-phase column using an aqueous methanol mobile phase. Analyses have been carried out using both, electron (EI) and chemical (CI) ionization. Positive and negative-ion CI spectra of the compounds are discussed. When PB-MS conditions are optimized, the detection limits for the fat-soluble vitamins tested have been typically in the 0.6–25 ng range when using the selected-ion monitoring technique.

Determination of diquat and paraquat in water using high-performance liquid chromatography with confirmation by liquid chromatography-particle beam mass spectrometry

A method was developed for the extraction of diquat and paraquat from environmental water samples by ion-exchange column chromatography. Determinations were performed using high-performance liquid chromatography with diode array detection. The HPLC method was developed to be compatible with LC-MS techniques. Results were confirmed with LC-particle beam (electron ionization) MS, where a unique ionization process was observed. Recoveries in drinking water were over 75% for both diquat and paraquat spiked at concentrations of 5–10 μg l . The method presented is uniquely specific since a diode array UV spectrum is obtained as well as an particle beam mass spectrum, insuring correct identification and quantitation of diquat and paraquat.

Characterisation of electron beam generated transformation products of irganox 1010 by particle beam liquid chromatography-mass spectrometry with on-line diode array detection

Transformation products of Irganox 1010 [pentaerythritol tetrakis-3-(3,5-di- tert.-butyl-4-hydroxyphenyl) propionate], in food contact polymers subjected to electron beam irradiation have been analysed by particle beam LC-MS with on-line UV diode array detection. It has been shown that the principal transformation products arise via loss of sub-units of the parent molecule, and the subsequent transformation of these sub-units. A total of 56 transformation products has been detected, for some of which structures are proposed. These results are compared to previous work on Irganox 1330 [1,3,5-trimethyl-2,4,6-tris(3′,5′-di- tert.-butyl-4-hydroxybenzyl)benzene], where transformations to yield p-quinone methide type structures were shown to occur.

Application of liquid chromatography-particle beam mass spectrometry and gas chromatography-mass spectrometry for the identification of metabolites of polycyclic aromatic hydrocarbons

Two liquid chromatography-particle beam mass spectrometry (LC-PBMS) systems have been used for analysis of polycyclic aromatic hydrocarbon metabolites in water samples from a biological decomposition model experiment. The results were compared with those obtained by classical gas chromatography-mass spectrometry. Evaluation of spectral data indicated the presence of six main metabolites; 1H,3H-naphtho [1,8-cd]pyran-1,3-dione, 1-(hydroxymethyl)naphthalene, and 1,2-acenaphthenedione were identified by use of standard substances and spiking experiments. Enrichment of the investigated water samples with online pre-column (C18) concentration, freeze-drying, and solvent extraction led to similar results with only slight differences. The application of microbore separation columns proved to be a promising tool in particle beam LC-MS measurements.

Particle beam liquid chromatography-mass spectrometry method with negative ion chemical ionization for the confirmation of oxacillin, cloxacillin and dicloxacillin residues in bovine muscle.

To ensure human food safety, the European Union has defined maximum residue limits (MRLs) for veterinary drug residues in food products. Analytical methods need to be developed to confirm the presence of drugs at the MRL level. A method using particle beam liquid chromatography-mass spectrometry was developed for the confirmation of oxacillin, cloxacillin and dicloxacillin in bovine muscle at the maximum residue limit of 300 micrograms kg-1. Beta-lactams were extracted from tissues with ethyl acetate under slightly acidic conditions and separated on a C18 bonded silica column with a methanol-aqueous formic acid (2%) solution-acetonitrile mobile phase. Negative ion chemical ionization with methane as the reagent gas was used to identify the compounds. The specificity required for a regulatory confirmation procedure was achieved by monitoring five fragment ions for each compound (selected ion monitoring mode): m/z 183, 198, 213, 214 and 241 for oxacillin; m/z 196, 248, 250, 275 and 277 for cloxacillin; m/z 165, 230, 232, 274 and 276 for dicloxacillin.

Identification of tylosin in bovine muscle at the maximum residue limit level by liquid chromatography-mass spectrometry, using a particle beam interface.

A particle beam liquid chromatography-mass spectrometric method is presented as a confirmatory technique for analysis of tylosin residues in bovine muscle. After chloroform extraction and a diol solid-phase extraction clean-up, on-line liquid chromatography-mass spectrometry (LC-MS) of extracts is carried out on an RP-18 bonded silica column. The analyte is introduced into the ion source by a particle beam interface and identified by negative chemical ionization with selective ion monitoring. The tylosin molecular ion is obtained with this ionization mode. The response of the ion chromatogram peak areas is linear for the three levels of spiked muscle analysed (0.5, 1 and 2 maximum residue limit). Under these LC-MS conditions, other macrolide antibiotics such as spiramycin and erythromycin do not interfere with tylosin.

Determination of the aza alkyl lysophospholipid 3-methoxy-2-N,N-methyloctadecylaminopropyloxyphosphorylcholine in rat plasma by liquid chromatography—particle beam—mass spectrometry

A sensitive and specific method for the determination of the aza alkyl lysophospholipid (AALP) 3-methoxy-2-N,N-methyloctadecylaminopropyloxyphosphorylcholine (I) in rat plasma is described. The target molecule was analyzed by high-performance liquid chromatography (HPLC)-mass spectrometry (MS) after one single liquid-liquid extraction with chloroform-methanol (2:1, v/v). 1,2-Didecanoyl-sn-glycero-3-phosphocholine was used as internal standard. HPLC was carried out using a polymeric reversed-phase column; the coupling to the mass spectrometer was a particle beam (PB) interface, and the ionization method was electron impact (EI). This simple and rugged method permits the measurement of I in rat plasma in the range of 25 ng/ml-5 micrograms/ml with good accuracy and precision and is used in pharmacokinetic studies.

Determination of polycyclic aromatic hydrocarbons by high-performance liquid chromatography—particle beam — Mass Spectrometry.

In this article, we report a high-performance liquid chromatography—particle beam—mass spectrometric (HPLC-PB-MS) method for the determination of polycyclic aromatic hydrocarbon (PAHS). The PB interface consists of a concentric ultrasonic nebulizer with temperature-controlled desolvation chamber and a three-stage momentum separator. The HPLC-PB-MS method showed greater sensitivity for PAHs with molecular weights above 178 than for those PAHs with molecular weight below 178. The percent relative standard deviations for the determination of 0.5 ng chrysene, 1.0 ng dibenzo[a,h]anthracene, 1.0 ng benzo[g,h,i]perylene, and 2.5 ng coronene were 20%, 2.5%, 13.7%, and 6%, respectively. The detection limits at signal/noise = 3 were 0.2 ng for chrysene, 1.0 ng for dibenzo[a,h]anthracene, 0.5 ng for benzo[g,h,i]perylene, and 1.5 ng for coronene.

Particle beam liquid chromatography—mass spectrometry behaviour of polynuclear metal carbonyl compounds

High-performance liquid chromatography (HPLC)-mass spectrometry (MS) was applied to organotransition-metal chemistry with the aim of studying the relationship between chromatographic behaviour and structural features of polynuclear organometallic compounds and of developing the methodological aspects of application of the combined technique in this field. In order to obtain significant structural information about organometallic compounds separated by HPLC, a particle beam LC-MS interface was used. As a first approach, some alkyne-carbonyl ruthenium derivatives and cyclopentadienyl nickel—ruthenium and nickel—osmium carbonyl clusters were considered all these compounds are of relevant interest in the field of both homogeneous and heterogeneous catalysis. The separation of all the examined clusters was performed under reversed-phase conditions with non-aqueous mobile phases. Full-scan electron impact and chemical ionization mass spectra were obtained from the LC eluates.

Liquid chromatography — Particle beam mass spectrometry for identification of unknown pollutants in water

Trace enrichment on a precolumn packed with copolymer material, coupled on-line with reversed-phase, column liquid chromatography-particle beammass spectrometry (RPLC-PB-MS) has been used for both target and non-target analysis of water samples. RPLC is carried out on a C-18-bonded silica column using a linear acetonitrile-0.1 M ammonium acetate gradient. Using optimised PB-MS conditions and 100–250 ml water samples, the detection limits for several phenylureas are in the 0.03–0.05 μg l−1 range using the full-scan mode; repeatability is good and the LC-PB-MS system is robust. Several surface and drinking water samples have been analysed and low levels of various environmental contaminants have been identified using electron impact mass spectra. Applying chemical ionisation with methane as reagent gas in both the positive and negative mode in conjunction with PB-MS provides relevant confirmatory information.

Determination of nicotine and two major metabolites in serum by solid-phase extraction and high-performance liquid chromatography, and high-performance liquid chromatography—particle beam mass spectrometry

A rapid and selective assay of nicotine, cotinine and rans-3'-hydroxycotinine in human serum, based on high-performance liquid chromatography with UV detection has been developed. The compounds were subjected to solid-phase extraction, using Extrelut 1 cartridges. Recoveries were ca. 95% for nicotine, 90% for cotinine and 50–55% for trans-3'-hydroxycotinine. The limit of quantitation observed with this method was 10 ng/ml for nicotine and 5 ng/ml for each of the metabolites. The compounds were also identified using high-performance liquid chromatography with particle beam mass spectrometry, to confirm their presence in human serum.

Particle beam liquid chromatography–mass spectrometry: instrumentation and applications. A review

Particle beam liquid chromatography–mass spectrometry: instrumentation and applications. A review

Evidence for thermal decomposition contributions to the mass spectra of chlorinated phenoxyacid herbicides obtained by particle beam liquid chromatography mass spectrometry

The spectral quality of a group of chlorinated phenoxyacid herbicides has been shown to degrade under certain conditions upon introduction into the mass spectrometer by a particle beam interface. Experiments were performed to investigate these changes in spectra. Normalized ion chromatograms were generated for the herbicides, and the results showed a broadening of the profiles of some ions, indicating a longer residence time in the ion source. These ions were postulated as coming from the ionization of thermal degradation products from the herbicides. The generation of these ions was dependent on ion source temperature, analyte concentration, and, by implication, ion source cleanliness. Tandem mass spectrometry experiments were performed on these ions from the herbicides and ions from the corresonding phenols. The tandem mass spectra of the ions from the herbicides were similar to the tandem mass spectra of the ions from the phenols. Therefore, it appears that the particle beam mass spectra of the chlorinated phenoxyacid herbicides are composite spectra with contributions from the gas phase ionization of the parent herbidides and thermal decomposition products.

Mass transport and calibration in liquid chromatography particle beam mass spectrometry

Differences in the designs of two liquid chromatography particle beam mass spectrometry systems result in differences in the transport of ammonium acetate and differences in ion abundance-enhancing carrier effects. The effect of mobile phase composition, especially the proportion of water in the mobile phase, on transport efficiency is described. Instrument detection limits for 12 compounds with two different interface designs are presented. The calibrations are generally nonlinear explained in terms of mass transport effects and supported by experiments with isotopically labeled species that coelute with the native species. Summary results of a small multilaboratory study are presented. Calibration with isotopically labelled internal standards is recommended for real-world environmental samples

A particle beam-liquid chromatography-mass spectrometry method for the determination of lipoxygenase metabolites of arachidonic acid

An application of the particle beam-liquid chromatography-mass spectrometry technique to the quantification of hydroxyeicosatetraenoic acids (15-, 12-, and 5-HETE) in biological samples is presented. The acids are extracted with Ethyl acetate and then transformed into pentafluorobenzyl esters, thus increasing the sensitivity of their detection by negative chemical ionization mass spectrometry. Reverse-phase HPLC separation of HETEs is performed in about 10 min with a water-methanol gradient. The procedure shows a detection limit of nearly 0.5 pmol, about one order of magnitude lower than that of the widely used HPLC/UV methods. The quantitative determination is linear ( r 2 > 0.998) for all of the HETEs in the range tested (3–1500 pmol) and a CV lower than 8.5% was observed for repeated analysis of samples. As an application of the method, HETEs formed from endogenous arachidonate were evaluated in extracts obtained from coincubates of platelets and neutrophils stimulated with calcium ionophore A23187.

Determination of chlorinated phenoxy acid and ester herbicides in soil and water by liquid chromatography particle beam mass spectrometry and ultraviolet absorption spectrophotometry

ADVERTISEMENT RETURN TO ISSUEPREVArticleNEXTDetermination of chlorinated phenoxy acid and ester herbicides in soil and water by liquid chromatography particle beam mass spectrometry and ultraviolet absorption spectrophotometryIn Suk. Kim, Fassil I. Sasinos, Robert D. Stephens, Jeanny. Wang, and Mark A. BrownCite this: Anal. Chem. 1991, 63, 8, 819–823Publication Date (Print):April 15, 1991Publication History Published online1 May 2002Published inissue 15 April 1991https://doi.org/10.1021/ac00008a017RIGHTS & PERMISSIONSArticle Views368Altmetric-Citations-LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InReddit PDF (625 KB) Get e-Alerts Get e-Alerts