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PubMed2005

Methyl benzoate as a marker for the detection of mold in indoor building materials.

A convenient analytical method to quantify volatile organic compounds (VOCs) emitted from various building materials has not been addressed yet. This work presents a new and rapid automated method using SPME combined with GC/MS. Methyl benzoate - as a metabolic biomarker for mold growth-was used to indicate VOCs and to determine and assess mold growth on damp samples. Gypsum board and wall-board paper were used as examples of common indoor building materials. Optimized extraction conditions were carried out manually, using a GC/flame ionization detector. Moldy samples were analyzed using an automated SPME-GC/MS analysis under optimized conditions. The amount of methyl benzoate emitted from the studied samples ranged from 32 to 46 ppb, where the density of the fungal biomass was found to be 8 x 10(4) cells/mL. A relationship between the amount of fungal biomass and the emitted concentration of methyl benzoate was found and assessed based upon cultured mold samples taken from indoor building sites. The analytical method shows promise for the compound methyl benzoate, which can easily be identified at low detection limits (LOD = 3 ppb) and good linearity (>0.988), and its extraction and detection can be accomplished cleanly by current extraction techniques. Results suggest that this method with easy sample preparation can be used for quantitation and, of importance, minimal matrix effects are observed.

Air Microbiology↗
PubMedDate not supplied

Quantitative analysis of flavonol glycosides in Ginkgo biloba: a comparison of two analytical methods.

A comparison of testing methods for constituents of Ginkgo biloba was performed as part of the process for determining which of the many available analytical methods was most appropriate for inclusion in the American Herbal Pharmacopoeia (AHP). Three primary methods were reviewed: those adopted by the European Pharmacopoeia, the National Science Foundation-Institute for Nutraceutical Advancement (NSF-INA) and the United States Pharmacopeia. Methods were compared by evaluating sample preparation and hydrolysis, precision and methods of total flavonol glycoside calculation by two independent laboratories. The AHP adopted the method of NSF-INA for inclusion in the AHP monograph owing to observed superiority of this method in terms of precision, glycoside calculation, ease of sample preparation and chromatographic parameters.

Chromatography, High Pressure Liquid↗
PubMed2005

Analysis of tetracyclines in honey by high-performance liquid chromatography/tandem mass spectrometry.

A confirmatory method coupling liquid chromatography to tandem mass spectrometry (LC/MS/MS) is described for the determination of tetracycline, oxytetracycline, doxycycline and chlortetracycline in honey. Demeclocycline, another tetracycline molecule not reported for its usage in honey, was used as internal standard to quantify the four analytes. The sample preparation entails a clean-up on an Oasis HLB solid-phase extraction cartridge and analyses were realised by LC/MS/MS in selected reaction monitoring mode. The stability of tetracyclines was checked under various storage conditions at -20, +4 and +20 degrees C (both under dark and light exposures). Indeed, tetracyclines are not stable molecules and the epimerisation phenomenon was evaluated in this work. Appropriate correction factors of the MS/MS responses of each epimer were studied for each of the four tetracyclines to accurately quantify them. Moreover, the matrix effects encountered during the LC/MS/MS analyses were also studied in spiked experiments from blank honey samples of various geographical origins and different flower types.

Anti-Bacterial Agents↗
PubMed1985

Determination of alpha-amanitin and beta-amanitin in human biological fluids by high-performance liquid chromatography.

A high-performance liquid chromatographic assay of alpha-amanitin and beta-amanitin in human serum, urine, or stomach washings is described. Sample preparation involves a chemical step with deproteinization and organic solvent treatment, and a selective cleanup and concentration step on reversed-phase prepacked cartridges. Separations are performed on a reversed-phase analytical column under isocratic conditions with uv detection at 280 nm. The method allows the quantitation of alpha- and beta-amanitin separately with a detection limit of 10 ng/ml for both toxins.

Amanitins↗
PubMed1981

Countercurrent chromatography.

Countercurrent chromatography is a newly developed versatile partition chromatography which totally eliminates the use of solid supports. The method utilizes the intriguing hydrodynamic behavior of two immiscible solvents in a rotating coiled tube. Various types of seal-free flow-through centrifuge schemes are introduced to facilitate a continuous elution process. The method yields high partition efficiencies comparable to liquid chromatography but without the complications arising from the use of solid supports. Countercurrent chromatography covers a wide spectrum of applicable samples ranging from small ions and molecules to macromolecules and even cell particles in both analytical and preparative scales.

Acceleration↗
PubMed1984

Separation and determination of the two components of glycerol formal by high-performance liquid chromatography.

The two isomeric components of glycerol formal, 1,3-dioxan-5-ol and 1,3-dioxolane-4-methanol, are marginally separated (Rs = 1.0) by polar-bonded-phase high-performance liquid chromatography (HPLC) on a cyanopropyl column with acetone-hexane as the eluent. Esterification of these components with 3,5-dinitrobenzoyl chloride produces derivatives which are, however, completely resolved (Rs > 2) by normal-phase HPLC on silica; derivatization has the added advantage of introducing an ultraviolet-absorbing chromophore into each component. Preparative scale chromatography is used to isolate each of the derivatives, which are characterized by their UV, NMR and mass spectral properties. These esters are used as reference standards for an analytical method based on derivatization and normal-phase chromatography. In this way a sample of glycerol formal is calibrated for use as a standard in the direct determination of the two components by polar-bonded-phase HPLC.

Journal Article↗
PubMed2006

Analysis of volatiles in water using headspace solid-phase microcolumn extraction.

A rapid solvent-free sample preparation method is presented in which volatilized organic substances are extracted via a solid-phase microcolumn mounted on a gas-tight syringe by the aspiration of an appropriate volume of headspace (tens of millilitres) of the sample under investigation. The microcolumn with the analytes concentrated on an adsorbent material is then transferred to the analytical instrument for desorption and analysis. The instrumental set-up consists of a Twister desorption unit (Gerstel) mounted on an Agilent 6890 GC system equipped with a CIS 4 programmed temperature vaporiser injector and coupled with an Agilent 5973 MS system. The instrumentation is slightly modified in comparison with the analysis made with a twister (stir bar coated with a layer of polydimethylsiloxane) after stir bar sorptive extraction and, thus, its utilization has been extended. For volatiles in water, the method is applicable to the qualitative screening at the microg/l to sub-microg/l level and to the quantitative determination at the ng/l level.

Chromatography, Gas↗
PubMed2006

Liquid-phase micro-extraction techniques in pesticide residue analysis.

Modern trends in analytical chemistry are towards the simplification and miniaturization of sample preparation, as well as the minimization of organic solvent used. In view of this aspect, several novel micro-extraction techniques are being developed in order to reduce the analysis step, increase the sample throughput and to improve the quality and the sensitivity of analytical methods. One of the emerging techniques in this area is liquid-phase micro-extraction (LPME). It is a miniaturized implementation of conventional liquid/liquid extraction (LLE) in which only microliters of solvents are used instead of several hundred milliliters in LLE. It is quick, inexpensive and can be automated. In the last few years, LPME has been combined with liquid chromatography (LC) and capillary electrophoresis (CE), besides the generally used coupling to gas chromatography (GC), and has been applied to various matrices, including biological, environmental, and food samples. This work is aimed at providing an overview of the major developments of LPME, coupled with chromatography and CE, as reported in the literature. The paper will focus on the application of the technique to different matrices and the aim is to reveal the panorama of opportunities and to try to indicate the potential of LPME in pesticide analysis. A critical review of the first applications to pesticide analyses is presented in the main part of the manuscript. The optimization of LPME as well as advantages and disadvantages are discussed. It is concluded that, because of its high pre-concentration factor, LPME can be introduced with benefit into water analysis for several pesticide groups. In particular, the application of LPME to non-polar pesticides in environmental analysis appears to be promising. However, similar to other micro-extraction techniques, such as solid phase micro-extraction (SPME), serious limitations still remain when analyzing semi-solid and solid environmental, food or biological matrices and/or highly polar compounds. Thus, other pre-concentration techniques may be a good alternative if an analytical problem cannot be sufficiently dealt with LPME.

Chromatography, Liquid↗
PubMed2006

19F NMR as a powerful technique for the assay of anti-psychotic drug haloperidol in human serum and pharmaceutical formulations.

19F nuclear magnetic resonance was used as a suitable analytical tool for the identification and selective determination of haloperidol in human serum and pharmaceutical preparations. The method is based on the integration of appropriate signals of haloperidol and trifluoroacetic acid as an internal standard. The proposed method is a rapid and facile, while without any sample pretreatment, manipulation of large samples and lengthy instrument time. The regression equation for haloperidol in human serum showed a good linearity in the range of 60-600 microg ml(-1) with a detection limit of 1.4 microg ml(-1). The mean recovery results on human serum samples ranged from about 96-103%, with relative standard deviations <8%. The method was also applied successfully to the determination of haloperidol in real pharmaceutical samples, and compared with the results obtained by a reference method. The drug's degradation was studied by the proposed method in hydrochloric acid media and main products were identified.

Antipsychotic Agents↗
PubMed2003

Extraction methods for lipopolysaccharides from Escherichia coli ATCC 25922 for quantitative analysis by capillary electrophoresis.

Lipopolysaccharides (LPS) are major constituents of the cell wall of Gram-negative bacteria. Capillary zone electrophoresis (CZE) was applied to distinguish between lipopolysaccharides extracted from Escherichia coli ATCC 25922 with various techniques. Extraction methods proposed by Westphal and Jann [Methods Carbohydr. Chem. 5 (1965) 83], Galanos et al. [Eur. J. Biochem. 9 (1969) 245], Ni Eidhin and Mouton [FEMS Microbiol. Lett. 110 (1993) 133] and Nichols [Infect. Immun. 62 (1994) 3753] for LPS preparation were evaluated. Electrophoresis buffers with varying pHs were applied to assess the structure stability of the extracted LPS samples. Variations in structural breakdown were apparent demonstrating that different extraction methods removed different LPS molecules. Furthermore, the results obtained proved the CZE useful as an analytical technique for LPS evaluation. The LPS removed with the Nichols extraction procedure presented a unique electrophorogram that could in future be applied in the rapid identification of Gram-negative foodborne pathogens.

Electrophoresis, Capillary↗
PubMed2002

[Determination of iron and nickel in crude oils by emulsification technique-FAAS method].

The methyl isobutyl ketone-dimethyl benzene solution of sample was emulsified into emulsion by emulsifier Triton X-100. The standard addition method was used to determine with polyisobutylene emulsion as the reference. An analytical method for rapid determination of iron and nickel in crude oils by FAAS had been developed. A principle and method of preparing blank solution had been advanced. Choices of solvent and emulsifier, preparing blank solution were studied. The determination results were consistent with those obtained by ashing method-FAAS.

English Abstract↗
PubMed1987

Influence of preanalytical factors on the atomic absorption spectrometry determination of trace elements in biological samples.

In the analysis of the concentration of trace elements in biological material there are many possible preanalytical sources of error. Precision and accuracy of trace element analyses are not so much determined by the analytical procedure--atomic absorption spectrometry--as by individual biological factors, contamination and loss of elements during sampling and sample preparation, influences resulting from the calibration procedure, or from the analytical equipment itself. Genetical factors like sex or race, ecological factors like age or pregnancy and short term factors like food intake, parenteral feeding or drug therapy can influence the final results. Different blood sampling methods with different duration and strength of compression may lead to hemolysis resulting in falsely elevated values of trace elements. Needles, syringes and tubes contribute to contamination by leaching trace elements from their walls or lead to loss of material by adsorption to the surface of the walls. As there is still no primary standard in order to guarantee precision and accuracy the calibration procedures have to be compared individually depending on the different matrices of the sample.

Calibration↗
PubMed1999

Opiate detection in saliva and urine--a prospective comparison by gas chromatography-mass spectrometry.

UNLABELLED: There is an increasing interest in saliva as an alternative analytic body fluid. OBJECTIVE: This study sought to determine the correlation of opiates analyzed in saliva and corresponding urine. METHODS: A total of 130 adequate and 24 inadequate samples were collected from patients participating in drug withdrawal therapy. To obtain saliva from the oral cavity, a newly developed collection device (Clin Rep), consisting of a treated cotton roll and a centrifugation vial with a filter inset, was tested. For the preparation of a purified solution of urine, liquid extraction was used. Solid phase extraction was utilized to prepare the saliva samples. For the detection by gas chromatography-mass spectrometry, an appropriate derivatization was necessary using N-methyl-N-(trimethylsilyl)trifluoroacetamide. The retention times were compared with defined standard solutions. The obtained mass spectra showed a characteristic fragmenting pattern and offered a reliable identification. RESULTS: The concordance of the analytic results of the saliva samples with urine was 93% for a decision limit of 100 ng/mL and 98% for a decision limit of 300 ng/mL (DHHS opiate cutoff) in urine. CONCLUSIONS: Saliva, of adequate amount in 85% of samples, may be appropriate for analysis of drugs of abuse.

Gas Chromatography-Mass Spectrometry↗
PubMed2002

Validated HPLC method for the determination of tinidazole in human serum and its application in a clinical pharmacokinetic study.

A high performance liquid chromatographic (HPLC) method for the determination of tinidazole in human serum using metronidazole as internal standard (IS) is described. Protein precipitation is used for the preparation of sample. Mobile phase consisting of 0.002 M phosphate buffer, methanol and acetonitrile mixture (85:7.5:7.5/v/v/v) was used at a flow rate of 1 ml/min on a C18 column. The eluate was monitored using an UV/Vis detector set at 320 nm. Ratio of peak area of analyte to IS was used for quantification of serum samples. The absolute recovery was greater than 95% over a concentration range of 0.5 to 30 micrograms/ml and the limit of quantitation was 0.05 microgram/ml. The intra-day relative standard deviation (RSD) measured at 0.5, 5, 15 and 30 micrograms/ml ranged from 0.36 to 6.14%. The inter-day RSD ranged from 1.14 to 4.21%. The method is simple, sensitive and has been successfully used in a pharmacokinetic study conducted in healthy human volunteers.

Antitrichomonal Agents↗
PubMed2006

Solvent-free MALDI-MS: developmental improvements in the reliability and the potential of MALDI in the analysis of synthetic polymers and giant organic molecules.

A dry sample preparation strategy was previously established as a new method for matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS), so-called solvent-free MALDI-MS. In this contribution, we examine systems that have been shown problematic with conventional solvent-based MALDI approaches. Problems frequently encountered are solubility, miscibility, and segregation effects during crystallization as a result of unfavorable analyte and matrix polarities. In all cases studied, solvent-free MALDI-MS simplified the measurement and improved the analysis. Solvent-free MALDI-MS enables more reliable results in well-known problematic systems such as polydimethylsiloxane with its segregation effects. However, even in highly compatible analyte/matrix systems such as polystyrene and dithranol, there were undesirable suppression effects when employing THF as solvent. Generally, the solvent-free method allows for more homogeneous analyte/matrix mixtures as well as higher shot-to-shot and sample-to-sample reproducibility. As a result, less laser power has to be applied, which yields milder MALDI conditions, reduced background signals, and provides better resolution of the analyte signals. Solvent-free MALDI-MS proved valuable for the characterization of nanosized material, e.g., fullereno-based structures, which indicated having an increased fragmentation-susceptibility. New analyte/matrix combinations (e.g., polyvinylpyrrolidone/dithranol) are accessible independent of solubility and compatibility in common solvents. An improved quantitation potential is recognized (e.g., insoluble polycyclic aromatic hydrocarbon against soluble dendrite precursor). The rapid and easy measurement of industrial products demonstrates the solvent-free method capable for improved throughput analysis of a variety of compounds (e.g., poly(butylmethacrylate) diol) in routine industrial analysis. Hence, this new MALDI method leads to qualitative and quantitative improvements, making it a powerful tool for analytical purposes, which may also prove to be valuable in future automation attempts.

Organic Chemicals↗
PubMed2002

One step and highly sensitive headspace solid-phase microextraction sample preparation approach for the analysis of methamphetamine and amphetamine in human urine.

A fiber-stable, repeatable and highly sensitive headspace solid-phase microextraction (HS-SPME) method was developed for the analysis of methamphetamine (MA) and amphetamine (AM) in urine using gas chromatography-mass spectrometry (GC-MS) in the selected ion monitoring mode. For sample preparation, the test specimen was placed in a 7 ml vial along with the additives (KOH and NaCl) and the internal standards (d8-MA and d8-AM), a glass insert containing heptafluorobutyric anhydride (HFBA) and heptafluorobutyric chloride (HFBCl) as derivatizing reagents was inserted into the vial, the vial was then sealed tightly. A SPME device with a 100 microm polydimethylsiloxane fiber was inserted into the vial and the fiber was exposed to the headspace in the insert, then the vial was heated and stirred at 100 degrees C and 600 rpm for 20 min for evaporation/adsorption/derivatization. The vaporized analytes (AM and MA) in the vial diffused into the glass insert though the holes on the insert, they absorbed onto the fiber, and then interacted with the vapor of the derivatizing reagent. Some of the analytes in the headspace of the glass insert may react with the vapor of the derivatizing reagent first, and then adsorb onto the fiber. The needle was finally removed and inserted into the injection port to desorb the analytes with the fiber exposed to the liner of the GC-MS system for analysis. By combining HFBCl and HFBA as derivatizing reagents and placing them in an insert, the HS-SPME method achieves high sensitivity for the analysis of AM and MA. Correlation coefficients derived from typical calibration curves in the 1.0-1700 ng ml(-1) range are 0.998 for MA and 0.994 for AM. The limits of detection and the limits of quantitation using a sample size of 1 ml are 0.3 and 1.0 ng ml(-1), respectively, for both MA and AM in urine specimens. Because the water hydrolysis of derivatizing reagent is much faster than the acylation reaction of the primary and secondary amines with the derivatizing reagent, the amphetamines cannot be acylated effectively over heated aqueous solution, and therefore this study provides a new acylation design in moisture surroundings. The proposed process also simplifies the procedure for urine sample preparation, and makes the automation of SPME possible.

Amphetamine↗
PubMed1997

An isotope-dilution gas chromatography-mass spectrometry method for trace analysis of xylene metabolites in tissues.

A gas chromatography-mass spectrometry (GC-MS) method using isotope dilution was developed to measure trace levels of xylene metabolites in brain tissues. The primary metabolites of xylene are dimethylphenol (DMP), methylbenzyl alcohol (MBA), toluic acid (TA), and methylhippuric acid (MHA). The internal standard was a mixture of deuterated DMP-d3, TA-d7, and MHA-d7. DMP-d3 was commercially available and was used as the internal standard for both DMP and MBA. TA-d7 and MHA-d7 were biosynthesized by administering xylene-d10 to rats and collecting their urine. Based on the noise peaks in 10 blank samples, the on-column limits of quantitation (mean +10 SD of noise peaks) were approximately 305, 1220, 545, and 386 pg for DMP, MBA, TA, and MHA, respectively. Analyte detection and recovery tests from brain tissues of control rats were conducted by spiking the tissues with 32 nmol/g of each analyte, together with the deuterated metabolites. The tissues were homogenized, extracted with ethyl acetate, and derivatized by trimethylsilylation. One microliter of the sample was injected into the GC-MS. The recoveries of the analytes were 104 +/- 8%, 80 +/- 9%, 93 +/- 10%, and 92 +/- 11% (mean +/- SD, n = 7) for DMP, MBA, TA, and MHA, respectively. The tissue preparation efficiency, which was indicated by absolute recoveries of internal standards, was approximately 33% for DMP, MBA, and TA and approximately 80% for MHA. No metabolites were detected in untreated control tissues. This simple and sensitive method to simultaneously detect major xylene metabolites in brain tissues could also be used for the analysis of blood and urine samples from workers to monitor p-xylene exposure.

Animals↗
PubMed2005

Separation of proteins with a molecular mass difference of 2 kDa utilizing preparative double-inverted gradient polyacrylamide gel electrophoresis under nonreducing conditions: application to the isolation of 24 kDa human growth hormone.

A method for separating proteins with a molecular mass difference of 2 kDa using SDS-PAGE under nonreducing conditions is presented. A sample mixture containing several human growth hormone (hGH) isoforms was initially separated on a weak anion-exchange column. Fractions rich in 24 kDa hGH as determined by analytical SDS-PAGE were pooled and further separated by cation-exchange chromatography. The fractions pooled from the cation-exchange chromatography contained two hGH isoforms with a 2 kDa molecular mass difference according to SDS-PAGE analysis, 22 and 24 kDa hGH. The 22 and 24 kDa hGH were separated using continuous-elution preparative double-inverted gradient PAGE (PDG-PAGE) under nonreducing conditions. The preparative electrophoresis gel was composed of three stacked tubular polyacrylamide matrices, a 4% stacking gel, a 13-18% linear gradient gel, and a 15-10% linear inverted gradient gel. Fractions containing purified 24 kDa hGH were pooled and Western blot analysis displayed immunoreactivity to antihGH antibodies. PDG-PAGE provides researchers with an electrophoretic technique to preparatively purify proteins under nonreducing conditions with molecular mass differences of 2 kDa.

Chromatography↗