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PubMed2004

Distinguishing N-oxide and hydroxyl compounds: impact of heated capillary/heated ion transfer tube in inducing atmospheric pressure ionization source decompositions.

In the pharmaceutical industry, a higher attrition rate during the drug discovery process means a lower drug failure rate in the later stages. This translates into shorter drug development time and reduced cost for bringing a drug to market. Over the past few years, analytical strategies based on liquid chromatography/mass spectrometry (LC/MS) have gone through revolutionary changes and presently accommodate most of the needs of the pharmaceutical industry. Among these LC/MS techniques, collision induced dissociation (CID) or tandem mass spectrometry (MS/MS and MS(n)) techniques have been widely used to identify unknown compounds and characterize metabolites. MS/MS methods are generally ineffective for distinguishing isomeric compounds such as metabolites involving oxygenation of carbon or nitrogen atoms. Most recently, atmospheric pressure ionization (API) source decomposition methods have been shown to aid in the mass spectral distinction of isomeric oxygenated (N-oxide vs hydroxyl) products/metabolites. In previous studies, experiments were conducted using mass spectrometers equipped with a heated capillary interface between the mass analyzer and the ionization source. In the present study, we investigated the impact of the length of a heated capillary or heated ion transfer tube (a newer version of the heated capillary designed for accommodating orthogonal API source design) in inducing for-API source deoxygenation that allows the distinction of N-oxide from hydroxyl compounds. 8-Hydroxyquinoline (HO-Q), quinoline-N-oxide (Q-NO) and 8-hydroxyquinoline-N-oxide (HO-Q-NO) were used as model compounds on three different mass spectrometers (LCQ Deca, LCQ Advantage and TSQ Quantum). Irrespective of heated capillary or ion transfer tube length, N-oxides from this class of compounds underwent predominantly deoxygenation decomposition under atmospheric pressure chemical ionization conditions and the abundance of the diagnostic [M + H - O](+) ions increased with increasing vaporizer temperature. Furthermore, the results suggest that in API source decompostion methods described in this paper can be conducted using mass spectrometers with non-heated capillary or ion transfer tube API interfaces. Because N-oxides can undergo in-source decomposition and interfere with quantitation experiments, particular attention should be paid when developing API based bioanalytical methods.

Journal Article↗
PubMed2004

Mass spectrometry of N-linked oligosaccharides using atmospheric pressure infrared laser ionization from solution.

An atmospheric pressure (AP) infrared (IR) laser ionization technique, implemented on a quadrupole ion trap mass spectrometer, was used to analyze underivatized, N-linked oligosaccharides in solution. Experiments were conducted on an atmospheric pressure infrared ionization from solution (AP-IRIS) ion source which differed from previous AP IR matrix-assisted laser desorption/ionization (MALDI) interfaces in that the ion source operated in the absence of an extraction electric field with a higher power 2.94 microm IR laser. The general term 'IRIS' is used as the mechanism of ionization differs from that of MALDI, and is yet to be fully elucidated. The AP-IRIS ion source demonstrated femtomole-level sensitivity for branched oligosaccharides. AP-IRIS showed approximately 16 times improved sensitivity for oligomannose-6 and the core-fucosylated glycan M3N2F over optimal results obtainable on a AP UV-MALDI with a 2,4,6-trihydroxyacetophenone matrix. Comparison between IR and UV cases also showed less fragmentation in the IR spectrum for a glycan with a conserved trimannosyl core, core-substituted with fucose. A mixture of complex, high-mannose and sialylated glycans resulted in positive ion mass spectra with molecular ion peaks for each sugar. Tandem mass spectrometry of the sodiated molecular ions in a mixture of glycans revealed primarily glycosidic (B, Y) cleavages. The reported results show the practical utility of AP-IRIS while the ionization mechanism is still under investigation.

Air Pressure↗
PubMed2003

Liquid chromatography/mass spectrometric determination of patulin in apple juice using atmospheric pressure photoionization.

This paper describes a comparison between atmospheric pressure chemical ionization (APCI) and the recently introduced atmospheric pressure photoionization (APPI) technique for the liquid chromatography/mass spectrometric (LC/MS) determination of patulin in clear apple juice. A column switching technique for on-line extraction of clear apple juice was developed. The parameters investigated for the optimization of APPI were the ion source parameters fragmentor voltage, capillary voltage, and vaporizer temperature, and also mobile phase composition and flow rate. Furthermore, chemical noise and signal suppression of analyte signals due to sample matrix interference were investigated for both APCI and APPI. The results indicated that APPI provides lower chemical noise and signal suppression in comparison with APCI. The linear range for patulin in apple juice (correlation coefficient >0.999) was 0.2-100 ng mL(-1). Mean recoveries of patulin in three apple juices ranged from 94.5 to 103.2%, and the limit of detection (S/N = 3), repeatability and reproducibility were 1.03-1.50 ng mL(-1), 3.9-5.1% and 7.3-8.2%, respectively. The total analysis time was 10.0 min.

Beverages↗
PubMed2005

Ion/molecule reactions in the orifice-skimmer region of an atmospheric pressure Penning ionization mass spectrometer.

Atmospheric pressure Penning ionization mass spectra of methanol were measured as functions of Ar or He gas pressure in the first vacuum chamber, the position of the skimmer, and the voltage applied between the orifice and the skimmer. When the orifice and the skimmer were coaxial with a distance of 4 mm, the distribution of CH3OH2+(CH3OH)n clusters was only weakly dependent on both Ar pressure (in the range of 19-220 Pa) and orifice-skimmer voltage (in the range of 1-45 V). The ion/molecule reaction CH3OH2+ + CH3OH --> CH3+(CH3OH) + H2O was observed in the free jet expansion, especially at high orifice-skimmer voltage values. When the orifice and the skimmer were off-centered and the distance between them was increased to 18 mm, the formation of large CH3OH2+(CH3OH)n clusters, as well as their dissociation, were seen. The endothermic proton transfer reaction, CH3+(CH3OH) + CH3OH --> CH3OH2+ + CH3OCH3, occurred at high orifice-skimmer voltage. The collision-induced dissociation of cluster ions by He gas in the first vacuum chamber was much more efficient than by Ar. These results demonstrated that the mass spectra are highly dependent on skimmer position and on orifice-skimmer voltage and that ions observed by mass spectrometry do not necessarily reflect the abundance of ions produced in the atmospheric pressure ion source.

Journal Article↗
PubMed2006

Characterization of typical chemical background interferences in atmospheric pressure ionization liquid chromatography-mass spectrometry.

The structures and origins of typical chemical background noise ions in positive atmospheric pressure ionization liquid chromatography/mass spectrometry (API LC/MS) are investigated and summarized in this study. This was done by classifying chemical background ions using precursor and product ion scans on most abundant background ions to draw a family tree of the commonly occurring chemical background ions. The possible structures and the origins of the major chemical background noise are clearly revealed in the family trees. In agreement with some suggestions in the literature, the chemical background ions studied so far can be classified mainly as either ions of contaminants (or their degradation fragments) or cluster-related ones. A significant contribution from the contaminants (airborne, from tubing and/or solvents) from plasticizer additives (phthalates, phenyl phosphates, sebacates and adipates, etc.) and silicones is concluded. These ions of contaminants can also serve as nuclei for the clustering of HPLC solvent or additives, such as water and acetic acid, thereby leading to a second family of background ions. This study explains the persistence of some chemical background noise even under fairly strong declustering conditions in API LC/MS. One of the other interesting conclusions is that there is a clear difference in structures between the chemical background ions and the protonated analytes generated under atmospheric pressure ionization. This conclusion will contribute to the on-going research efforts to exclusively remove or reduce the interference of chemical background noise in API LC/MS.

Journal Article↗
PubMed2002

Determination of selected sulfonamide antibiotics and trimethoprim in manure by electrospray and atmospheric pressure chemical ionization tandem mass spectrometry.

A method for the determination of sulfonamides and trimethoprim in the complex matrix liquid manure has been developed using reversed-phase liquid chromatography and atmospheric pressure chemical ionization (APCI) tandem mass spectrometry. A comparison was made between electrospray and atmospheric pressure chemical ionization. APCI proved to be more robust and less sensitive to matrix effects. High-performance liquid chromatographic (HPLC) separation of the analytes was achieved in less than 7 min. The compounds were extracted with ethyl acetate and the extracts were cleaned up by solid-phase extraction on an aminopropyl column. Recoveries were not dependent on the concentration level. The mean recoveries were as follows: trimethoprim 79.0%, sulfadiazine 80.5%, N(4)-acetylsulfadiazine 91.0%, sulfamerazine 78.6%, sulfadimidine 77.2% and sulfamethoxazole 82.8%. Linearity was established over a concentration range of 5 to 5000 microg/kg with correlation coefficients greater than 0.99. The method had a limit of quantitation (LOQ) of 5 microg/kg manure.

Animals↗
PubMed2002

Influence of the eluent composition on the ionization efficiency for morphine of pneumatically assisted electrospray, atmospheric-pressure chemical ionization and sonic spray.

A comparative study of three atmospheric-pressure ionization (API) sources for liquid chromatography/mass spectrometry (LC/MS), namely pneumatically assisted electrospray or ionspray (IS), atmospheric-pressure chemical ionization (APCI), and sonic spray (SS), with respect to the influence of the eluent composition on the ionization of morphine, is presented. The effect of organic modifiers, volatile acids, and buffer systems (with and without pH adjustment) in the LC mobile phase on the ionization efficiency of each interface is described. We conclude that for all three ion sources, the composition of the liquid phase had a serious impact on the ionization of the target compound. For IS and SS, very similar behavior towards the LC eluent was observed. In both cases, an increase in organic modifier resulted in an increase in ionization, while an increasing amount of volatile acid or buffer caused signal suppression. APCI, on the other hand, proved to respond completely differently towards the changes in the eluent. Again, an increased ionization was observed with an increase in organic modifier content but this time also in the presence of mobile phase additives like acids or buffers. Finally, we concluded that APCI proved to be the preferred ion source for the test compound because of its robust character and its direct applicability in traditional LC analysis.

Chromatography, Liquid↗
PubMed2003

Positive and negative gas-phase ion chemistry of chlorofluorocarbons in air at atmospheric pressure.

This paper presents a report on the ionization/dissociation of some representative chlorofluorocarbons (CFCs) induced by corona discharges in air at atmospheric pressure. Both positive and negative ions formed from Freons 1,1,1-trichlorotrifluoroethane (CFC 113a), 1,1,2-trichlorotrifluoroethane (CFC 113), and 1,1,1,2-tetrachlorodifluoroethane (CFC 112a) were analyzed using an atmospheric pressure chemical ionization mass spectrometry (APCI-MS) instrument. Energy-resolved mass spectra were obtained by modulating the kinetic energy of the ions via adjustment of the sampling cone potential (V(cone)). Positive ion spectra of the CFCs (M) at low V(cone) show no signals due to either M(+)* or MH(+) but only those due to species [M - Cl](+) and CX(3)(+) (X = Cl, F), likely formed via C-Cl and C-C bond cleavages following ionization via charge exchange. Charge localization in the products of C-C bond cleavage in M(+)* is driven by the stability of the neutral fragment. At low V(cone) the hydrates [M - Cl](+)(H(2)O) are also observed. In the case of 1,1,2,-trichlorotrifluoroethane, [M - F](+) species also form as a result of ion-molecule reactions. As V(cone) is increased collision-induced dissociation of [M - Cl](+) and [M - F](+), i.e., the perhalogenated cations C(2)X(5)(+) (X = Cl, F), takes place via carbene elimination. In some cases such elimination is preceded or accompanied by rearrangements involving transfer of halogen from one carbon to the other. Evidence is also presented for the occurrence of a condensation reaction of C(2)Cl(3)F(2)(+) with water to form a C(2)Cl(2)F(2)HO(+) species via elimination of HCl. Negative ion spectra are dominated by Cl(-) and its ion-neutral complexes with M and with water. Additional components of the plasma include ion-neutral complexes O(3)(-)(M), the molecular anion M(-) (observed only with 1,1,2-trichlorotrifluoroethane), and an interesting species corresponding to [M - Cl + O](-). The origin and structure of these [M - Cl + O](-) species are discussed in terms of available thermochemical and reactivity data and current mechanistic views concerning reaction of O(2)(-) with halogenated compounds. The observation of both positive and negative ions containing oxygen is of special relevance to development of new processes for the treatment of volatile organic compounds (VOCs) based on oxidative decomposition induced by corona discharges in air at room temperature and pressure.

Journal Article↗
PubMed1999

Effects of atmospheric pollution on a Lichenophagous lepidopteran.

Terrestrial epiphytic algae were used to absorb atmospheric pollutants and this material was then fed to larvae of a bagmoth to assess the toxicological effects of the pollutants. Samples of algae were amended with pesticides to simulate agricultural spray drift and with vehicle exhaust gases to simulate road traffic emissions. Larval mortality, immobilization, and feeding were used as the toxicological endpoints. Feeding was the most sensitive of these, but clear dose-response relationships were observed with all three endpoints. The effects of atmospheric pollution on an impacted environment were then investigated using these organisms. Algal samples were collected along a transect that included an area of arable farming, a motorway, and a woodland. Feeding was reduced when the larvae were fed algae from the areas proximal to the arable land and to the motorway. It is suggested that pesticide spray drift and vehicle exhaust emissions may have been the causal agents for these effects.

Air Pollutants↗
PubMed1998

The biogeochemistry of an ombrotrophic bog: evaluation of use as an archive of atmosphere mercury deposition.

The utility of ombrotrophic bogs as archives of atmospheric mercury deposition was assessed with an investigation in Arlberg Bog, Minnesota, U.S.A. Since the use of ombrotrophic bogs as archives depends on the immobility of deposited trace metals, we examined the postdepositional transport processes revealed by the solid-phase distributions of mercury and ancillary metals (Fe, Al, Mn, and Pb) in this bog. We modeled metal speciation in bog porewaters as a function of pe in order to understand metal behavior in ombrotrophic peat. Specifically, we considered the effect of water movement and resultant shifts in redox potential gradients on metal retention. Our results indicate that Hg and Pb are immobile in ombrotrophic peat, so their distribution can be used to determine temporal changes in deposition. To substantiate the deposition estimates determined in this study, we emphasized the importance of confirming the validity of the dating scheme, assessing the degree of horizontal homogeneity in the accumulation record, and providing evidence for retention of Hg based on geochemical modeling. As recorded in Arlberg Bog, historic atmospheric Hg deposition increased gradually after the mid-1800s, peaked between 1950 and 1960, and may have declined thereafter. Preindustrial deposition was about 4 micrograms/m2 year and recent deposition about 19 micrograms/m2 year. The results of this study indicate that deposition at Arlberg Bog has been influenced by a regional and/or local-scale source.

Air Pollutants↗
PubMed1999

Spectral Profiles for Atmospheric Absorption by Isolated Lines: A Comparison of Model Spectra with P- and R-Branch Lines of CO in N(2) and Ar.

There is a need in atmospheric research to accurately model absorption profiles over a wide range of pressures and temperatures. Here we explore the suitability of four profiles to describe absorption by an isolated line. Three of the profiles, a Lorentzian, a Voigt profile, and a hard-collision model, are speed independent. The fourth profile is an empirical speed-dependent hard-collision model. We test the quality of the profile and the pressure dependence of the broadening by fitting to precise experimental absorption curves for CO broadened by N(2) and Ar. Of the four profiles, we find that only the empirical model is satisfactory. This profile also meets the need of atmospheric modeling in that it is easily evaluated. Copyright 1999 Academic Press.

Journal Article↗
PubMed1996

Potential health risks related to carcinogens in the atmospheric environment in India.

In India, rapid urbanization and industrialization have contributed positively toward meeting the materialistic needs of the citizens, but have also resulted in contamination of the atmospheric environment. This paper deals with the assessment of potential health risks posed by carcinogenic substances, namely cadmium, chromium, and nickel, present in certain atmospheric environments in India. Average air concentrations of these carcinogenic metals have been assessed for different states and regions of India (C. R. Krishnamurti and P. Vishwanathan, Toxic Metals in the Indian Environment, Tata/McGraw-Hill, New Delhi, 1991). Based on these assessments, both individual and societal risks have been estimated in different states of the country, and comparisons were made. Reported concentration, release sources, potential health risks including cancer risk estimates, and ambient air interim guidelines are discussed. The reported environmental releases and cancer risk from cadmium are minimal. There is a potential for increased respiratory cancer risk from exposure to chromium and nickel in some northern Indian states. These metals are irritants to nasal passages and the respiratory tract. Chromium is also corrosive to mucus membranes. They have the potential to cause chronic respiratory problems. Since it appears that these metals may cause some adverse health effects in humans, exposure to these ambient air pollutants should be minimized by managing the release of these contaminants to the environment. There is a need for the development and strict enforcement of national and state regulatory standards.

Air Pollutants↗
PubMed1995

Expression of Staphylococcus saprophyticus surface properties is modulated by composition of the atmosphere.

Expression of two major surface proteins of Staphylococcus saprophyticus, the haemagglutinin and the Staphylococcus saprophyticus surface-associated protein (Ssp), required carefully defined culture conditions. The Ssp is produced when bacteria are grown on agar, whereas expression of the haemagglutinin requires growth in broth. We sought to identify the environmental signals that are responsible for this modulation. Varying the pH, the osmolarity of the growth medium or the temperature did not influence expression of the proteins. In contrast, growth in an anaerobic atmosphere increased haemagglutination titres and fibronectin binding (both mediated by the haemagglutinin) but suppressed production of the Ssp. As the influence of the CO2 level could be excluded, we conclude that expression of these surface proteins is probably modulated by the O2 content of the atmosphere.

Adhesins, Bacterial↗
PubMed1996

A morphometric and functional study of the toxicity of atmospheric ammonia in the extrathoracic airways in pigs.

The effects of atmospheric ammonia (NH3) on the nasal and tracheal mucosa of pigs were investigated by morphometric and functional methods. Pigs were exposed to four concentrations of NH3 [5 (control), 25, 50 and 100 ppm] for 6 days in a specially designed air-pollutant exposure chamber. Samples were taken from the turbinates and the trachea, and the respiratory mucosa was examined by light and scanning electron microscopy. Dose-response curves to carbachol and isoproterenol were constructed using isolated strips of tracheal smooth muscle, with or without epithelium. In pigs exposed to ammonia, considerable mucosal injuries were observed in the turbinates but not in the trachea. The number of neutrophils in the epithelial layer and in the lamina propria, and epithelial hyperplasia were closely and significantly correlated with the concentrations of ammonia (r = 0.894, p < 0.001; r = 0.727, P < 0.001; and r = 0.818, p < 0.001, respectively). Except for the lamina propria, all these changes were significant (p < 0.05) at ammonia concentrations as low as 25 ppm. The percentage of the surface of the turbinate mucosa that was ciliated tended to decrease with increasing ammonia concentration (r = 0.439, p < 0.082). Ammonia induced smooth-muscle hyperresponsiveness to carbachol with a close linear correlation between individual values of the carbachol-induced maximal effect and the NH3 concentrations (r = 0.526, p < 0.003). While mechanical destruction of the epithelium induced an increase in Emax in the control group, no difference was observed between the intact and denuded strips from animals exposed to ammonia. The response to isoproterenol was not influenced by ammonia. It was concluded that quantitative histological analysis of the inflammatory infiltration and epithelial hyperplasia in the turbinates is a useful tool for quantifying the effects of atmospheric pollutants in pigs; a 6-day exposure to ammonia induces nasal irritation and functional disturbances of the tracheal smooth-muscle contractions at concentrations as low as 25 ppm.

Adrenergic beta-Agonists↗
PubMed1986

Phthalic acid excretion as an indicator of exposure to phthalic anhydride in the work atmosphere.

The concentration of phthalic acid was determined in the urine of nine subjects occupationally exposed to phthalic anhydride. For the determination, the urine samples were acidified, extracted with dimethyl ether, esterified with boron trifluoride/methanol and measured by electron capture gas chromatography. Environmental air samples were collected in Tenax tubes, eluted with methyl-t-butyl ether and assayed by electron capture gas chromatography. Significant correlations were found between the concentration in urine samples (range: 0.3-14.0 mumol/mmol creatinine), collected at different times of the day, and the time-weighed average atmospheric concentrations (range: 0.03-10.5 mg/m3). No conjugation of phthalic acid in the urine was observed. The detection limit for urine samples (10 ml) was 0.05 mumol/l) and that for air samples 0.4 microgram/m3. The method has potential for biological monitoring of workers exposed to phthalic anhydride. It was found that at atmospheric anhydride concentrations of about 30% of the hygienic reference value (6 mg/m3), which is applied in many market economies, a body-burden was caused which was not eliminated overnight.

Body Burden↗
PubMed1977

Influence of emulsion type and atmospheric oxygen on the fading of latent image in electron microscopic radioautography.

The intensity of radioautographic reactions in Ilford L4, Sakura NR-H2 and Kodak NTE emulsions was compared after exposure in either dry air or dry helium gas at 4 degrees C to test the stability of latent images in the presence or absence of oxygen. A light proof container is described in which slides bearing radioactive sections coated with the three emulsions were exposed in dry helium at a constant pressure of approximately 0.5 atm. The comparison of air and helium atmospheres during exposure of radioautographs was estimated qualitatively for 125I-labeled thyroid sections stored for several years and, in addition, quantitative data was derived from 3H-labeled methacrylate sections stored from 21 days to 1 year. With the three emulsions under study, the background fog remains low under both exposure conditions at 4 degrees C for as long as several years duration. Using L4 emulsion, similar high grain densities are obtained in air and helium, and therefore, the latent images in L4 emulsion remain stable in the presence of oxygen. In the case of NTE and NR-H2 emulsions, as the exposure time increases, substantially lower reaction intensities are observed in air than in helium. This difference in reaction intensity is evident by 3 weeks with NTE and after 4 weeks with NR-H2. Hence, there is fading of the latent images in the latter emulsions in the presence of oxygen. It is concluded that reliable results may be obtained with the L4 emulsion by exposure of radioautographs in dry air, whereas with the NR-H2 and NTE emulsions, exposure should be in an oxygen-free medium, such as is provided by a dry helium atmosphere.

Autoradiography↗
PubMed1982

Formation of amino acids from models of Titan and more oxidized atmospheres.

Protein and non-protein amino acids were synthesized following hydrolysis of products obtained by high frequency discharge techniques applied to model atmospheres consisting of N2 as a nitrogen source together with CH4 and/or CO2 as a carbon source. Highest yields were obtained in the absence of CO2 and from mixtures rich in CH4. Amino acids would indeed be expected on the frozen surface of Titan with its CH4-N2 atmosphere.

Amino Acids↗