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PubMed1999

Capillary zone electrophoresis separations of enantiomers present in complex ionic matrices with on-line isotachophoretic sample pretreatment.

Analytical capabilities of capillary zone electrophoresis (CZE) with on-line coupled capillary isotachophoresis (ITP) sample pretreatment in the column-coupling capillary electrophoresis equipment to separate and determine enantiomers present in multicomponent ionic matrices were studied. Tryptophan was used as a model analyte in the ITP-capillary zone electrophoresis experiments performed in this context while a 90-component model mixture of UV-light absorbing organic anions and urine served as multicomponent sample matrices. Various working modes in which the on-line coupled capillary isotachophoresis-capillary zone electrophoresis combination in the column-coupling separation system can operate were employed in the anionic regime of the separation with direct injections of the samples. Advantages and limitations of these working modes in the separations of enantiomers present in model and urine matrices were assessed. Experiments with model mixtures of tryptophan enantiomers revealed that the two were resolved in the capillary zone electrophoresis stage with the aid of alpha-cyclodextrin also when their concentration ratio in the sample was 1:200 while the concentration of L(-)-tryptophan was 25 nmol/l. The limits of detection for the enantiomers were at approximately 10 nmol/l (approximately 1.5 ng/ml) concentrations for a 220 nm detection wavelength of the UV detector employed in the capillary zone electrophoresis stage and for a 30 microliters sample load. A high sample load capacity of the on-line coupled capillary isotachophoresis stage was effective in separating the samples corresponding to 3-6 microliters volumes of undiluted urine. The results from the runs with urine samples showed that only the capillary isotachophoresis-capillary zone electrophoresis combination with a post-column on-line coupled capillary isotachophoresis sample clean-up (responsible for a removal of more than 99% of the sample anionic constituents migrating in the on-line coupled capillary isotachophoresis stack and detectable in the capillary zone electrophoresis stage) provided a universal alternative for the detection and quantitation of the model analyte (L(-)-tryptophan).

Anions↗
PubMed1999

Rapid determination of glyphosate in cereal samples by means of pre-column derivatisation with 9-fluorenylmethyl chloroformate and coupled-column liquid chromatography with fluorescence detection.

A rapid procedure for the determination of glyphosate in cereals has been developed. Convenient sample pretreatment is carried out by (i) a overnight standing extraction of 1.0 g homogenized sample with 20 ml of water, (ii) centrifugation of the samples, (iii) a passing of 2.5 ml of the clear layer through a 100 mg C18 solid-phase extraction cartridge and (iv) collection of the last 1.5 ml of the eluent into a calibrated tube. For the instrumental analysis, the efficient approach developed earlier for environmental water samples [J.V. Sancho, F. Hernández, F.J. LUpez, E.A. Hogendoorn, E. Dijkman, P. van Zoonen, J. Chromatogr. A, 737 (1996) 75] was successfully adopted for the determination of glyphosate in the obtained cereal extracts. The procedure includes a 15 min derivatisation step of the analyte with 9-fluorenylmethyl chloroformate and a 16 times dilution step prior to instrumental analysis employing coupled-column LC with fluorescence detection. The developed procedure has a sample throughput of more than 25 samples per day and a limit of quantification of 0.5 mg/kg. The method was validated by analyzing freshly spiked cereal samples and samples with aged residues at levels between 1.0 and 10 mg/kg. The overall recovery of the freshly spiked samples was 86% (n = 10) with a repeatability of 6.5% and a reproducibility of 9.5%. For samples with aged residues recoveries performed at different time intervals (range 80-150 days) did not differ significantly; the overall recovery (n = 10) was 74% with a repeatability and reproducibility of 14 and 20%, respectively.

Chromatography, High Pressure Liquid↗
PubMed2001

Ex vivo induction of cytokine mRNA expression in human blood samples.

The interest in the quantitative analysis of cytokine mRNA profiles has increased substantially in recent years. This is based on the potential use of basal cytokine mRNA expression as sensitive markers for in vivo lymphocyte activation in a variety of clinical settings. However, it is less well known to what extent differences in blood collection and preparation techniques may cause ex vivo alteration of quantitative cytokine mRNA levels. We therefore evaluated the effect of blood sampling and the impact of cell separation on interleukin (IL)-2, IL-4, interferon (IFN)-gamma and tumour necrosis factor (TNF)-alpha mRNA expression in an intraindividual study design (n=8). Two different blood sampling procedures were applied. A whole blood sample 1 was collected by constant moderate blood flow into a blood collection tube containing lithium-heparin. Moreover, a second sample from the same donor was collected by a 5-fold acceleration of blood flow. Furthermore, peripheral blood mononuclear cell (PBMC) were isolated from the first whole blood sample by density separation over Ficoll-Hypaque. The quantification of cytokine mRNA expression was performed by real-time PCR in native whole blood/PBMC samples or unstimulated cultures. We found a significant increase of IL-2, IL-4 and TNF-alpha mRNA expression (P=0.018, P=0.028, P=0.018) in whole blood samples collected by rapid sampling. The isolation of PBMC by density gradient separation prompted on upregulation of the mRNA levels of IL-2, IL-4 and TNF-alpha 5-9-fold (P=0.018, P=0.018, P=0.018). In contrast, IFN-gamma mRNA expression was not significantly influenced by differences in blood sample preparation. Our data clearly demonstrate that differences in the blood sampling technique or cell separation should be considered as important factors for non-physiological ex vivo induction of cytokine mRNA expression. The current data emphasize the need for data on the impact of ex vivo variation in order to extract reliable and consistent information, particularly when cytokine mRNA expression data from healthy blood donors are included in clinical studies.

Blood Cells↗
PubMedDate not supplied

Total and specific anti-Trypanosoma cruzi immunoglobulin E in pericardial fluid samples from patients with chronic Chagas disease.

Levels of total and specific anti-Trypanosoma cruzi immunoglobulin E (IgE) were determined by immunoenzymatic assay among 101 samples of pericardial fluid from patients who had died in one trypanosomiasis endemic area in central Brazil. These samples were divided into 6 groups. Group I, 17 samples from patients with the cardiac form of Chagas disease; group II, 11 samples from patients with the digestive form of Chagas disease, presenting megaoesophagus and/or megacolon; group III, 41 samples from patients with the indeterminate form of Chagas disease; group IV, 4 samples from patients with both cardiac and digestive forms of Chagas disease; group V, 5 samples from patients who suddenly died and were seropositive for T. cruzi antibodies; group VI, 23 samples, used as a control group, which came from patients seronegative for T. cruzi antibodies. Significantly high levels of total IgE were observed in groups I, II, III, IV and V when compared with group VI (mean concentrations 708-1157 iu/mL compared with 394 iu/mL). In groups I-V, 32 samples (41%) had specific anti-T. cruzi IgE antibodies. The individual percentage positivity rates in these groups were 64.7% (group I), 45.4% (group II), 34.1% (group III), nil (group IV), and 40.0% (group V). A significant correlation between total IgE and specific anti-T. cruzi IgE was observed only in the samples from patients with the cardiac form of Chagas disease (group I).

Animals↗
PubMed2002

Beamforming with a reduced sampling rate.

The beamforming process requires a high delay resolution to avoid the deteriorating effects of the delay quantization lobes on the image dynamic range and signal to noise ratio. Wideband transducers require delay resolutions in the order of 1/16 the signal period. If oversampling is used to achieve this timing resolution, a huge data volume has to be acquired and processed in real time. This is usually avoided by sampling just above the Nyquist rate and interpolating to achieve the required delay resolution. However this increases the hardware complexity. Baseband sampling has been alternatively proposed with sampling rates as low as the transducer frequency or even lower. This approach uses two A/D converters and processing chains for every channel, thus doubling the hardware requirements. Quadrature sampling can be used instead with a single A/D converter, but the sampling rate must be a multiple of four times the transducer frequency, decreasing the application flexibility. Furthermore, it produces relatively high errors in the detected envelope if wideband transducers are used. This work presents a new approach, the selective sampling technique (SST), which keeps the lowest sampling rate required by the imaging process or the signal bandwidth (whatever is larger) and, at the same time, provides a high delay resolution to keep the highest image dynamic range. The SST is based on a second order sampling process which, differently from the mentioned approaches, does not pose any constraints in the time interval between samples and produce lower errors in the detected envelope. The hardware requirements are low (a single A/D converter and processing chain for every transducer element), working at the lowest data rate compatible with the Nyquist criterion, thus reducing the data bandwidth. Furthermore, the sampling points can be also freely chosen, so that the SST simplify the usually required scan conversion process to a simple linear interpolation easily carried out by software in real-time.

Journal Article↗
PubMed2002

Assessment of efficient sampling designs for urban stormwater monitoring.

Monitoring programs for urban runoff have not been assessed for effectiveness or efficiency in estimating mass emissions. In order to determine appropriate designs for stormwater, total suspended solids (TSS) and flow information from the Santa Ana River was collected nearly every 15 min for every storm of the 1998 water year. All samples were used to calculate the "true load" and then three within-storm sampling designs (flow-interval, time-interval, and simple random) and five among-storm sampling designs (stratified by size, stratified by season, simple random, simple random of medium and large storms, and the first m storms of the season) were simulated. Using these designs, we evaluated three estimators for storm mass emissions (mean, volume-weighted, and ratio) and three estimators for annual mass emissions (median, ratio, and regular). Designs and estimators were evaluated with respect to accuracy and precision. The optimal strategy was used to determine the appropriate number of storms to sample annually based upon confidence interval width for estimates of annual mass emissions and concentration. The amount of detectable trend in mass emissions and concentration was determined for sample sizes 3 and 7. Single storms were most efficiently characterized (small bias and standard error) by taking 12 samples following a flow-interval schedule and using a volume-weighted estimator of mass emissions. The ratio estimator, when coupled with the simple random sample of medium and large storms within a season, most accurately estimated concentration and mass emissions; and had low bias over all of the designs. Sampling seven storms is the most efficient method for attaining small confidence interval width for annual concentration. Sampling three storms per year allows a 20% trend to be detected in mass emissions or concentration over five years. These results are decreased by 10% by sampling seven storms per year.

Environmental Monitoring↗
PubMed2001

Human placenta as a 'dual' biomarker for monitoring fetal and maternal environment with special reference to potentially toxic trace elements. Part 1: physiology, function and sampling of placenta for elemental characterisation.

Choice of specimen from human subjects for monitoring pollutants proven to be detrimental to human health depends on the criteria chosen, namely real-time monitoring (RTM) or long-term monitoring (LTM). Specimens such as whole blood, urine, saliva and breast milk are commonly used from living subjects for RTM of toxic metals. However, sampling blood requires an invasive procedure. On the other hand, hair (with some limitations), bone (especially for the assessment of bone seeking elements), adipose tissue (mainly for organic pollutants) and liver (for both organic and inorganic toxicants) are used as specimens for LTM. With the exception of hair, generally these specimens are obtained at post-mortem. In context of health-related biomonitoring, placenta as a specimen has not received as much attention as it deserves. It is a unique sample requiring no invasive procedure, and offers possibilities for RTM, in particular as a dual purpose specimen for evaluating the pollutant burden exerted on the mother as well as on the fetus. Obtaining representative samples of placenta for elemental composition studies is a difficult task, because of heterogeneous mix of placental cells and decidual matter tainted with maternal and fetal blood. Therefore, the present sampling practices for placental tissue, and guidelines to safeguard the validity of the sampled material have been reviewed in part 1 with the following conclusions: medico-legal and ethical matters should be properly addressed before collecting the placenta; it is advisable to collect the entire placenta even if it includes the umbilical cord; further preparatory work is to be carried out in a clean laboratory and depends upon the purpose of the investigation; homogenising the entire sample may prove to be technically challenging but this step is crucial to obtain representative samples, handling the entire sample may be unavoidable; and an alternative method of procuring representative samples would require random samples from multiple sites, pooled, homogenised and assayed to confirm homogeneity.

Adult↗
PubMed2003

Prospective evaluation of a 21-sample needle biopsy procedure designed to improve the prostate cancer detection rate.

OBJECTIVES: To evaluate prospectively the diagnostic yield of a 21-sample ultrasound-guided needle biopsy procedure for prostate cancer in patients with elevated serum prostate-specific antigen and/or abnormal digital rectal examination findings. METHODS: Between December 2000 and May 2002, 303 patients underwent 21-sample needle biopsy under local anesthesia, comprising sextant biopsies at a 45 degrees angle, 3 biopsies in each peripheral zone at an 80 degrees angle, 3 biopsies in each transition zone (TZ), and 3 biopsies in the midline peripheral zone. Morbidity was assessed clinically. A short questionnaire was filled out by 90 consecutive patients. RESULTS: The cancer detection rate using 6 biopsy samples (sextant biopsies only), 12 samples (sextant plus lateral biopsies), 18 samples (sextant plus lateral plus TZ biopsies), and 21 samples (sextant plus lateral plus TZ, plus midline biopsies) was 22.7%, 28.3%, 30.7%, and 31.3%, respectively. The 21-sample procedure statistically improved the cancer detection rate by 37.9% relative to the 6-sample procedure. The improvement was most marked in patients with a prostate volume of more than 40 cm(3) (48.3%), patients with Stage T1c prostate disease (44.9%), patients undergoing repeat biopsy (66.2%), and patients with prostate-specific antigen levels greater than 10 ng/mL (38.5%). Adverse effects were infrequent (3%), consisting of prostatitis in 3 patients, acute urinary retention in 6 patients, and rectal bleeding requiring hospitalization in 1 patient taking aspirin. Using the questionnaire, 84% of patients reported macroscopic hematuria for an average of 3.4 days and hematospermia for 12.8 days, and 45% reported minor rectal bleeding lasting 1.1 days. The mean pain score, with a visual analog scale ranging between 0 (no pain) and 10 (intense pain), was 4.56. CONCLUSIONS: A 21-sample needle biopsy procedure increased the prostate cancer detection rate relative to a 6-sample procedure, without increasing morbidity. Patients with elevated prostate-specific antigen values should undergo sextant biopsies and at least 6 additional biopsies in the peripheral zone and 6 in the TZ.

Aged↗
PubMed1995

Prostate-specific antigen variability in men without prostate cancer: effect of sampling interval on prostate-specific antigen velocity.

OBJECTIVES: To evaluate short-term and long-term variability between prostate-specific antigen (PSA) measurements to determine the most appropriate PSA sampling interval and rate of PSA change (PSA velocity) to distinguish between men with and without prostate cancer. METHODS: Retrospective study of PSA variability and PSA velocity in three groups of men without a diagnosis of prostate cancer and PSA levels less than 10 ng/mL: 56 men with a histologic diagnosis of benign prostatic hyperplasia (BPH; histologic BPH group) and 527 men with no history of cancer (noncancer group) who were part of the Baltimore Longitudinal Study of Aging and had PSA sampled at 2-year intervals (long-term), and 223 men with a clinical diagnosis of BPH (clinical BPH group) who had PSA sampled at 3-month intervals (short-term). PSA variability (deviation between consecutive measurements) and PSA velocity based on both two consecutive measurements and three consecutive measurements (average velocity) were calculated for each study group. RESULTS: PSA velocity is the deviation in PSA measurements relative to the elapsed time between the measurements. Because the variability in PSA between measurements was similar for the groups, the major factors that influenced PSA velocity were the sampling interval between PSA measurements, and to a lesser extent, the number of repeat PSA measurements. The 99th percentile for PSA velocity was 0.7 (histologic BPH group) and 0.75 ng/mL per year for the noncancer group when three measurements with a 24-month PSA sampling interval were used. However, the 99th percentile for PSA velocity was 5.8 and 2.4 ng/mL per year when three measurements with 3-month and 6-month PSA sampling intervals were used. Using three measurements, the percentage of subjects with a PSA velocity more than 0.75 ng/mL per year was 1% for the groups with a 24-month PSA sampling interval and 28% and 17% for 3-month and 6-month PSA sampling intervals, respectively. The 99th percentile for PSA velocity and the percentage of subjects with a PSA velocity more than 0.75 ng/mL per year was higher using two measurements compared to three measurements regardless of PSA sampling interval. CONCLUSIONS: PSA velocity is inversely related to the interval between PSA measurements. A PSA velocity more than 0.75 ng/mL per year is useful in distinguishing between men with and without prostate cancer when: (1) velocity is based on three consecutive measurements; and (2) PSA is sampled long-term (2 years) but not short-term (3 to 6 months).

Aged↗
PubMed2002

In vivo monitoring of amino acids by direct sampling of brain extracellular fluid at ultralow flow rates and capillary electrophoresis.

Extracellular levels of glutamate (GLU), aspartate (ASP), glycine (GLY), phosphoethanolamine (PEA), and gamma-aminobutyric acid (GABA) were measured in the striatum of anesthetized rats using a novel sampling approach in which extracellular fluid (ECF) was removed at 1-50 nl/min using a fused silica capillary tube with 18-40 microm inner diameter and a outer diameter of 90 microm. The samples of ECF were analyzed by capillary electrophoresis with laser-induced fluorescence detection. Basal levels for GABA, GLY, and GLU measured using direct sampling at 1 nl/min were 270 +/- 40, 4950 +/- 1100, and 1760 +/- 150 nM, respectively in good agreement with the values obtained using microdialysis sampling calibrated by the low-flow rate method. ASP levels were approximately four-fold higher in directly sampled fluid than in dialysate. At higher direct sampling flow rates (10-50 nl/min), detected levels of the amino acids were lower by 70-90% indicating depletion of analyte under these conditions. PEA, an indicator of membrane disruption, was 5.5-fold higher in dialysate than in directly sampled ECF indicating greater tissue damage associated with microdialysis. In addition to the basal measurements, the direct sampling technique was applied to monitoring concentration changes of GLU and ASP in the striatum with better than 90 s temporal resolution after perfusion of either 120 mM K(+) or 400 microM L-trans-pyrrolidine-2,4-dicarboxylic acid (PDC) through a microdialysis probe immediately adjacent to the direct sampling capillary. Levels of GLU and ASP increased 615 +/- 95 and 542 +/- 96%, respectively (n=4) upon addition of 120 mM K(+) to the perfusate and 622 +/- 234 and 672 +/- 218% (n=5) for PDC. It is concluded that direct sampling at low-flow rates allows determination of extracellular levels of the amino acids with spatial resolution that is at least 500-fold better than microdialysis.

Amino Acids↗
PubMed2002

Antigen-induced production of interferon-gamma in samples of peripheral lymph nodes from sheep experimentally inoculated with Mycobacterium avium subsp. paratuberculosis.

The production of interferon-gamma (IFN-gamma) in response to Johnin purified protein derivate was measured in samples of the prescapular lymph node (PLN) from 10 sheep, aged 2 years, and nine sheep, aged 1 year that had been inoculated orally with Mycobacterium avium subsp. paratuberculosis within their first month of life. Ten non-inoculated sheep, aged 1 year, constituted the negative control group. The results obtained in the PLN IFN-gamma assay were compared with those derived from serological tests: a complement fixation test (CFT), agar gel diffusion test (AGID) and enzyme-linked immunosorbent assay (ELISA), as well as an IFN-gamma test on samples of blood. Among the 19 inoculated sheep, 16 gave positive reactions in the PLN IFN-gamma assay on samples incubated overnight, and 18 tested positive when the assay was applied to PLN samples incubated for 48h. In comparison, three, four and seven inoculated sheep gave positive reactions in the ELISA, CFT and in the blood IFN-gamma assay on samples incubated overnight, respectively. The AGID and IFN-gamma assay on blood samples incubated for 48h detected eight inoculated animals. Twelve inoculated sheep, that tested positive in the PLN IFN-gamma assay were clinically normal, gave negative results in an IS900-based polymerase chain reaction (PCR) assay on samples of ileum and ileocaecal lymph node and had no histological evidence of paratuberculosis, but tested positive on more than two occasions in sequential serological testing before necropsy. None of the 10 non-inoculated sheep tested positive in the AGID, CFT, ELISA, blood IFN-gamma assay on samples incubated overnight and for 48h or the PLN IFN-gamma assay on samples incubated overnight, but one gave a positive result in the PLN IFN-gamma assay on samples stimulated for 48h. It is likely that the positive reactions obtained by the PLN IFN-gamma assay in the 12 inoculated sheep that tested negative in the PCR assay and histopathological examination represents immunological evidence of latent infection or previous exposure to M. paratuberculosis rather than active infection.

Animals↗
PubMed1997

Gas chromatographic method using electron-capture detection for the determination of musk xylene in human blood samples. Biological monitoring of the general population.

Musk xylene (2,4,6-trinitro-1,3-dimethyl-5-tert.-butylbenzene, MX), a synthetic musk often used in different fragrances and soaps to substitute the natural musk, is a potential contaminant of humans. In this publication, a specific and sensitive detection method for the determination of musk xylene in human blood samples is described. The clean-up of the blood samples includes an extraction step followed by a solid-phase adsorption to separate MX from other plasma components. Separation and detection was carried out by capillary gas chromatography and an electron capture detector (GC-ECD). The results were verified using qualitative capillary gas chromatography and a mass selective detector with electron impact ionisation (GC-EI-MS). epsilon-Hexachlorocyclohexane (epsilon-HCH) is used as internal standard. The reliability of the GC-ECD method has been proved. The relative standard deviations of the within-series imprecision were 12.7% for samples with a concentration of 0.5 microg/l and 2.1% for samples with a concentration of 5.0 microg/l, whereas the relative standard deviations for the between-day imprecision were 14.9% (0.5 microg/l samples) and 3.4% (5.0 microg/l samples). The losses during sample treatment were between 10.1% and 17.8%. No interfering peaks were observed. The absolute detection limit was 0.1 microg/l plasma. A total of 72 human blood samples were analysed to determine the MX concentrations within the general population. In 66 of the 72 human blood samples, the MX concentrations ranged from 0.10 to 1.12 microg/l plasma for the described method. In six samples no MX was detected. The median concentration was 0.24+/-0.23 microg MX/l plasma. The 95 percentile was 0.79 microg/l. No correlation could be found between MX concentrations and smoking habit, broca index, age, sex as well as fish consumption habits. Nevertheless, the results demonstrate the exposure of the general population to MX.

Chromatography, Gas↗
PubMed2000

The personal identification of many samples recovered from under the sea.

An automatic and rapid DNA typing system was employed for personal identification, using fragmentary tissue samples from victims in an airplane accident. Two victims were crushed into small pieces, and 33 samples suspected to belong to them were recovered from under the sea. From each sample, 10 mg was used for testing. The parents' bloods of two presumptive victims were also examined. DNA extraction from samples was performed by the NaI method, and the obtained DNA samples were analyzed with the ABI PRISM system. Among 33 samples, 31 samples were identified to be human tissues, possibly from two victims. The other two samples seemed to be parts of marine animals. ABO blood group, STR polymorphism, and mitochondrial DNA polymorphism typing were possible in every examined human sample. Two victims' fragmentary tissues were identified by determining ABO genotype, STR type and mitochondrial DNA type. The system we employed enabled an accurate typing of many fragmentary samples in a short time, thus contributing to the fast and secure identification of many victims in such cases as big air accidents.

ABO Blood-Group System↗
PubMed2003

Use of control sample for estimation of prediction error in multivariate determination of lidocaine solutions with non-column chromatographic diode array UV spectroscopy.

The aim of this study was to investigate the ability of a control sample, of known content and identity, to diagnose and correct errors in the predictions when the same multivariate calibration model was used for analysis of new samples over time. A calibration set consisting of 16 samples with a known content of lidocaine was analysed and two external test sets, A and B, were used for the validation. Test set A contained 15 samples with different concentrations of lidocaine and test set B contained three samples with different lidocaine content, which were analysed six times in order to obtain a measure of repeatability. The multivariate calibration was done with PLS regression on UV spectra collected between 245 and 290 nm. A representative UV spectrum was exported from the collected DAD files by two methods, average spectrum over the whole file and average spectrum over the sample plug. Test set A was analysed further on another three occasions together with a control sample. The results showed that the control sample could be used to give a diagnosis and estimate of the prediction error. Moreover, the measured prediction error of the control sample could also be used to correct the predictions, thereby reducing the prediction error. Finally, some practical considerations regarding use of the proposed DAD method with a control sample are presented. The procedure suggested could lead to an efficient analytical approach where the same calibration model could be used over time without recalibration, which may be attractive in industrial quality control or screening analysis in pharmaceutical research.

Chromatography, High Pressure Liquid↗
PubMed1997

A sensitive method for the determination of uranium in biological samples utilizing kinetic phosphorescence analysis (KPA).

Kinetic phosphorescence analysis is a technique that provides rapid, precise and accurate determination of uranium concentration in aqueous solutions. This technique utilizes a laser source to excite an aqueous solution of uranium, and measures the emission luminescence intensity over time to determine the luminescence decay profile. The lifetime of the luminescence decay profile and the linearity of the log luminescence intensity versus time profile are indications of the specificity of the technique for uranium determination. The luminescence intensity at the onset of decay (the initial luminescence intensity), which is the luminescence intensity at time zero after termination of the laser pulse used for excitation, is proportional to the uranium concentration in the sample. Calibration standards of known uranium concentrations are used to construct the calibration curve between the initial luminescence intensity and uranium concentration. This calibration curve is used to determine the uranium concentration of unknown samples from their initial luminescence intensity. We developed the sample preparation method that allows the determination of uranium concentrations in urine, plasma, kidney, liver, bone spleen and soft tissue samples. Tissue samples are subjected to dry-ashing in a muffle furnace at 600 degrees C and wet-ashing with concentrated nitric acid and hydrogen peroxide twice to destroy the organic component in the sample that may interfere with uranium determination by KPA. Samples are then solubilized in 0.82 M nitric acid prior to analysis by KPA. The assay calibration curves are linear and cover the range of uranium concentrations between 0.05 micrograms l-1 and 1000 micrograms l-1 (0.05-1000 ppb). The developed sample preparation procedures coupled with the KPA technique provide a specific, sensitive, precise and accurate method for the determination of uranium concentration in tissue samples. This method was used to quantify uranium in different tissue samples obtained over a period of 90 days following a single intraperitoneal uranium dose of 0.1 mg kg-1 in rats.

Animals↗
PubMed2000

Comparison of the composition of some petroleum samples which may be applied for skin and mucous membrane treatment.

A particular Croatian petroleum (sample P1) and its three derivatives (samples P2, P3 and P4), potentially applied as healing preparations for skin and mucous membrane treatment, were studied in order to learn their composition and to discriminate them according to two criteria: composition of natural petroleum compounds, and lacking aromatics. Elemental (C, H, N and S) and group composition (by LC, UV/VIS, IR and 1H NMR) were determined and the single component distributions were analyzed (by GC) and identified (by GC-MS). Focussed saturated compounds (n-alkanes, pristane and phytane, drimanes/eudesmanes, steranes and hopanes) were studied in order to emphasize the preservation or destruction of genuine petroleum structures in derivatives. Samples P2 (petroleum-brownish color, petroleum like smell) and P3 (colorless, transparent, slight pine-like odor), were found, now constituting petroleum, to still be composed of the components of their native structure. Compared to sample P1, they were missing light and heavy compounds. While sample P2 contained different compound classes, sample P3 comprised exclusively saturated hydrocarbons, satisfying pharmacopoeia's requirement regarding the low aromatics content. Almost a half of sample P3 was composed of cyclic moieties, including terpenoids, possibly responsible for the odor. Samples P1, P2 and P3 were found rather rich in steranes. Sample P4 (colorless, transparent, no smell) was found denaturalized. In spite of high similarity in bulk properties to sample P3, it comprised no detectable amount of n-alkanes, pristane and phytane, or drimanes/eudesmanes, steranes and hopanes (although found rich in oligocycles).

Administration, Topical↗
PubMed2000

Addiction severity index data from general membership and treatment samples of HMO members. One case of norming the ASI.

The Addiction Severity Index (ASI) is a widely used interview among substance-dependent populations in treatment. Its value as a treatment planning and evaluation tool has been diminished by the lack of comparative data from nonclinical samples. The present study included four scales from the ASI collected on samples of adult subscribers to a large health maintenance organization (HMO) in northern California, as well as an adult clinical sample from the same geographic region with the same HMO insurance, thereby offering informative contrasts. Interviews (N = 9,398) of non-alcohol-dependent or abuse adults from a random sample of members of a large HMO were analyzed. We collected complete ASI data on the alcohol, drug, medical, and psychiatric composite scales and partial data on the employment scale. A sample of 327 adult members of the same HMO from one of the counties included in the survey, who were admitted to treatment for alcohol and/or drug addiction, was administered the same ASI items at treatment admission. Analyses compare problem severities in the two samples by age and gender. The general membership reported some problems in most of the ASI problem areas, although at levels of severity that were typically far below those seen in the clinical sample. General membership and clinical samples were somewhat similar in medical status and in employment. As expected, alcohol, drug, and psychiatric status were much more severe in the clinical sample. The data from the HMO general membership sample provide one potential comparison group against which to judge the severity of problems presented by drug- and alcohol-dependent patients at treatment admission and at posttreatment follow-up. The authors discuss the implications for treatment planning and the evaluation of treatment outcome.

Adolescent↗
PubMed1995

Patterns of fundamental frequency for three types of voice samples.

The purpose of this study was to determine the variability in speaking fundamental frequency (Fo) associated with sample type in two age groups of normal male and female speakers and a group with vocal-fold paralysis. Young and elderly normal control men and women produced a sustained vowel, read a passage, and spoke extemporaneously in the morning, early afternoon, and late afternoon on three different days. The vocal-fold-paralysis group produced two voice samples at different times on the same day. Two patterns of variability emerged in the normal groups. Young men produced sustained phonation at a significantly lower Fo than their reading or extemporaneous samples. Young and older women and older men produced sustained phonation with a higher Fo than their reading or extemporaneous samples. The eight subjects with unilateral vocal-fold paralysis (seven women, one man) produced samples with a pattern similar to that of the older normal groups but with greater differences between the sustained vowel and speech samples. The use of different sample types resulted in variations in mean speaking Fo in the normal subjects as well as in the vocal-fold-paralysis group. Within-day sampling of all normal subjects resulted in approximately the same variability as across-day sampling. In the vocal-fold-paralysis group, within-day sampling resulted in greater variability of mean Fo for vowels than for connected speech, following a pattern similar to the older normal control subjects and various speech materials for voice.(ABSTRACT TRUNCATED AT 250 WORDS)

Adult↗