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PubMed1994

Multi-residue screening and confirmatory analysis of anabolic steroids in urine by gas chromatography coupled with tandem mass spectrometry.

The diversity of substances used illegally as growth promoters in meat production requires the development of multi-analyte methods of analysis involving a sample pretreatment step that is as rapid and as easy as possible, followed by a specific and sensitive determination of several residues within the same run. A general strategy for the screening and confirmatory analysis of fifteen artificial anabolic compounds in urine samples is described. It is based on solid-phase extraction on C18 Empore discs and amino-bonded columns followed, after derivatization (trimethylsilyl or methyloxime-trimethylsilyl derivatives), by gas chromatography coupled with collisionally activated dissociation tandem mass spectrometry.

Anabolic Agents↗
PubMed1989

Trace-level determination of 3'-azido-3'-deoxythymidine in human plasma by preconcentration on a silver (I)-thiol stationary phase with on-line reversed-phase high-performance liquid chromatography.

A method was developed for the determination of 3'-azido-3'-deoxythymidine (AZT) in plasma. The method is based on the trace enrichment of AZT on a pre-column packed with a silver-loaded thiol stationary phase at pH 11.6. On-line desorption to the reversed-phase liquid chromatographic system is performed by injecting a plug of 50 microliters of 1 M perchloric acid on the silver (I)-thiol pre-column. Two different sample pretreatment methods - protein precipitation with perchloric acid and on-line clean-up via a polymeric PRP-1 pre-column - were applied for the determination of AZT in human plasma. The latter method allows the direct injection of plasma samples into the analytical system and can therefore easily be automated. With both methods detection limits in the order of 10(-8) M AZT were obtained after preconcentration of 1.0 ml of plasma, using UV detection at 267 nm.

Autoanalysis↗
PubMed1987

Training effects on vowel production by two profoundly hearing-impaired speakers.

Two profoundly hearing-impaired adolescents received systematic speech training to improve their production of the vowels /i/ and /ae/. Acoustic measures of F1, F2, and duration, and listener judgements of vowel acceptability, were used to quantify vowel production before and after training. Both subjects demonstrated significant changes in their production of the two vowels at the acoustic and perceptual levels following treatment. The changes were highly individualized. For some features, significant improvement occurred posttreatment with differences between the hearing-impaired subject and a control group of subjects with normal hearing no longer present. There was a significant improvement in the acceptability of the two vowels in each subject's speech after training. Vowel duration remained unchanged in the speech of one subject whereas it increased in the speech of the other subject following training. There was a trend toward reduced token-to-token variation in the posttreatment samples. Acoustic and perceptual measures also were obtained on two vowels not directly trained in the program. Significant changes occurred in the production of these segments but some of the changes resulted in greater deviation in the post- than in the pretreatment samples.

Adolescent↗
PubMed2005

A QCM immunosensor for Salmonella detection with simultaneous measurements of resonant frequency and motional resistance.

A quartz crystal microbalance (QCM) immunosensor was described for the detection of Salmonella Typhimurium with simultaneous measurements of the resonant frequency and motional resistance. The immunosensor was fabricated using protein A for the antibody immobilization. High-frequency impedance analysis indicated that the changes in resonant frequency and motional resistance (DeltaF and DeltaR) of the QCM were significant while the changes in static capacitance, motional capacitance, and motional inductance were insignificant. In the direct detection of S. Typhimurium in chicken meat sample, DeltaF and DeltaR were proportional to the cell concentration in the range of 10(5) - 10(8) and 10(6) - 10(8) cells/ml, respectively. Using anti-Salmonella-magnetic beads as a separator/concentrator for sample pretreatment as well as a marker for signal amplification, the detection limit was lowered to 10(2) cells/ml based on the DeltaR measurement; however, DeltaF was not related to the cell concentration. No interference was observed from E. coli K12 or the sample matrix.

Bacterial Adhesion↗
PubMed2000

Method development for the determination of anthocyanins in red wines by high-performance liquid chromatography and classification of German red wines by means of multivariate statistical methods.

A simple and fast HPLC method without sample pretreatment is described for the separation of anthocyanins in red wines using a new pH-stable stationary phase. The linearity between peak area and concentration and ruggedness of the method were checked. Investigations were made about the safekeeping of red wine samples concerning anthocyanins. Classification of 52 different wine samples was performed by multivariate statistical methods.

Anthocyanins↗
PubMed1998

High-performance liquid chromatographic determination of ritonavir in human plasma, cerebrospinal fluid and saliva.

A simple, ion-pair high-performance liquid chromatographic method has been developed and validated for the quantitative determination of the HIV protease inhibitor ritonavir in human plasma, cerebrospinal fluid and saliva. Sample pretreatment consisted of precipitation of proteins with acetonitrile prior to high-performance liquid chromatography with ultraviolet detection at 239 nm. The method has been validated over the range of 50 ng/ml to 50 microg/ml with use of 100-microl volumes of sample. The currently described assay has been used successfully for the analysis of ritonavir in plasma, cerebrospinal fluid and saliva in HIV-1 infected patients.

Acquired Immunodeficiency Syndrome↗
PubMed2000

Liposomal lurtotecan (NX211): determination of total drug levels in human plasma and urine by reversed-phase high-performance liquid chromatography.

Lurtotecan (GI147211; LRT) is a semisynthetic and water-soluble analogue of the topoisomerase I inhibitor camptothecin. To determine whether the therapeutic efficacy of LRT in patients could be improved, the drug was encapsulated in liposomes (NX211; Gilead Sciences). In order to allow accurate description of the pharmacokinetic behavior of NX211 in cancer patients, we have developed sensitive RP-HPLC assays with fluorescence detection (lambdaex=378 nm; lambdaem=420 nm) for the determination of total LRT levels in human plasma and urine. Sample pretreatment involved deproteinization with 10% (w/v) aqueous perchloric acid-acetonitrile (2:1, v/v), and chromatographic separations were achieved on an Inertsil-ODS 80A analytical column. The lower limit of quantitation (LLQ) was established at 1.00 ng/ml in plasma (200-microl sample) and at 100 ng/ml in urine (200 microl of 40-fold diluted sample). The within-run and between-run precisions were <7.5%. LRT concentrations in urine of <100 ng/ml were determined by a modified procedure comprising a single solvent extraction with n-butanol-diethyl ether (3:4, v/v). In this assay, the fluorescence signal of LRT was increased 14-fold prior to detection by post-column exposure to UV light (254 nm) in a photochemical reaction unit. The LLQ of this assay was 0.500 ng/ml (150-microl sample) and the within-run and between-run precisions were <10%.

Acetonitriles↗
PubMed2003

Direct HPLC analysis of quercetin and trans-resveratrol in red wine, grape, and winemaking byproducts.

A simple and fast reversed-phase HPLC method using diode array detection was developed and validated for the simultaneous determination of trans-resveratrol and quercetin in Sicilian red wine from the Nero d'Avola red grape variety. Investigation was also extended to the quantitative determination of resveratrol and quercetin in grape skins and winemaking byproducts obtained from the same cultivar. Samples were eluted using a C18 narrow-bore column under isocratic conditions in less than 20 min. Quantification of trans-resveratrol and quercetin in red wine was performed without any sample pretreatment, whereas the determination of these phenolic compounds in grape skins and wine pomage required a solvent extraction procedure. Linearity was demonstrated over the 0.39-12.5 and 0.45-57.6 microg/mL range for trans-resveratrol and quercetin, respectively. Detection limits in real samples were in the low ppm level (0.07 mg/L for trans-resveratrol and 0.12 mg/L for quercetin). The HPLC-UV/DAD method was applied for the routine analyses of red wine and grape skin and winemaking byproduct extracts to evaluate their trans-resveratrol and quercetin content. In particular, a very high content of quercetin was found in wine pomace, suggesting the use of this wine byproduct as a potential source of this health-promoting phenolic compound.

Chromatography, High Pressure Liquid↗
PubMedDate not supplied

Determination of thallium in urine with Zeeman effect graphite furnace atomic absorption.

Thallium is determined in urine with a simple dilution as the only sample pretreatment. Zeeman effect background correction provides adequate accommodation for non-atomic absorption such that sufficient diluted urine can be introduced into the furnace to achieve a detection limit of 0.5 ng/mL. Precision and accuracy were evaluated with Environmental Protection Agency water samples and in vitro spiked urine pools; precision of 15% at the 6 ng/mL level was observed. Diluted urine was used in calibration, with only 4 to 5% difference in slope observed within run among randomly selected urine specimens.

Humans↗
PubMed2005

Head space sensor array for the detection of aflatoxin M1 in raw ewe's milk.

A novel screening method was developed for simple and rapid detection of aflatoxin M1 contamination in raw ewe's milk samples without the need for sample pretreatment. The method was based on the use of a commercial head space sensor array system constituted by 12 metal oxide semiconductor sensors, 10 metal oxide semiconductor field-effect transistor sensors, and a pattern recognition software. Twenty-four raw milk samples collected from two different groups of ewes fed with a formulated feed that contained increasing amounts of aflatoxin B1 and six noncontaminated ewe's milk samples were analyzed. The results obtained by using the head space sensor array, processed by statistical methods, made it possible to group the samples according to the presence or the absence of aflatoxin M1. Sample classification was in complete agreement with the aflatoxin M1 content measured by an enzyme-linked immunosorbent assay procedure. This is the first report, to our knowledge, of detection of aflatoxin M1 in ewe's milk by a multisensor array.

Aflatoxin M1↗
PubMed2002

Prospective molecular profiling of melanoma metastases suggests classifiers of immune responsiveness.

We amplified RNAs from 63 fine needle aspiration (FNA) samples from 37 s.c. melanoma metastases from 25 patients undergoing immunotherapy for hybridization to a 6108-gene human cDNA chip. By prospectively following the history of the lesions, we could correlate transcript patterns with clinical outcome. Cluster analysis revealed a tight relationship among autologous synchronously sampled tumors compared with unrelated lesions (average Pearson's r = 0.83 and 0.7, respectively, P < 0.0003). As reported previously, two subgroups of metastatic melanoma lesions were identified that, however, had no predictive correlation with clinical outcome. Ranking of gene expression data from pretreatment samples identified approximately 30 genes predictive of clinical response (P < 0.001). Analysis of their annotations denoted that approximately half of them were related to T-cell regulation, suggesting that immune responsiveness might be predetermined by a tumor microenvironment conducive to immune recognition.

Adult↗
PubMed2004

Combining headspace gas chromatography with mass spectrometry detection for confirmation of hydrocarbon residues in virgin olive oil following automatic screening.

Hydrocarbon residues can be present in virgin olive oils either naturally or as contaminants. Presence of benzene, toluene, ethylbenzene, xylene isomers and styrene (BTEXS) in virgin olive oil, demanded the establishment of a cut-off level to discriminate oil samples containing these residues at normal levels from those at high levels caused by contamination. By introducing volatile components present in the headspace (HS) of the oil samples (without prior chromatographic separation) into the ionization source of a mass spectrometer, samples were classified as containing normal or high levels of BTEXS (recommendable or non-recommendable forhuman consumption). Confirmation and quantification of contaminated virgin olive oils were achieved by combining HS sampling with gas chromatography-mass spectrometry (GC-MS). No sample pretreatment was necessary for the chromatographic method, but the addition of 600 microl of ethyl acetate as chemical modifier for 10 ml of virgin olive oil. Detection limits ranged between 3 and 9 ng/ml. Oil analysis showed the presence of toluene in all samples, as well as the absence of benzene, ethylbenzene and o-xylene.

Automation↗
PubMed1983

Diagnosis of pneumococcal pneumonia: a comparison between microscopic examination of expectorate, antigen detection and cultural procedures.

Attempts to demonstrate Streptococcus pneumoniae, or its soluble type-specific polysaccharide antigen were made on specimens from 205 patients with acute community-acquired pneumonia by (i) blood, nasopharynx and sputum culture, (ii) counterimmunoelectrophoresis (CIE) of serum, urine and sputum specimens utilizing omni-, pool- and type-specific rabbit antisera, and (iii) microscopy of gram-stained sputum smears. Pneumococci could be cultured and/or pneumococcal antigen detected in specimens from 93 (45%) of the patients with the following frequencies in samples obtained before (and after) start of antimicrobial treatment: culture from blood 25% (6%), nasopharynx 59% (18%) and sputum 80% (13%), CIE on serum 3% (9%), urine 8% (18%), urine 20X concentrated 18% (24%), and sputum 56% (56%). Microscopy of sputum smears revealed pneumococci in 65% (17%) of the 93 patients. The value of cultures from blood and sputum was most evident when the samples were obtained early in the course of the disease. With nasopharynx culture and CIE on sputum the number of positive results was doubled if the sampling was repeated. For rapid diagnosis direct Gram stain and CIE on sputum were about equally effective and also strikingly complementary, alone diagnosing 42% and 48% of the patients, respectively, but together detecting 65% of them. Gram stain was most rewarding on early pretreatment samples and CIE on post-treatment samples.

Adolescent↗
PubMed1992

Separation of serum bilirubin species by micellar electrokinetic chromatography with direct sample injection.

Four major bilirubin species in serum were separated by micellar electrokinetic chromatography with 25 mM sodium dodecyl sulfate (SDS) and 20 mM sodium tetraborate-boric acid buffer at pH 8.5. Due to the solubilization of the serum proteins by the SDS micelles, serum samples were injected directly into a 50 cm x 75 microns I.D. fused-silica capillary and complete separation of the four bilirubin species was accomplished within ca. 10 min without extensive sample pretreatment. Detection was performed by absorbance at 450 nm and average limit of detection was in the 6.0 microM concentration range. The usefulness of this method was demonstrated for the separation and detection of a number of bilirubin species present in pathological human serum samples.

Animals↗
PubMed1987

Photometric detection at 405 nm in trace analysis by capillary isotachophoresis.

The possibilities of photometric detection at 405 nm were investigated for trace isotachophoretic analysis of various ionic constituents. Increased selectivity of the detection enabled, for example, the detection and determination of nitrophenols at 10(-8) M in a 25-microliter sample. 5-Nitrofurylacrylic acid, a wine stabilizer, could be detected with confidence at ca. 0.1 ppm in wine without any sample pretreatment. Approximately 250-fmol amounts of amino acids, labelled with 2,4-dinitrophenyl, were detectable with the technique employed. This is almost three decades lower in comparison to what is achievable with an high resolution universal detector. The adsorption of the analytes in the sample handling devices as well as in the separation compartment were problems in the analysis at this concentration level. The detection limit given above was achieved when these phenomena were suppressed by the addition of naphthalene-1,3,6-trisulphonate or pyrophosphate to the sample solution.

Acrylates↗
PubMedDate not supplied

Capillary electrophoresis determination of urinary muconic acid as a biological marker for benzene in cigarette smoke.

trans,trans-Muconic acid (MA), a benzene metabolite in urine, has currently been indicated as a biological marker for benzene in cigarette smoke. The available methodologies for MA present a few shortcomings, such as lack of specificity and labor-intensive sample pretreatment. In this work, a capillary electrophoresis method for separation, identification, and quantification of urinary muconic acid has been implemented. The electrolyte consisted of a 60-mM phosphate buffer solution (pH 7), containing 0.1 mM cetyltrimethylammonium bromide (CTAB) as an electroosmotic flow modifier. Urine samples from nonsmokers and smokers were filtered through a 0.22-micron membrane prior to injection in a 75 microns i.d. x 80 cm capillary. The analysis was conducted under constant voltage conditions of -30 kV and direct UV detection at 262 nm. The detection capability of the electrophoresis system was enhanced by employing a high-sensitivity optical cell, positioned at 60 cm from the injection port. The CE methodology presented an overall analysis time of less than 10 min, with 5 min spent for capillary conditioning and approximately 5 min for run completion. The method was found to be sensitive for the determination of MA down to 25 micrograms/L, with a percentage recovery of 100 +/- 8%, and suitable for discriminating urinary MA from nonsmokers and smokers.

Benzene↗
PubMed2001

Determination of the herbicide 4-chloro-2-methylphenoxyacetic acid and its main metabolite, 4-chloro-2-methylphenol in water and soil by liquid chromatography-electrospray tandem mass spectrometry.

A rapid and sensitive LC-electrospray tandem mass spectrometry method has been developed for the quantitation of 4-chloro-2-methylphenoxyacetic acid (MCPA) and 4-chloro-2-methylphenol in both water and soil samples. Soil samples were extracted in alkaline media and cleaned-up by solid-phase extraction with C18 cartridges before LC-MS analysis. The selectivity and sensitivity offered by the triple quadrupole allowed the direct injection of the water samples rendering a sample throughput of around 100 samples per day, without any sample pretreatment, rendering for MCPA a limit of detection of 40 ng/l. In order to increase the method sensitivity, mainly for metabolite, a previous solid-phase extraction step was also performed. The method was validated by means of recovery experiments using fortified water and soil samples, obtaining satisfactory recoveries for both compounds in water and for MCPA in soil. The validated procedures can be used for the specific monitoring of residues of MCPA and its main metabolite in environmental samples, as ground and surface waters and soils, providing more selectivity and sensitivity than the current UV-based methodology. Besides, sample manipulation is greatly reduced in comparison to other GC-MS based methods which require a previous derivatization.

2-Methyl-4-chlorophenoxyacetic Acid↗
PubMed1991

Analysis of barbiturates in human serum and urine by high-performance capillary electrophoresis-micellar electrokinetic capillary chromatography with on-column multi-wavelength detection.

The analysis of barbiturates in human serum (or plasma) and urine by high-performance capillary electrophoresis-electrokinetic capillary chromatography with on-column fast-scanning multi-wavelength detection is discussed. The use of a buffer of ca. pH 8 and containing sodium dodecyl sulphate provides a medium suitable for fast and high-resolution separations of barbiturates. Seven barbiturates are characterized by their retention and absorption spectra between 195 and 320 nm. Comparison of these computer-stored data with those of unknown samples is shown to allow the identification of barbiturates in samples of patients undergoing pharmacotherapy and in toxicological urine and serum specimens. Three-dimensional electropherograms provide reliable information on the requirement and suitability of sample pretreatment procedures. With urine, extraction of barbiturates prior to analysis is necessary. With human serum several barbiturates, including phenobarbital, are shown to elute in an interference-free window in front of uric acid and the proteins, allowing these substances to be determined by direct sample injection. The need for multi-wavelength detection over a relatively wide wavelength range as a means of peak confirmation in electrokinetic capillary analyses is demonstrated and limitations of this technique for compounds with similar retention behaviour and absorption spectra are discussed.

Barbiturates↗