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At least 1,243 records · Page 69Linked to original sources
PubMed1995

Effects of different sampling strategies on predictions of blood cyclosporine concentrations in haematological patients with multidrug resistance by Bayesian and non-linear least squares methods.

The Bayesian method (BM) can use previous information for the optimization of dosage regimen. However, Bayes' law remains true when the parameters are obtained from the infinite population. Therefore a bias might exist in the previous information and affect BM predictive performance. To overcome this shortcoming, the blood drug concentration of a patient can be used to individualize his pharmacokinetic parameters. Until now, at least two sampling strategies, i.e. steady-state and non-steady-state sampling strategies, have been developed to individualize and predict blood drug concentration. In the present study we used five sampling strategies: (1) all samples; (2) post-infusion samples; (3) during-infusion samples; (4) samples within 95% confidence interval/interquartile range of a steady-state concentration; (5) the sample of the mean/median at the mid-time-point of a steady-state to individualize and predict blood cyclosporine concentrations in haematological patients with multidrug resistance. We investigated the effects of different sampling strategies on BM and the nonlinear least squared method (NLLSM) predictive performances. The results showed that BM predictive performance was better than NLLSM. But the results did not prove that the steady-state sampling strategies were superior to the non-steady-state ones.

Adult↗
PubMed2000

Evaluation of a prototype Amplicor PCR assay for detection of human immunodeficiency virus type 1 DNA in blood samples from Tanzanian adults infected with HIV-1 subtypes A, C and D.

BACKGROUND: In previous evaluations, the standard Amplicor HIV-1 DNA PCR test (Roche Diagnostic Systems) has been reported to have low sensitivity for the detection of some non-B HIV-1 subtypes. It has therefore become necessary to determine the performance of commercially available as well as prototype HIV-1 PCR assays for HIV-1 DNA detection in samples from various geographical settings, in order to assess their ability to detect the different HIV-1 genotypes. OBJECTIVES: To determine the performance of the prototype Roche Amplicor version 1.5 PCR test in comparison to that of the standard Roche Amplicor PCR test for the detection of HIV-1 DNA in blood samples from HIV-1 seropositive pregnant Tanzanian women infected with various HIV-1 subtypes. STUDY DESIGN: This was a cross-sectional study done on 161 blood samples collected from 106 HIV-1 seropositive and 55 seronegative asymptomatic pregnant women attending antenatal clinic in Dar es Salaam, Tanzania. METHODS: Cell pellets for PCR were prepared from EDTA blood by the Amplicor whole blood PCR sample preparation method. Plasma was used for HIV serology by enzyme linked immunosorbent assays. Subtyping was done by the heteroduplex mobility assay (HMA) using cell pellets and/or plasma. RESULTS: The sensitivities of the prototype PCR and the standard assays were 99.1% (105/106) and 97% (99/102), respectively. All samples from 55 HIV-1 seronegative women were negative by both PCR assays. Among the 101 samples subtyped by HMA, 48 (47%) were subtype A, 30 (30%) subtype C, 20 (20%) subtype D and 3 (3%) were indeterminate. In the standard DNA PCR assay, a statistically significantly higher proportion of subtype A samples had a low level of reactivity as measured as optical density compared with the subtypes C and D samples while in the prototype assay all three subtypes showed a high level of reactivity. CONCLUSIONS: The Amplicor version 1.5 DNA PCR test has a high sensitivity for the detection of HIV-1 DNA in blood samples from Tanzanian adults. Since performance of this assay does not appear to be influenced by differences in HIV-1 subtypes A, C and D, it has the potential for use in the detection of HIV-1 DNA in samples from geographic areas where these subtypes are prevalent.

Adult↗
PubMed2002

Life situation related to the ICD implantation; self-reported uncertainty and satisfaction in Swedish and US samples.

The aim of the study was to describe changes in the life situation related to the ICD implantation of Swedish and US samples with regard to uncertainty and satisfaction. The life situation was measured by reference to the uncertainty caused by the condition and satisfaction with the life situation. Inferential statistics were used to analyse changes within and between the Swedish and US samples. Uncertainty showed a statistically significant difference between the Swedish and US samples before as well as after the ICD implantation. A higher level of uncertainty was indicated for the US sample prior to the ICD implantation and for the Swedish sample following the implantation. In the Swedish sample, satisfaction with life showed a statistically significant difference within the socio-economic domain, indicating a higher degree of satisfaction 3 months after implantation. Satisfaction within the domains of health and functioning, socio-economics and psychological-spiritual showed a statistically significant difference between the Swedish and US samples both before and after ICD implantation, indicating a higher degree of satisfaction in the US sample. The previous study shows that the ICD-patient's life situation is changed after the implantation and that it is necessary to provide the patient with information and education based on their own preconditions. The fact that US sample was investigated at a later stage after ICD implantation than the Swedish sample may have influenced the results of the study.

Aged↗
PubMed2005

Ultrasound scan-guided core sampling for diagnosis versus freehand FNAC of the thyroid gland.

BACKGROUND AND AIM: Freehand fine needle aspiration cytology (FNAC) is an obligatory investigation of the thyroid nodule. Between 5.0-43.1% of FNAC samples are reported as being initially unsatisfactory. In our unit, thyroid freehand FNAs are performed with a small needle (21 or 23G). Non-dominant nodules as part of multinodular goitres, difficult to palpate nodules or nodules with previously unsatisfactory freehand FNACs are sampled under ultrasound scan (USS) guidance with the larger 20G cutting core sampling technique. We aimed to compare the satisfactory sampling rate and safety of the two different methods. PATIENTS AND METHODS: Cytology forms were reviewed for 262 freehand FNACs and USS-guided core samples, performed in our unit over a two-year interval (1 July 1999 to 30 June 2001). RESULTS: Ultrasound-guided core samples for cytology were unsatisfactory (AC0-1) in 19/121 (15.6%) of the cases, compared with 66/141 (46.8%) of freehand FNACs (p value = < 0.0001). Ten out of eleven patients (91%) had a satisfactory USS-guided core after an unsatisfactory freehand FNA; 7/15 patients (46.7%) had satisfactory repeat freehand FNACs following an initial unsatisfactory freehand FNAC (p value = 0.0191). There were no complications as a result of either freehand FNAC or USS-guided core sampling. CONCLUSION: USS-guided cores provided more satisfactory samples for assessment than freehand FNACs. The USS-guided technique is safe despite the use of the larger cuffing needle. The USS-guided core sampling was also a useful tool for repeat thyroid nodule sampling after an unsatisfactory freehand FNAC.

Biopsy, Fine-Needle↗
PubMed2006

Evaluating sample medications in primary care: a practice-based research network study.

BACKGROUND: No reports have objectively evaluated safety of samples in primary care practices. A study was conducted to determine adherence to the Institute for Safe Medication Practices (ISMP) recommendations for safe distribution of medication samples to minimize medication errors. METHODS: In 2004, 17 urban and rural primary care practices participated in a two-phase observational study: (1) a site visit to collect inventory data and perform assessment of medication sample dispensing procedures and (2) a survey questionnaire for providers and patients upon sample medication provision. RESULTS: No practices were compliant with all seven ISMP recommendations. Twelve of 17 practices had policies for sample medication dispensing, and 7 had policies for labeling. Sample medication use was evaluated for 585 office visits and 27 patient surveys. Fifty-eight sample medications were dispensed during 55 of 585 patient visits. Common reasons for using sample medications included availability and need for a short-term trial for a chronic medication. Verbal communication only was provided most of the time for patient education regarding appropriate sample medication use and side effects. DISCUSSION: Primary care practices in this research network did not follow safe and appropriate sample medication dispensing procedures as outlined by ISMP. Both labeling and patient instructions were inadequate and may increase the risk for medication errors.

Colorado↗
PubMed2006

Self-sampling for group B streptococcus in women 35 to 37 weeks pregnant is accurate and acceptable: a randomized cross-over trial.

OBJECTIVE: In Canada, screening for group B Streptococcus (GBS) in pregnant women is recommended at 35 to 37 weeks' gestation. Since there is normally no other indication for pelvic examination at this stage of pregnancy, women may be more comfortable performing the test themselves. We assessed the accuracy of self- sampling versus clinician sampling for GBS and women's preference for each collection method. METHODS: Consecutive patients presenting between October 2003 and April 2005 to a maternity centre in Hamilton for their 35- to 37-week prenatal visit were randomly allocated to having vaginal-rectal swabs self-collected, and then collected by a clinician, or to having the swabs clinician-collected, and then self-collected. The main outcomes were prevalence of infection and sensitivity of the two methods. Other analyses compared women who refused participation in the study with those who participated, and preference for sampling method before and after conducting the tests. RESULTS: Of the 386 women approached, 330 (85.5%) agreed to participate. The prevalence of GBS was 17.0% (56/330) and 18.8% (62/330) in the self-obtained and clinician-obtained specimens respectively (difference =1.8%; 95% confidence intervals [CI] -2.0-6.0). Sensitivity was 87.5% (95% CI 77.0-93.8) and 96.9% (95% CI 88.7-99.8) for the self-obtained and clinician-obtained specimens respectively. Women who declined to participate in self-sampling were significantly more likely not to have completed high school and to prefer clinician sampling. Prior to testing, 79% of women preferred self-sampling or had no preference. Preference was unchanged for approximately two-thirds of women after sampling. CONCLUSION: Self-sampling for GBS is an accurate and acceptable alternative for the majority of pregnant women. Less-educated women may be hesitant to self-sample, and clinician sampling should remain an option.

Adult↗
PubMed2000

Prestructured MALDI-MS sample supports.

Prestructured MALDI-MS sample supports have been developed that simplify high-throughput analysis of biomolecules and improve the detection sensitivity. The mass spectrometric sample support is coated with a thin layer of hydrophobic Teflon that carries an array of 200-microm gold spots, which provide hydrophilic sample anchors. Each transferred sample droplet contacts one anchor, on top of which, after solvent evaporation, the sample is exclusively deposited due to the strongly water repellent nature of the Teflon surface. The initial matrix concentration is kept low, enabling sample up-concentration by more than 2 orders of magnitudes before crystallization commences. As a result, the detection sensitivity is improved as documented by mass spectra recorded from 100 amol of various peptides, 1 fmol of a DNA 20 mer, and 5 fmol of a 130 bp PCR product. Size and spacing of the hydrophilic anchors are optimized for MALDI-MS performance (sample spot size approximately = laser irradiation spot size), for short analysis times (predetermined sample coordinates), and for high throughput sample preparation (sample anchor array according to the 1536 microtiter plate format).

DNA↗
PubMed2002

A high-throughput continuous sample introduction interface for microfluidic chip-based capillary electrophoresis systems.

The development of efficient sample introduction and pretreatment systems for microfluidic chip-based analytical systems is important for their application to real-life samples. In this work, world-to-chip interfacing was achieved by a novel flow-through sampling reservoir featuring a guided overflow design. The flow-through reservoir was fabricated on a 30 x 60 x 3 mm planar glass chip of crossed-channel design used for capillary electrophoresis separations. The 20-microL sample reservoir was produced from a section of plastic pipet tip and fixed at one end of the sampling channel. Sample change was performed by pumping 80-microL samples sandwiched between air segments at approximately 0.48 mL/min flow rate through the flow-through reservoir, introduced from an access hole on the bottom side of the chip. A filter paper collar wrapped tightly around the reservoir guided the overflowing sample solution into a plastic trough surrounding the reservoir and then to waste. The performance of the system was demonstrated in the separation and determination of FITC-labeled arginine, glycine, phenylalanine, and glutamic acid with LIF detection, by continuously introducing a train of different samples through the system without electrical interruption. Employing a separation channel of 4 cm (2-cm effective separation length) and 1.4-kV separation voltage, maximum throughputs of 80/h were achieved with <4.1% carryover and precisions ranging from 1.5% for arginine to 2.6% RSD (n = 11) for glycine. The sampling system was tested in the continuous monitoring of the derivatizing process of amino acids by FITC over a period of 4 h, involving 166 analytical cycles. An outstanding overall precision of 4.8% RSD (n = 166) was achieved for the fluorescein internal standard.

Journal Article↗
PubMed2004

An analytical device for on-site immunoassay. Demonstration of its applicability in semiquantitative detection of aflatoxin B1 in a batch of samples with ultrahigh sensitivity.

A simple analytical device has been developed for performing noninstrumental immunofiltration-based assay on a batch of samples. The device consists of membrane strips, with antibody-immobilized zones, attached to a polyethylene card. A moist filter paper placed between the membrane and the polyethylene card acts as the absorbent body. The device was used to estimate very low concentrations of aflatoxin B1 (AFB1) present in food samples by using an improved catalyzed reporter deposition (Super-CARD) method of signal amplification involving biotinylated tyramine (B-T) and avidin-horseradish peroxidase conjugate. 4-chloro-1-naphthol was used as the substrate for visualization. Semiquantitative results are obtained by visual comparison of the color intensity (inversely related to the analyte concentration) of a sample spot with those of reference standards. Quantitative estimation is possible by densitometric analysis (detection limit 0.25 pg/spot, 0.01 ng mL(-1)). Dilute samples can be assayed by in situ concentration with improved dose-response characteristics. A batch of 12 extracted samples can be analyzed in a single test card within 12 min. Spiked and contaminated samples of groundnut, corn, wheat, cheese, and chilli were analyzed without sample cleanup. The matrix interferences were eliminated by using appropriate dilution of the aqueous methanol extracts. Mean recoveries from different food samples were between 91 and 104%. The values obtained for infected corn and groundnut samples correlated well (R2=0.99) with the estimates by HPLC. The method is well-suited for visual screening of agricultural and food samples for AFB1 under field conditions.

Aflatoxin B1↗
PubMed2005

Sample handling for mass spectrometric proteomic investigations of human sera.

Proteomic investigations of sera are potentially of value for diagnosis, prognosis, choice of therapy, and disease activity assessment by virtue of discovering new biomarkers and biomarker patterns. Much debate focuses on the biological relevance and the need for identification of such biomarkers while less effort has been invested in devising standard procedures for sample preparation and storage in relation to model building based on complex sets of mass spectrometric (MS) data. Thus, development of standardized methods for collection and storage of patient samples together with standards for transportation and handling of samples are needed. This requires knowledge about how sample processing affects MS-based proteome analyses and thereby how nonbiological biased classification errors are avoided. In this study, we characterize the effects of sample handling, including clotting conditions, storage temperature, storage time, and freeze/thaw cycles, on MS-based proteomics of human serum by using principal components analysis, support vector machine learning, and clustering methods based on genetic algorithms as class modeling and prediction methods. Using spiking to artificially create differentiable sample groups, this integrated approach yields data that--even when working with sample groups that differ more than may be expected in biological studies--clearly demonstrate the need for comparable sampling conditions for samples used for modeling and for the samples that are going into the test set group. Also, the study emphasizes the difference between class prediction and class comparison studies as well as the advantages and disadvantages of different modeling methods.

Humans↗
PubMed2006

Centrifuge microextraction coupled with on-line back-extraction field-amplified sample injection method for the determination of trace ephedrine derivatives in the urine and serum.

Although sample stacking has enjoyed some degree of success in electrophoretic separation techniques, there is still a major problem with complex matrix sample as it suffers tremendously from sample matrix effects. A novel method that combines two concentration techniques, centrifuge microextraction (CME) and on-line back-extraction field-amplified sample injection (OLBE-FASI), is used to determine trace ephedrine derivatives in urine and serum by capillary zone electrophoresis. The CME, integrating the sample cleanup and preconcentration into a single step, is a promising sample preparation method for biological samples. The CME technique provided 9-14-fold enrichment within 10 min. The OLBE-FASI eliminated the need to perform solvent exchange and provided a further concentration of the analytes. Using CME coupled with OLBE-FASI, over a 3800-fold increase in sensitivity could be obtained as compared with the normal hydrodynamic injection without sample stacking. For a 1-mL urine sample, the linear range was 5/10-200 ng/mL with the square of the correlation coefficients (r(2)) ranging from 0.9988 to 0.9994. Detection limits were from 0.15 to 0.25 ng/mL using a photodiode array UV detection at wavelength 192 nm. The possibility of this method to determine ephedrine derivatives in 20-muL serum samples was also demonstrated.

Centrifugation↗
PubMed2003

Use of chloroflurocarbons as internal standards for the measurement of atmospheric non-methane volatile organic compounds sampled onto solid adsorbent cartridges.

Solid adsorbents have proven useful for determining the vertical profiles of volatile organic compounds (VOCs) using sampling platforms such as balloons, kites, and light aircraft, and those profiles provide valuable information about the sources, sinks, transformations, and transport of atmospheric VOCs. One of the largest contributions to error in VOC concentrations is the estimation of the volume of air sampled on the adsorbent cartridge. These errors arise from different sources, such as variations in pumping flow rates from changes in ambient temperature and pressure with altitude, and decrease in the sampling pump battery power. Another significant source for sampling rate variations are differences in the flow resistance of individual sampling cartridges. To improve the accuracy and precision of VOC measurements, the use of ambient chlorofluorocarbons (CFCs) as internal standards was investigated. A multibed solid adsorbent, AirToxic (Supelco), was chosen for its wide sampling range (C3-C12). Analysis was accomplished by thermal desorption and dual detection GC/FID/ECD, resulting in sensitive and selective detection of both VOCs and CFCs in the same sample. Long-lived chlorinated compounds (CFC-11, CFC-12, CFC-113, CCl4 and CH3CCl3) banned by the Montreal Protocol and subsequent amendments were studied for their ability to predict sample volumes using both ground-based and vertical profiling platforms through the boundary layer and free troposphere. Of these compounds, CFC-113 and CCl4 were found to yield the greatest accuracy and precision for sampling volume determination. Use of ambient CFC-113 and CCl4 as internal standards resulted in accuracy and precision of generally better than 10% for the prediction of sample volumes in ground-, balloon-, and aircraft-based measurements. Consequently, use of CFCs as reference compounds can yield a significant improvement of accuracy and precision for ambient VOC measurements in situations where accurate flow control is troublesome.

Adsorption↗
PubMed2005

Single-particle characterization of four "Asian Dust" samples collected in Korea, using low-Z particle electron probe X-ray microanalysis.

A single-particle analytical technique, named low-Z particle electron probe X-ray microanalysis (low-Z particle EPMA), employing an ultrathin window X-ray detector and enabling the quantitative determination of even low-Z elements such as C, N, and O, is applied to characterize "Asian Dust" samples, collected in ChunCheon, Korea, during four Asian Dust storm events on March 7, 2000, April 7, 2000, March 22, 2001, and May 17, 2001. In this study, it is demonstrated that single-particle analysis using the low-Z particle EPMA provides detailed information on various types of chemical species in the samples. The most abundantly encountered particles, both in coarse and fine fractions, are aluminosilicates. The relative abundances of those particles on the basis of their size are different between the four Asian Dust samples. The sample collected on March 7, 2000 did not experience any chemical modification during its transport because the sample does not contain particles of chemical species that result from atmospheric reactions. The sample collected on April 7, 2000 contains both genuine and reacted sea-salt particles. The genuine sea-salts are in the form of a mixture of NaCl and MgCl2 entrained during their passage over the Yellow Sea. The reacted sea-salts particles are encountered very much in fine fraction. The sample collected on March 22, 2001 shows somewhat significant chemical modification both for CaCO3 and sea-salts particles. For this sample, a significant number of reacted CaCO3 and sea-salt particles, such as those containing nitrate and/or sulfate, are encountered, implying that CaCO3 and sea-salts particles have reacted with sulfur or nitrogen oxide species during their long-range transport. The sample collected on May 17, 2001 experienced the most extensive chemical modification during its transport. In addition to the observation of the extensively reacted CaCO3 and sea-salt particles, reacted K2CO3 particles are also extensively encountered in this sample, which implies that K2CO3 species should be regarded as an additional important chemical species in the study of the chemical modification of Asian Dust particles during long-range transport.

Air Movements↗
PubMed2002

Characterization of soil organic matter content of two sample size populations along a climatic transect.

Soil organic matter (SOM) content was determined in two populations of soil samples that were taken from 0-2 soil depth. One population represented soil samples that were taken from a square of 25 cm2 in size (small-S population) and the other population represented soil samples that were taken from a square of 2500 cm2 in size (large-L population). The samples were collected on hillslopes in different climatic regions: Mediterranean (GIV), semi-arid (MAL), mildly-arid (MIS) and arid (KAL). The results of both S and L populations showed decreasing SOM mean and variance from the Mediterranean site to the arid site. Statistical and spatial characteristics of each population were compared between the climatic regions. In addition, comparison between the two populations was made for each site. The difference in sample size did not significantly affect the mean values of SOM of the two populations in sites GIV, MAL and KAL, but did affect the mean at site MIS. At all study sites, except for site MAL, the variance increased with decreasing sample size. At sites GIV and KAL the coefficient of variation of S population was higher (more than 1.5 times) than that of L population, whereas at sites MAL and MIS, the differences were negligible. The relationships between the values of S and L samples at the individual sampling points defined the background of the study sites, which reflects the effect of vegetation (type), grazing, biological crust and soil properties. It was found that at the extreme sites GIV and KAL the background was characterized by relatively low SOM content with small areas of high organic matter content. At site MIS the background was characterized by relatively high SOM with small areas of low organic matter content. At site MAL the background was not dominated by high values of SOM nor by low ones. The spatial pattern of L population became more simple with increasing aridity. At the relatively wet sites the spatial pattern did not depend on the sample size while in the more arid sites it was sample size dependent. It was indicated that the spatial structure of SOM at the semi-arid and mildly arid sites is anisotropic whereas at the Mediterranean and arid sites it is isotropic.

Climate↗
PubMed2003

Indonesia: statistical sampling technique in validation of radiation sterilisation dose of biological tissue.

The aim of the work is to find the best solution for statistical sampling technique in validation of radiation sterilization dose (RSD) for biological tissues, according to ISO standard. As a model for sampling are biological tissues retrieved from one cadaver donor which consist of frozen bone grafts (18 packets), lyophilized allografts (68 packets) and demineralized bone powder grafts (40 packets). The size and type of products vary from long bones, cancellous chips to bone powders, tendons and facia lata, that make the number of bioburden per product could not be treated equally. Frozen samples could not be considered as the same production batch with lyophilized samples, because of different processing and irradiation temperature. The minimum number of uniformed samples needed for validation per production batch size, according to ISO 13409, is from 20 to 79 and 20 of them will be used for the test sample size, i.e. 10 for bio-burden determination and the remaining 10 for verification dose. Based on the number of uniformed grafts, statistical sampling can be carried out on lyophilized and demineralized bone grafts, but not on frozen bone grafts. Bioburden determinations were carried out and validated according to ISO 11737-1. Results of average bioburden determination (cfu/per packet), using sample item portion (SIP) = 1, are 5 cfu/packet for lyophilized bone grafts and 4 cfu/packet for demineralized bone powder grafts. Verification doses obtained were 2.40 kGy for lyophilized grafts and 2.24 kGy for demineralized bone powder grafts. The results of verification dose were accepted and the RSD of 25 kGy is substantiated It can be concluded that a statistical sampling technique can be applied if all the grafts produced in the same process such as lyophilized, demineralized as well as frozen are assumed to be in one production batch regardless of sample uniformity such as size, type and weight; for this ISO 13409 can be applied for the validation of RSD.

Journal Article↗
PubMed2005

Comparison of organophosphorus pesticide metabolite levels in single and multiple daily urine samples collected from preschool children in Washington State.

A total organophosphorus pesticide exposure study was conducted in Washington State in 1998 in a sample population of 13 children aged 2.5-5.5 years. The children were roughly split between rural and suburban populations and had been previously identified as having potentially elevated organophosphorus pesticide exposures. One component of the study was urine collection and analysis. Urine samples were collected from each subject up to four times in 24 h in two different seasons. Samples were collected at specific time points: before bed, first morning void, after lunch, and before dinner. Urine samples were analyzed initially for the six nonspecific dialkylphosphate (DAP) metabolites and subsequently for eight specific metabolites including malathion dicarboxylic acid (MDA), 3,5,6-trichloro-2-pyridinol (TCPy), and paranitrophenol (PNP). Relatively large percentages of the urine samples contained quantifiable amounts of two of the nonspecific DAP metabolites (DMTP-97%; DETP-67%), and three of the specific metabolites (MDA (71%), TCPy (79%), and PNP (96%)). A percent deviation analysis was employed to determine which of the spot sample time points was the best predictor of the estimated volume-weighted daily average. Of the four spot samples collected, first morning void samples were consistently found to be the best predictors of weighted-average daily metabolite concentration. This finding also held when the data were creatinine-adjusted. The results of this analysis suggest that if spot sampling is to be conducted as part of a biological monitoring study, first morning void samples should be preferentially collected.

Child, Preschool↗
PubMed1998

Optimisation of sample presentation for the near-infrared spectra of pharmaceutical excipients.

The effects of sample presentation on near-infrared (NIR) reflectance spectra were examined. Using a Foss NIRSystems Rapid Content Analyzer, which uses sample cups for sample presentation, four important parameters were identified: cup diameter, sample thickness, cup material and packing method. Below a critical diameter of 20 mm, which is dependent on the detector geometry, the spectra became increasingly distorted (i.e., changes in spectral intensities and spectral shape, shifts in peak positions and occurrence of Wood's peak). The minimum sample thickness not to cause spectral distortion was dependent on the physical and chemical nature of the substance. A thickness > or = 10 mm was found to be adequate for most pharmaceutical excipients. The method of packing was also important. Tapping a powdered sample sometimes caused significant changes (P < 0.05) in the spectral absorbance values compared with simply pouring the sample into the sample cup. Standard sample cups made from quartz were to be preferred owing to their lack of background absorptivity. However, the two commercially available flat based vials examined, which were made from soda glass and clear neutral glass, proved to be as suitable for all except applications of the most exacting nature. The spectral distortions resulting from variations in cup diameter, sample thickness and cup material were also shown to alter significantly the values of two commonly used identification algorithms, correlation coefficient (< 0.95) and maximum distance (> 3.0 standard deviation distance), sufficiently to cause misidentifications.

Pharmaceutical Preparations↗
PubMed2001

Sources of variability in collection and preparation of paint and lead-coating samples.

Chronic exposure of children to lead (Pb) can result in permanent physiological impairment. Since surfaces coated with lead-containing paints and varnishes are potential sources of exposure, it is extremely important that reliable methods for sampling and analysis be available. The sources of variability in the collection and preparation of samples were investigated to improve the performance and comparability of methods and to ensure that data generated will be adequate for its intended use. Paint samples of varying sizes (areas and masses) were collected at different locations across a variety of surfaces including metal, plaster, concrete, and wood. A variety of grinding techniques were compared. Manual mortar and pestle grinding for at least 1.5 min and mechanized grinding techniques were found to generate similar homogenous particle size distributions required for aliquots as small as 0.10 g. When 342 samples were evaluated for sample weight loss during mortar and pestle grinding, 4% had 20% or greater loss with a high of 41%. Homogenization and sub-sampling steps were found to be the principal sources of variability related to the size of the sample collected. Analysis of samples from different locations on apparently identical surfaces were found to vary by more than a factor of two both in Pb concentration (mg cm-2 or %) and areal coating density (g cm-2). Analyses of substrates were performed to determine the Pb remaining after coating removal. Levels as high as 1% Pb were found in some substrate samples, corresponding to more than 35 mg cm-2 Pb. In conclusion, these sources of variability must be considered in development and/or application of any sampling and analysis methodologies.

Child↗