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PubMed1999

Multielement analysis of human hair and kidney stones by instrumental neutron activation analysis with the k0-standardization method.

This paper focuses on the evaluation of the k0 method of instrumental neutron activation analysis in biological materials. The method has been applied in multielement analysis of human hair standard reference materials from IAEA, No. 085, No. 086 and from NIES (National Institute for Environmental Sciences) No. 5. Hair samples from people resident in different parts of Malaysia, in addition to a sample from Japan, were analyzed. In addition, human kidney stones from members of the Malaysian population have been analyzed for minor and trace elements. More than 25 elements have been determined. The samples were irradiated in the rotary rack (Lazy Susan) at the TRIGA Mark II reactor of the Malaysian Institute for Nuclear Technology and Research (MINT). The accuracy of the method was ascertained by analysis of other reference materials, including 1573 tomato leaves and 1572 citrus leaves. In this method the deviation of the 1/E1+ alpha epithermal neutron flux distribution from the 1/E law (P/T ratio) for true coincidence effects of the gamma-ray cascade and the HPGe detector efficiency were determined and corrected for.

Citrus↗
PubMed1991

Trace element determinations using a 15-keV synchrotron X-ray microprobe.

At the Synchrotron Radiation Source (SRS), Daresbury, U.K., a synchrotron microprobe was constructed, in order to create an instrument capable of analyzing at the ppm or in favorite cases sub-ppm level with a lateral resolution of 10 x 15 microns2. In order to span a wide range of elements to be analyzed, a beam energy of 15 keV was chosen. Focusing and monochromation of the white beam was done in one single step with a high-precision ellipsoidally concave curved Si(111) crystal. Sufficient flux of X-rays in a narrow energy band is available in the spot to measure trace elements at the femtogram level. Measurements on standard materials, reference standard materials, and biological samples showed the lower relative minimum detection limits and higher sensitivity for the higher Z-elements obtainable with micro-SXRF (synchrotron X-ray fluorescence) as compared with microtechniques using ion accelerators. Moreover, the much lower energy deposited in the specimen represents a major argument to prefer X-rays to ions for the analysis of radiation-sensitive samples.

Animals↗
PubMed1993

Determination of methylmercury in fish samples using GC/AA and sodium tetraethylborate derivatization.

A simple technique is described for the rapid determination of methylmercury in fish tissue. Following simple dissolution in methanolic KOH solution, aqueous phase ethylation by derivatization with NaB(C2H5)4, cryogenic trapping on a packed chromatographic column, and GC separation, volatile mercury species are detected by atomic absorption spectrometry. Absolute detection limits are 4 pg of Hg for CH3Hg+ and 75 pg of Hg for labile Hg2+. Concentration detection limits for this optimized procedure are 4 ng of Hg for CH3Hg+ and 75 ng of Hg for labile Hg2+ per gram of pulverized dried fish tissue. Analysis of standard reference materials demonstrates the accuracy, precision, and reproducibility of the analytical method.

Animals↗
PubMed2001

Analysis of cocaine, benzoylecgonine, codeine, and morphine in hair by supercritical fluid extraction with carbon dioxide modified with methanol.

Supercritical fluid extraction (SFE) using CO2 modified with methanol (10%) was employed for the extraction of cocaine from human hair. Extraction conditions were developed by using designed experiments to characterize the effects of pressure, temperature, and percent methanol on the recovery of cocaine from hair. When compared to the conventional acid hydrolysis method for hair analysis, SFE was faster and gave higher recoveries. Amounts of cocaine, benzoylecgonine (cocaine metabolite), codeine, and morphine in a hair standard reference material were determined by SFE-gas chromatography/ mass spectrometry (GC/MS) and found to be in agreement with reported levels. Analyses of hair from forensic case studies are also reported.

Carbon Dioxide↗
PubMed1995

"Standardless" quantitative electron probe microanalysis with energy-dispersive X-ray spectrometry: is it worth the risk?

"Standardless" procedures for quantitative electron probe X-ray microanalysis attempt to eliminate the need for standardization through calculation of standard (pure element) intensities. Either "first principles" calculations, which account for all aspects of X-ray generation, propagation, and detection, or "fitted standards" calculations, which use mathematical fits to measured intensities from a limited set of pure standards, can form the basis for standardless analysis. The first principles standardless analysis procedure embedded in the National Institutes of Health/National Institute of Standards and Technology comprehensive X-ray calculation engine and database, Desktop Spectrum Analyzer, has been tested against spectra measured on NIST standard reference materials, research materials, and binary compounds. The resulting distribution of errors is broad, ranging from -90% to +150% relative. First principles standardless analysis can thus lead to unacceptably large errors.

Electron Probe Microanalysis↗
PubMed1998

Determination of total iodine in nutritional and biological samples by ICP-MS following their combustion within an oxygen stream.

A mineralization and determination method for total iodine in nutritional and biological samples is described. Combustion of the sample in an oxygen stream is followed by collection of the combustion products in a 5% water-soluble tertiary amine solution. Iodine is determined by inductively coupled plasma mass spectrometry. The accuracy and precision of the quantitative iodine analysis using standard addition is better than +/- 10%. A semi-quantitative analysis of four standard reference materials is evaluated. Owing to the presence of low-level iodine contaminant in the blank solution, the determination limit of the method is +/- 10 micrograms kg-1. Good agreement with certified iodine values is obtained for six reference materials. The use of the tertiary amine matrix solution permits the simultaneous determination of iodine and other trace metals of biological and toxicological importance, including Mn, Co, Ni, Cu, Zn, Rb, Cd, and Pb.

Amines↗
PubMed2003

High-resolution comparative genomic hybridisation yields a high detection rate of chromosomal aberrations in childhood acute lymphoblastic leukaemia.

BACKGROUND: Cytogenetic aberrations are of prognostic significance in childhood acute lymphoblastic leukaemias and a high detection rate could improve the biological understanding and classification of these diseases. METHODS: Bone-marrow samples from 92 children with acute lymphoblastic leukaemia were studied by high-resolution comparative genomic hybridisation (HRCGH) using dynamic standard reference intervals that enhance both specificity and sensitivity in the detection of aberrations. RESULTS: In 80 patients (87%) HRCGH revealed a total of 405 aberrations, mostly whole chromosome gains (n = 265) and partial losses (n = 80). The 25 leukaemias with a gain of more than five whole chromosomes by HRCGH harboured only 7% of all losses. With G-band karyotyping 59 patients (64%) had aberrations. HRCGH revealed more aberrations per patient than did G-band karyotyping (median: 3 vs. 1, P = 0.005), revealed aberrations in 27 of the 34 patients for whom the G-band karyotyping failed or was found to be normal, and specifically revealed more 9p losses (21% vs. 5%, P < 0.005), 12p losses (12% vs. 2%, P < 0.05) and 17q gains (11% vs. 1%, P < 0.01). Compared to the present study, the frequency of patients with aberrant karyotypes was significantly lower in previous conventional CGH studies (64% vs. 87%, P < 0.0001), as was the rate of partial aberrations per patient (1.1% vs. 1.7, P < 0.001), particularly with fewer 6q losses, 9p losses and 17q gains detected. CONCLUSION: HRCGH is superior to conventional CGH as an adjunct to G-band karyotyping as it detects recurrent aberrations at a significantly higher rate than both these techniques.

Adolescent↗
PubMed2002

A prospective comparison of the diagnostic accuracy of ERCP, MRCP, CT, and EUS in biliary strictures.

BACKGROUND: The differential diagnosis of biliary strictures remains a challenge. This study evaluated magnetic resonance cholangiopancreatography (MRCP) as a new procedure in comparison with the established methods of diagnosis including ERCP or percutaneous transhepatic cholangiography (PTC), CT, and EUS. METHODS: Fifty patients (21 men, 29 women, mean age 65.7 years) with jaundice but no pain suspected to have biliary strictures were enrolled in this prospective study. MRCP, ERCP/PTC, CT, and EUS were performed prospectively; images and videotapes (EUS) of these tests were reviewed blindly under standardized conditions. Reference standards for comparison were surgery, a biopsy confirming malignancy, or the clinical course during follow-up (at least 12 months) in cases without histopathologic proof of malignancy. RESULTS: Seven patients ultimately proved to have jaundice caused by parenchymal liver disease and 43 had a biliary stricture (17 benign, 26 malignant). Forty patients underwent all 4 imaging tests. There were 10 patients in whom patient-specific problems precluded some procedures but who were included in an intention-to-diagnose analysis. The sensitivity and specificity for diagnosis of malignancy in the 50 patients were as follows: 85% / 75% for ERCP/PTC, 85% / 71% for MRCP, 77% / 63% for CT, and 79% / 62% for EUS, with similar values in the 40 patients who underwent all 4 imaging methods. The combination of MRCP and EUS improved specificity. CONCLUSIONS: Although MRCP provides the same imaging information as direct cholangiography, it has limited specificity for the diagnosis of malignant strictures. In the differential diagnosis of biliary strictures, several tests including ERCP-guided tissue diagnosis are still required, and MRCP has only a limited clinical role.

Adult↗
PubMed2002

Urinary excretion of dithiocarbamates and self-reported Cruciferous vegetable intake: application of the 'method of triads' to a food-specific biomarker.

OBJECTIVE: Greater intake of Cruciferous vegetables (e.g. broccoli) may prevent cancer at several sites. Urinary excretion of isothiocyanate conjugates (dithiocarbamates, DTC) provides a specific biomarker of Cruciferous vegetable consumption suitable for epidemiological investigations. However, no gold-standard referent is available for evaluating urinary DTC levels as an estimator of Cruciferous vegetable consumption. We compared urinary DTC levels to intake as measured by two self-reported dietary assessment techniques. DESIGN: Cruciferous vegetable consumption was measured before and after a behavioural dietary intervention using multiple 24-hour recalls (24HR), a food-counting questionnaire (VFQ) and urinary DTC excretion levels. Analysis included a structural equation approach (Method of Triads) combining these three assessment techniques to estimate the relationship between DTC level and the study population's 'true' Cruciferous vegetable intake. SETTING: The intervention curriculum assisted participants in consuming about 2 servings per day for a 6-week period. Participants attended four classes emphasising problem-solving skills, dietary counselling and vegetable preparation skills. There were no dietary restrictions. SUBJECTS: Thirty-three healthy, free-living, post-menopausal women. RESULTS: Although few participants reported Cruciferae consumption prior to the intervention, 30 participants reported Cruciferae consumption after the intervention (Post-intervention). Urinary DTC levels were correlated with estimated intake derived from either the 24HR (r = 0.57; 95% confidence interval (95% CI) 0.28, 0.76) or VFQ (r =0.49; 95% CI 0.17, 0.71). The validity coefficient (Method of Triads) between urinary DTC excretion and an index of true Cruciferous intake was stronger than the Pearson correlation (r(v) = 0.65; 95% CI 0.35, 0.90), and comparable to estimates derived from the 24HR (r(v) = 0.82; 95% CI 0.65, 1.00) or VFQ (r(v) = 0.76; 95% CI 0.47, 0.92) method. These associations were not affected by adjustment for body mass index, energy intake, or social approval or desirability response sets. CONCLUSIONS: Food-frequency questionnaires (FFQ) suitable for large epidemiological studies may not be designed to measure all Cruciferae, and cannot capture exposure to phytochemicals derived from those vegetables. Urinary DTC measurement was significantly correlated with Cruciferae intake derived from two dietary assessment approaches, and urinary DTC levels could supplement traditional FFQ data by providing an index of recent Cruciferous vegetable intake not susceptible to reporting biases.

Aged↗
PubMed2002

Analysis of cigarette mainstream smoke for 1,1-dimethylhydrazine and vinyl acetate by gas chromatography-mass spectrometry.

1,1-Dimethylhydrazine, also known as unsymdimethylhydrazine (UDMH) and vinyl acetate (VA), are both classified by the International Agency for Research on Cancer as 2B carcinogens (possibly carcinogenic to humans) and listed as cigarette smoke constituents; however, there is little or no quantitative data available on them. For UDMH in cigarette smoke, neither a yield nor a method has been published. For VA, the most recent information on yields dates back to 1965. To bridge this gap, we have developed new gas chromatographic-mass spectrometric methods for both compounds to determine their yields in cigarette smoke. UDMH is determined by derivatization with 2-nitrobenzaldehyde in methanol and is not found in cigarette smoke at levels above the detection limit of 19 ng/cig. In further experiments, when UDMH is added to the smoke stream or air stream of lit or unlit cigarettes, the derivative 2-nitrobenzaldehyde-2,2-dimethylhydrazone is found only in the air stream of the unlit cigarettes. From this, we conclude that UDMH is either not formed during smoking at all or, if it is, it reacts immediately and quantitatively with other smoke constituents (e.g., aldehydes) and is therefore not detectable in cigarette smoke. VA is determined by trapping in acetone at -78 degrees C and is found at a concentration of 270 ng/cig for a standard reference cigarette with a cellulose acetate filter (the reference cigarette 1 R4F). In the literature, VA is reported at concentrations of 1.6 microg/cig for a cigarette with a cellulose acetate/charcoal filter and 4 microg/cig for a cigarette with a cellulose acetate filter and for an unfiltered cigarette.

Calibration↗
PubMedDate not supplied

Antimicrobial susceptibility testing of anaerobic bacteria: review and update on the role of the National Committee for Clinical Laboratory Standards.

The National Committee for Clinical Laboratory Standards (NCCLS) has published a standard method (M11-A) and alternative methods (M17-P) for susceptibility testing of anaerobic bacteria. (These will be combined in the next edition of M11.) Even though M11-A describes the "standard reference" method, there is not agreement as to which method, if any, is the "best" method. In recent years NCCLS subcommittee members have realized that results obtained by microdilution or disk elution may vary markedly from those obtained with the reference agar dilution method. Furthermore, they have recognized the difficulty of relating in vitro susceptibility results to clinical success or failure. In response to these problems, the NCCLS convened a working group to consider recommendations about susceptibility testing. This group has concluded that for most individual patients a susceptibility test may not be required but that present methods can be useful for comparisons of the activity of various drugs and for surveillance of resistance patterns.

Bacteria, Anaerobic↗
PubMedDate not supplied

Determination of arsenic in fish by hydride generation atomic absorption spectrometry.

A method utilizing microwave dissolution in a closed Teflon bomb followed by hydride generation atomic absorption spectrometry has been used for the routine analysis of arsenic in fish species from the coast of the province of Granada, Spain. The technique was evaluated for decomposing biological standard reference material (BCR mussel tissue) for arsenic analyses. The precision of the results ranged from 2.78 to 6.99%. The recovery percentages ranged from 96.33 to 100.00%. The values determined in the samples indicated slight contamination by this element in the zone. The concentrations of arsenic in fish ranged from 0.396 to 45.716 micrograms/g.

Animals↗
PubMed1987

Determining picogram quantities of U in human urine by thermal ionization mass spectrometry.

The U concentration in Standard Reference Material 2670 (Toxic Metals in Freeze-Dried Urine) and the urine of two preschool-age children were determined by measuring the chemically separated U by isotope dilution thermal ionization mass spectrometry using ion counting detection. This procedure can detect about 1% of the U atoms loaded into the mass spectrometer and has a total chemical blank of about 5 pg U. The U concentration in SRM 2670 was found to be 113 +/- 2 pg 238U/ml (1 s). At this concentration, a 1-ml sample is sufficient for a determination with a total uncertainty of less than 5%. The U concentrations in the two children were 3.1 +/- 0.9 and 3.6 +/- 0.9 pg 238U/g. These values suggest that the U concentration in urine of unexposed persons may be at this low level or lower.

Child, Preschool↗
PubMed2006

New formulae for predicting tracheal tube length.

BACKGROUND: The aim of this study was to determine the accuracy of standard techniques for estimating oral and nasal tracheal tube length in children and to devise more accurate predictive formulae that can be used at the bedside. METHODS: Data were collected from 255 children who required tracheal intubation whilst on the Pediatric Intensive Care Unit over a period of 1 year. Age, weight, the final length of the tracheal tube and the internal diameter were documented. Patients with a tracheostomy were excluded from the study. RESULTS: Using linear regression the following formulae best predicted final tracheal tube length. For children over 1 year of age: Insertion depth (cm) for orotracheal intubation = age/2 + 13 Insertion depth (cm) for nasotracheal intubation = age/2 + 15 For children below 1 year of age: Insertion depth of orotracheal tube (cm) = weight/2 + 8 Insertion depth of nasotracheal tube (cm) = weight/2 + 9 CONCLUSIONS: Current Advanced Paediatric Life Support guidelines underestimate the appropriate tracheal tube lengths for orotracheal intubation in children over 1 year of age. Similarly, the novel weight-based formulae for tracheal tube lengths in children below the age of 1 year proved more accurate than standard reference charts. We therefore recommend that these new formulae are prospectively evaluated.

Adolescent↗
PubMed1964

STUDIES ON BACTERIAL PYROGENICITY. 3. SPECIFICITY OF THE UNITED STATES PHARMACOPEIA RABBIT PYROGEN TEST.

The specificity of the first or "presumptive" portion of the USP rabbit pyrogen test was investigated by use of a new absolute standard of reference. The reference standard was a 0.9% sodium chloride solution prepared to be pyrogen-free. Details of the preparation were described. The hypothesis was explored that the temperature response of rabbits after intravenous injection of the standard solution was independent of exogenous pyrogen. Reactions observed among the rabbits in our colony allowed a classification of these animals ranging from "consistently reliable" to "consistently unreliable." Details of the experimental results and implications for pyrogen testing are discussed. The recommendation was made that all rabbit test animals be "screened" in sham and actual tests before being used for pyrogen testing.

Animals↗
PubMed1991

Serum antibody in Actinobacillus actinomycetemcomitans-infected patients with periodontal disease.

This study was designed to (i) delineate the characteristics of serum antibody responses to Actinobacillus actinomycetemcomitans in patients with periodontitis who are infected with A. actinomycetemcomitans; irrespective of disease classification; (ii) assess the relationship of the elevated antibody levels to colonization of the oral cavity by A. actinomycetemcomitans; and (iii) describe the serotype distribution of A. actinomycetemcomitans and antibodies to the microorganism in infected patients with various clinical classifications. To compare the levels of various isotype-specific antibodies to the different antigens, studies were performed that allowed quantitation of each isotype-specific antibody in a human reference standard. By using this reference standard, it was shown that the levels of immunoglobulin G (IgG), IgM, and IgA responses to A. actinomycetemcomitans were similar among the infected patients, irrespective of disease classification. Also, we demonstrated that the serum antibody response to serotype b was quantitatively greater in all isotypes. Our findings indicate that b was the most frequent A. actinomycetemcomitans serotype detected in the patients and appears to be capable of initiating a substantial serum IgG antibody response that may contain cross-reactive antibodies to other serotypes of A. actinomycetemcomitans. Generally, in cases in which the response to a single serotype was elevated, only that type of A. actinomycetemcomitans was detected in the plaque. Individuals exhibiting elevated antibodies to multiple serotypes were most consistently colonized by the serotype b microorganism. This study represents the first report detailing the distribution of IgG subclass antibodies to A. actinomycetemcomitans in periodontal disease. The results demonstrated that the primary responses of patients with periodontitis to A. actinomycetemcomitans were of the IgG1 and IgG3 subclasses, which is consistent with elicited responses to protein antigens. In contrast, the primary subclass response in normal subjects was limited to the IgG2 subclass and may represent broader cross-reactivity to polysaccharide antigens-lipopolysaccharide from the bacteria.

Actinobacillus↗
PubMed1981

Facilitating quality control of the antimicrobial susceptibility test.

Standard reference strains of Staphylococcus aureus, Escherichia coli, and Pseudomonas aeruginosa were suspended in sterile deionized water and tested daily via disk agar diffusion for their antimicrobial susceptibilities. Inocula of E. coli and P. aeruginosa yielded acceptable results for up to 32 days; however, results on S. aureus were unacceptable due to loss of viability of the organism in water. E. coli and P. aeruginosa inocula, in water, can be used daily for quality control of the disk gear diffusion test.

Anti-Bacterial Agents↗
PubMed1996

Evaluation of Alamar colorimetric broth microdilution susceptibility testing method for staphylococci and enterococci.

We compared the results of the Alamar broth microdilution susceptibility testing method with the results of the National Committee for Clinical Laboratory Standards reference broth microdilution method for 119 gram-positive organisms. The strains were tested for their susceptibilities to 20 antimicrobial agents. Only appropriate antimicrobial agents were evaluated for each species of bacteria. Absolute categorical agreement between the reference method and the test method was 91.5% for enterococci, 99.8% for oxacillin-susceptible staphylococci, and 97.4% for oxacillin-resistant staphylococci. Essential agreement (percent complete agreement plus percent minor errors) was > 99% for all organisms tested. The results for enterococci showed no very major errors, one major error with ofloxacin, and numerous minor errors with the quinolones. However, all except one of the minor errors were within +/- 1 log2 dilution of the reference result. For staphylococci, only 2 very major errors (one each with chloramphenicol and oxacillin), 1 major error (chloramphenicol), and 15 minor errors (multiple drugs) were observed. The Alamar colorimetric system was easy to use and the results were easy to read. It appears to be an acceptable method for antimicrobial susceptibility testing of staphylococci and enterococci.

Colorimetry↗