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PubMed2003

Comparison of electrospray ionization and atmospheric pressure chemical ionization techniques in the analysis of the main constituents from Rhodiola rosea extracts by liquid chromatography/mass spectrometry.

Rhodiola rosea L. (Golden Root) has been used for a long time as an adaptogen in Chinese traditional medicine and is reported to have many pharmacological properties. A liquid chromatographic (LC) method with mass spectrometric (MS) detection based on selected ion monitoring (SIM) was developed for determining salidroside, sachaliside 1, rosin, 4-methoxycinnamyl-O-beta-glucopyranoside, rosarin, rosavin, cinnamyl-(6'-O-beta-xylopyranosyl)-O-beta-glucopyranoside, 4-methoxy-cinnamyl-(6'-O-alpha-arabinopyranosyl)-O-beta-glucopyranoside, rosiridin and benzyl-O-beta-glucopyranoside from the callus and plant extracts in one chromatographic run. Good linearity over the range 0.5-500 ng ml(-1) for salidroside, 2-2000 ng ml(-1) for rosavin and 2-500 ng ml(-1) for benzyl-O-beta-glucopyranoside was observed. The intra-assay accuracy and precision within quantitation ranges varied between -10.0 and +13.2% and between 0.7 and 9.0%, respectively. Optimization of the ionization process was performed with electrospray and atmospheric pressure chemical ionization techniques using four different additive compositions for eluents in the LC/MS scan mode, using both positive and negative ion modes. The best ionization sensitivity for the compounds studied was obtained with electrospray ionization when using pure water without any additives as the aqueous phase.

Atmospheric Pressure↗
PubMed2001

Phenyl-modified reversed-phase liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry: a universal method for the analysis of partially oxidized aromatic hydrocarbons.

A new liquid chromatographic method for the efficient separation of aromatic compounds having a wide range of sizes, molecular structures, and polarities has been developed. Based on a phenyl-modified silica reversed stationary phase and a methanol-water solvent gradient, it allows the separation of mono- and polycyclic aromatic hydrocarbons (PAHs) having up to five condensed aromatic rings and partially oxidized derivatives within a single chromatographic run of 40-min duration. The applicability of the method is demonstrated using 81 reference substances (PAHs, phenols, quinones, acids, lactones, esters, etc.) and real samples of environmental, medical, and technical relevance (ozonized PAHs, lake water, human urine, diesel exhaust condensates). The retention times of the investigated aromatics exhibit a regular increase with molecular mass and a systematic decrease with increasing number and polarity of functional groups. In case of intramolecular hydrogen bonding, a positive shift of retention time provides additional structural information. The combination of chromatographic retention time with the molecular mass and structural information from mass spectrometric detection allows the tentative identification of unknown aromatic analytes at trace levels, even without specific reference substances. With atmospheric pressure chemical ionization (APCI), low detection limits and highly informative fragmentation patterns can be obtained by in-source collision-induced fragmentation in a single-quadrupole LC-APCI-MS system as applied in this study, and multidimensional MS experiments are expected to further enhance the potential of the presented method.

Atmospheric Pressure↗
PubMed2006

Fragmentation study of protonated chalcones by atmospheric pressure chemical ionization and tandem mass spectrometry.

Fragmentation mechanisms of protonated chalcone and its derivatives with different functional groups were investigated by atmospheric pressure chemical ionization with tandem mass spectrometry (MS/MS). The major fragmentation pathways were loss of the phenyl group from the A or B ring, combined with loss of CO. Losses of H(2)O and CO from the precursor ions of [M+H](+) are proposed to occur via rearrangements. Elimination of water from protonated chalcones was observed in all the title compounds to yield a stable ion but it was difficult to obtain skeletal fragmentation of a precursor ion. Loss of CO was found in the MS/MS spectra of all the compounds except the nitro-substituted chalcones. When the [M+H--CO](+) ion was fragmented in the MS/MS experiments, there were distinctive losses of 15 and 28 Da, as the methyl radical and ethylene, respectively. The ion at m/z 130, found only in the nitro-substituted chalcones, was assigned as C(9)H(6)O by Fourier transform ion cyclotron resonance (FTICR)-MS/MS; m/z 130 is a common fragment ion in the electron ionization (EI) spectra of chalcones. In order to more easily distinguish the constitutional isomers of these chalcones, breakdown curves were produced and these provided strong support in this study.

Journal Article↗
PubMed2005

A combination atmospheric pressure LC/MS:GC/MS ion source: advantages of dual AP-LC/MS:GC/MS instrumentation.

Modification of commercial LC/MS instrumentation to allow both atmospheric pressure (AP) LC/MS and GC/MS is described. Advantages of this additional capability versus LC/MS alone include higher chromatographic resolution in the GC versus LC mode, greater peak capacity for complex mixture analysis, higher sensitivity for a variety of volatile compounds, and the ability to observe compounds of low polarity that are not readily observed in LC/MS. Advantages over conventional GC/MS include the ability to use higher carrier gas flow and shorter columns for passing less volatile materials through the gas chromatograph, selective ionization, and rapid switching between positive and negative ion modes. Other advantages include application of the enhanced capabilities of LC/MS instrumentation to GC/MS analyses such as cone voltage fragmentation, MS(n), high mass resolution, and accurate mass measurement. Limitations of APGC/MS include the inability to observe saturated hydrocarbon and certain other highly nonpolar compounds and less odd-electron fragmentation for computer aided library searching. For some analyses, the limitation related to ionization of highly nonpolar compounds is advantageous, as is the simplified mass spectrum and easy molecular weight identification that results from less fragmentation observed in the AP ionization mode.

Chromatography, High Pressure Liquid↗
PubMed2004

Atmospheric pressure photo-ionization liquid chromatography/mass spectrometric determination of aflatoxins in food.

A comparison between electrospray ionization (ESI) and the recent introduced atmospheric pressure photo-ionization (APPI) technique is described for the liquid chromatography/mass spectrometric (LC/MS) determination of aflatoxin B1, B2, G1 and G2 in food. For the optimization of APPI, several APPI ion source parameters were examined. Furthermore, the chemical noise and signal suppression of ESI and APPI by sample matrix interference were investigated. The results indicated that APPI has the low chemical noise and the little signal suppression in comparison with ESI. The mean recovery of each aflatoxin from peanuts, corn, nutmeg and red pepper sample spiked at 1 ng g(-1) ranged from 89 to 105% with relative standard deviations of 3.3-5.1%. The limit of detection (S/N = 3) in all food was in the range 0.11-0.5 ng g(-1). From these studies, it is suggested that APPI can be used as an additional tool in food residue analysis.

Aflatoxin B1↗
PubMed2003

Surface-activated no-discharge atmospheric pressure chemical ionization.

A new ionization method named surface-activated chemical ionization (SACI) has been realized. In this invention a commercially available atmospheric pressure chemical ionization (APCI) chamber, employed without any corona discharge (no-discharge APCI), has been modified with the insertion of a gold surface, leading to a significant improvement in the ionization efficiency. The ionization of the sample takes place by both gas-phase and surface-activated processes. This new ionization source is able to generate ions with high molecular mass and low charge states, leading to improved sensitivity and reduced noise. The new device has been tested in the analysis of some peptides. A comparison between the performance with and without the presence of the surface, and the optimization of the operating conditions (nebulizing gas flow, sample solution flow, pH of solution, and surface area), are reported and discussed.

Air Pressure↗
PubMed2002

Structural analysis of oligosaccharides by atmospheric pressure matrix-assisted laser desorption/ionisation quadrupole ion trap mass spectrometry.

An ion source incorporating a fibre optic interface has been constructed for atmospheric pressure matrix-assisted laser desorption/ionisation quadrupole ion trap mass spectrometry. The configuration has been applied to the study of linear and complex oligosaccharides. Multi-stage tandem mass spectrometry (MSn, n = 2-4) experiments carried out in the ion trap enable extended fragmentation pathways to be investigated that yield structural information. Collisional activation of sodiated oligosaccharides, as demonstrated on the model compound maltoheptaose, produces primarily B and Y fragments resulting from cleavage of glycosidic bonds; fragments from cross-ring cleavages are also observed following further stages of tandem mass spectrometry, providing additional linkage information. The analyses of mixtures of complex oligosaccharides are demonstrated for N-linked glycans from chicken egg glycoproteins and a ribonuclease glycan mixture. Mass spectrometric and tandem mass spectrometric data for sugars with molecular weights up to 4000 Da is shown for mixtures of linear dextrans and N-linked glycans. The use of MSn (n = 3, 4) on these complex molecules enabled structural information to be elucidated that confirms data observed in the MS/MS spectra.

Carbohydrate Sequence↗
PubMed2004

Application of pentafluorophenyl hydrazine derivatives to the analysis of nabumetone and testosterone in human plasma by liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry.

Two carbonyl compounds, nabumetone and testosterone, were derivatized with pentafluorophenyl hydrazine (PFPH) and analyzed by atmospheric-pressure chemical-ionization mass spectrometry. The PFPH derivatives underwent dissociative electron capture in negative-ion APCI (ECAPCI) and gave intense [M-20](-) ions in the mass spectra. In positive-ion APCI, the PFPH derivatives underwent efficient protonation and gave intense [M + H](+) ions in the mass spectra. In CID, the major product ions of the [M-20](-) ions in ECAPCI corresponded to the partial moiety of PFPH. In contrast, the major product ions of [M + H](+) corresponded to the partial moiety of the analyte. By using selected reaction monitoring (SRM) detection, low pg of nabumetone (1 pg) and testosterone (7 pg) could be detected in both ECAPCI and positive-ion APCI. In comparison with the detection limits (SRM) of the underivatized analytes, use of the PFPH derivatives resulted in 2500-fold and 35-fold sensitivity enhancements for nabumetone and testosterone, respectively. The PFPH derivatives were applied to the analysis of nabumetone and testosterone in human plasma by both ECAPCI and positive-ion APCI and were found to enable detection of 0.1 ng mL(-1) nabumetone in spiked plasma. For testosterone, endogenous testosterone in female plasma was detected in both ECAPCI and positive-ion APCI.

Butanones↗
PubMed2005

Comparison of the surface characteristics of polypropylene films treated by Ar and mixed gas (Ar/O2) atmospheric pressure plasma.

In an attempt to modify the hydrophobic surface properties of polypropylene (PP) films, this study examined the optimum process parameters of atmospheric pressure plasma (APP) using Ar gas. Under optimized conditions, the effects of a mixed gas (Ar/O2) plasma treatment on the surface-free energy of a PP film were investigated as a function of the O2 content. The polar contribution of the surface-free energy of the PP film increased with increasing O2 content in the gas mixture. However, slightly more oxygen-containing polar functional groups such as CO, CO, and COO were introduced on the PP film surface by the Ar gas only rather than by the Ar/O2 gas mixture. In addition, AFM analysis showed that the Ar plasma treatment of the PP film produced the smoothest surface as a result of the relatively homogeneous etching process.

Journal Article↗
PubMed1999

Mass spectrometric and tandem mass spectrometric behavior of nitrocatechol glucuronides: a comparison of atmospheric pressure chemical ionization and electrospray ionization.

The mass spectrometric (MS) and tandem mass spectrometric (MS/MS) behavior of six nitrocatechol-type glucuronides using atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI) was systematically studied, and the effect of operation parameters on the fragmentations are presented. The positive ion APCI- and ESI-MS spectra showed an intense protonated molecule and the respective negative ion spectra a deprotonated molecule with minimal fragmentation. The main fragment ions in the MS/MS spectra of the protonated and deprotonated molecules were [M + H - Glu]+ and [M - H - Glu]-, respectively, formed by the loss of the glucuronide moiety. The measured limits of detection indicated that ESI is a significantly more efficient ionization method than APCI in the negative and positive ion modes for the compounds studied. MS/MS was found to be less sensitive, but more reliable and simple than MS due to the absence of chemical noise.

Algorithms↗
PubMed2006

Atomization of hydride with a low-temperature, atmospheric pressure dielectric barrier discharge and its application to arsenic speciation with atomic absorption spectrometry.

This paper describes a novel hydride atomizer based on atmospheric pressure dielectric barrier discharge (DBD) plasma. The plasma was generated with a 3700-V, 20.3-kHz, and 5-W electrical power supply and easily sustained with inert gases (He or Ar) at a flow rate of 250 mL.min(-1) after optimization. However, it cannot be sustained with N2. This atomizer offers the advantages of low operation temperature and low power consumption in comparison with the currently used electrothermal quartz atomization operated at 900 degrees C with a power supply of several hundred watts. To confirm the utility of the proposed atomizer, four arsenic species (As(III), As(V), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA)) were determined by the present atomization technique. A hyphenation of HPLC coupled to hydride generation AAS with the optimized DBD atomizer has been successfully used for the speciation of arsenic in order to demonstrate the potential of this atomizer in the present study. The characteristics of the DBD atomizer and the effects of different parameters (discharge gas, gas flow rate, voltage, HCl concentration, KBH4 concentration) are discussed in the paper. Compared with other hydride atomization techniques, the proposed method shows the following features: (1) small size (70 mm x 15 mm x 5 mm), which is preferable for the miniaturization of the total analytical system; (2) low power consumption (< or =5 W), which indicates the possibility of the development of portable, fieldable analytical instrumentation for in situ detection using battery as power supply; (3) low atomizer temperature (approximately 70 degrees C), which is in favor of the compactness of the total instruments; (4) avoidance of residue moisture removal in comparison with the existed GD system, which leads to the facility of the system. The analytical figures of the present technique were evaluated. The detection limits of As(III), As(V), MMA, and DMA obtained with HG-DBD-AAS were 1.0, 11.8, 2.0, and 18.0 microg.L(-1), respectively. The accuracy of the system was verified by the determination of arsenic in reference material of orchard leaves SRM 1571. The concentration of As determined by the present method agreed well with the reference values. The speciation of arsenic in the freeze-dried urine SRM 2670 were carried out, and the results obtained were in agreement with the results of HPLC-ICPMS and the reported values by other laboratories.

Journal Article↗
PubMed2006

Miniature differential mobility spectrometry using atmospheric pressure photoionization.

Positive and negative ion spectra have been obtained with a miniature differential mobility spectrometer equipped with a photoionization source operating at atmospheric pressure. With benzene as a dopant, providing C6H6+ as reactant ion, protonated molecular ions and proton-bound dimer ions were obtained with dimethyl methylphosphonate and butanone. The spectra obtained from gas chromatographic injections of aromatic hydrocarbons, benzene, toluene, and the xylenes, produced the molecular ions when the moisture level was very low, but at a high level the hydrated proton was also present. Possible mechanisms for the formation of protonated products are discussed. Negative ions were produced from electron capture by sulfur hexafluoride using benzene or acetone as dopant. Photoionization of nitrogen dioxide led to the formation of the nitrate ion whose yield was a nonlinear function of concentration. The use of a suitable dopant enhanced ion formation by up to 2 orders of magnitude, and limits of detection in both the positive and negative modes were all at the sub ppm(v) level. The study makes a strong case for the use of a photoionization source as an alternative to the radioactive 63Ni source.

Journal Article↗
PubMed2000

A novel approach for sensitivity enhancement in atmospheric pressure chemical ionisation liquid chromatography/mass spectrometry of chlorophylls.

Differences in the ionisation efficiency of chlorophylls and their phaeophytin counterparts result in lower sensitivity for atmospheric pressure chemical ionisation mass spectrometric detection of the former. Improvement in the sensitivity of detection of chlorophyll of around an order of magnitude at a concentration of 1 x 10(-6)mol L(-1) has been achieved using post-column addition of methanoic acid during analysis by liquid chromatography/mass spectrometry (LC/MS). The method gives linear response and is a simple strategy to improve sensitivity both for LC/MS and LC/MS/MS without loss of information relating to the precise nature of the tetrapyrrole distributions. Detection levels achieved exceed those obtained by absorbance detection.

Chlorophyll↗