Search PubMed⌕ Search

SEARCH · Search PubMed

Results for “Analytic Sample Preparation Methods”

Search indexed PubMed citations on genomics, clinical trials, systematic reviews and public health. Explore titles, authors and supplied subject terms, then open the PubMed record.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 541 records · Page 30Linked to original sources
PubMed2003

A sensitive method for detection of sulfamethazine and N4-acetylsulfamethazine residues in environmental samples using solid phase immunoextraction coupled with MALDI-TOF MS.

Sulfamethazine (SMT) and its major metabolite, N(4)-acetylsulfamethazine (NA-SMT), were each recovered from spiked water (0.1 ppb) and 10% (w/v) aqueous suspensions of soil (1 ppb) or composted manure (1 ppb), by using a three-stage solid phase immunoextraction (SPIE) system, followed by detection with matrix-assisted laser/desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS). Sulfonamide recovery rates are reported for separate stages of the SPIE system and for trace-level sulfonamide SPIE extraction from the environmental samples. SPIE MALDI-TOF MS is a rapid and definitive technique with potentially better efficiency relative to other established trace-level sulfonamide analytical methods. SPIE MALDI-TOF MS required 1.5 h per batch (8-24 samples/batch) for sample enrichment, 5 min per batch for probe preparation, and 5 min per sample to acquire and process the spectrum. This is the first time MALDI-TOF MS has been reported as a potential means of detecting trace-level drug residues in complex environmental samples.

Anti-Infective Agents↗
PubMedDate not supplied

TLC determination of mebendazol and pentoxifylline as residues on pharmaceutical equipment surfaces.

This paper presents the applicability of thin-layer chromatographic methods with a subsequent densitometric or video densitometric quantitation for determination of residues in controlling pharmaceutical equipment cleanliness. Analytical methods were developed for monitoring residues of pentoxifylline at 10 mg/M2 and mebendazol at 1 mg/M2 on stainless steel surfaces. Simulated samples were prepared by addition of a calculated amount of pharmaceutical (as a solution) on a 35 x 35 cm stainless steel surface. After evaporation of solvent, the residues were wiped with wetted cotton. The cotton was extracted with dichloromethan-methanol (1 + 1). Filtered extract was concentrated by vacuum evaporation and an aliquot applied to the plate, where standards were also applied. In the narrow concentration range near the acceptable residue limits, linear calibration curve could be obtained for both substances. The mean recovery (n = 4) obtained by densitometric quantitation was 93.4% for pentoxifylline and 85.6% for mebendazol, with coefficients of variation of 3.5 and 8.3%, respectively. Results of video densitometric quantitation did not differ significantly. However, data acquisition and evaluation is faster compared with densitometry and allows better archiving possibilities as required by the regulatory authorities. Both quantitation modes can be applied to routine control of pharmaceutical equipment cleanliness.

Calibration↗
PubMed1990

Liquid-chromatographic measurement of biopterin and neopterin in serum and urine.

We report an improved "high-performance" liquid-chromatographic (HPLC) method for measuring biopterin and neopterin in serum and urine. Specimens are acidified, treated with iodine in 0.2 mol/L trichloroacetic acid, party purified on Bio-Rad MP-50 cation-exchange columns, and analyzed by reversed-phase HPLC with fluorometric detection. The minimal concentration of biopterin detectable is 0.3 micrograms/L in a 50-microL injection. The total CV is less than or equal to 10%. Improvements over other reported methods include the use of a single, simplified sample-preparation step with a Baker-10 SPE System, and a guard column to increase analytical column stability and analyte recovery. The assay is semiautomated to reduce technician time and improve precision. Mean observed values for biopterin and neopterin in sera of normal human adults were 1.64 and 5.52 micrograms/L, respectively. The mean ratio of neopterin to biopterin in acidified adult urine samples was lower than that found in matched nonacidified samples (n = 10). Serum specimens from diagnosed phenylketonuric (PKU) and hyperphenylalaninemic patients were also analyzed for biopterin and neopterin; the findings agreed with reported values for similar patients. One patient, previously identified as an atypical PKU patient, showed serum values of neopterin and biopterin suggestive of a defect in biopterin synthesis.

Adolescent↗
PubMedDate not supplied

Determination of platinum in wine by graphite furnace atomic absorption spectrometry.

A method based on graphite furnace atomic absorption spectrometry (GFAAS) was developed for determining platinum in wine. Wine samples were prepared by microwave acid digestion or dry mineralization. The method of standard addition was used for Pt determination in untreated wine samples and mineralized samples. Analyte modifiers and furnace conditions were optimized. Effects of cations (Mg2+, Ca2+, K+, Na+, and NH4+) and anions (PO4(3)-, SO4(2)-) were tested separately and in combination. Analytical characteristics of the method were optimized for analyte recovery and signal enhancement. Recoveries ranged from 92.5 to 102%, and precision reproducibility relative standard deviation varied from 7.5 to 10%. Red, rosé, and white wines from France were analyzed. Platinum levels found in most wines were very low (< 10 micrograms/L).

Calcium↗
PubMed1996

Determination of alosetron in human plasma or serum by high-performance liquid chromatography with robotic sample preparation.

A method of analysis for the determination of alosetron in human plasma or serum has been developed. The method was fully automated using a laboratory robot in order to improve analytical precision, efficiency and safety. The assay involved solid-phase extraction with reversed-phase HPLC separation and fluorescence detection. A validation exercise over the concentration range of 0.1 to 20 ng/ml demonstrated the selectivity, linearity, sensitivity, accuracy, precision, extraction efficiency, ruggedness and stability of the method. The method has been applied in support of numerous human pharmacokinetic/biopharmaceutic studies over the last five years.

Carbolines↗
PubMedDate not supplied

Analyte stability study of N-methylcarbamate pesticides in beef and poultry liver tissues by liquid chromatography.

To optimize conditions for sample collection, preparation, storage, and analysis and to assure the validity of our previously published liquid chromatographic (LC) method for carbamate analysis in tissue, stabilities of 16 N-methylcarbamates in beef, duck, and chicken liver tissues were studied by using 2 sampling protocols. Tissue samples were fortified at room temperature to a concentration 5 to 10 times greater than either the Environmental Protection Agency tolerance level for each compound (if established) or the concentration used in the previously published method. Thereafter, samples were continuously frozen at -4 degrees C for varying time intervals. In the first study, samples were analyzed one day (initial) and 0.5, 1, 1.5, 2, 3, 4, 5, and 6 months after fortification. In the second study, samples were analyzed one day (initial) and 0.5, 1, 2, 3, and 6 months after fortification. For each residue and species, a minimum of 4 samples were analyzed by LC at each point in time, and the mean represented analyte concentration at the end of each time interval. Rates of residue depletion varied among analytes and among species. Depletion rates were greater in duck livers than in beef livers. Methomyl and oxamyl were depleted completely within 2 weeks. Between 2 and 6 months after sample fortification, residue depletions to levels below detection limits were observed for aldicarb, aldicarb sulfoxide, aldicarb sulfone, dioxacarb, promecarb, propoxur, and bendiocarb. The initial loss of certain carbamates during sample preparation in tissues exposed to room temperature for up to 8 h was greater than the subsequent rate of loss. Results indicate that cryogenic conditions are required for sample preparation and storage.(ABSTRACT TRUNCATED AT 250 WORDS)

Animals↗
PubMed1993

Evaluation of sampling and analytical methods for the determination of chlorodifluoromethane in air.

In January 1989, the Occupational Safety and Health Administration (OSHA) published revised permissible exposure limits (PELs) for 212 compounds and established PELs for 164 additional compounds. In cases where regulated compounds did not have specific sampling and analytical methods, methods were suggested by OSHA. The National Institute for Occupational Safety and Health (NIOSH) Manual of Analytical Methods (NMAM) Method 1020, which was developed for 1,1,2-trichloro-1,2,2-trifluoroethane, was suggested by OSHA for the determination of chlorodifluoromethane in workplace air. Because this method was developed for a liquid and chlorodifluoromethane is a gas, the ability of NMAM Method 1020 to adequately sample and quantitate chlorodifluoromethane was questioned and tested by researchers at NIOSH. The evaluation of NMAM Method 1020 for chlorodifluoromethane showed that the capacity of the 100/50-mg charcoal sorbent bed was limited, the standard preparation procedure was incorrect for a gas analyte, and the analyte had low solubility in carbon disulfide. NMAM Method 1018 for dichlorodifluoromethane uses two coconut-shell charcoal tubes in series, a 400/200-mg tube followed by a 100/50-mg tube, which are desorbed with methylene chloride. This method was evaluated for chlorodifluoromethane. Test atmospheres, with chlorodifluoromethane concentrations from 0.5-2 times the PEL were generated. Modifications of NMAM Method 1018 included changes in the standard preparation procedure, and the gas chromatograph was equipped with a capillary column. These revisions to NMAM 1018 resulted in a 96.5% recovery and a total precision for the method of 7.1% for chlorodifluoromethane. No significant bias in the method was found. Results indicate that the revised NMAM Method 1018 is suitable for the determination of chlorodifluoromethane in workplace air.

Air Pollutants, Occupational↗
PubMed2005

High extraction efficiency fiber coated with calix[4] open-chain crown ether for solid-phase microextraction of polar aromatic and aliphatic compounds.

The calix[4] open-chain crown ether, 5,11,17,23-tetra-tert-butyl-25,27-di(2-allyloxyethoxyl)-26,28-dihydroxycalix[4]arene was synthesized and used for preparation of solid-phase microextraction (SPME) fibers of enhanced extraction efficiency. The new SPME coating made from calix[4] open-chain crown ether and hydroxyl-terminated silicone oil was developed with the aid of vinyltriethoxylsilane as bridge using sol-gel method and cross-linking technology. The efficiency of the novel fiber in the extraction of polar aromatic and aliphatic compounds, such as phenols, alcohols, and volatile fatty acids, was also investigated. Due to the introduction of the polar open-chain crown ether in calix[4]arene molecules, the calix[4] open-chain crown ether fiber showed much better selectivity and sensitivity to these polar compounds in comparison with calix[4]arene fiber. It also had superior extraction efficiency when compared to commercial poly(dimethylsiloxane)-divinylbenzene and polyacrylate fibers. Parts per billion to parts per trillion level detection limits were achieved for most of the analytes through SPME in conjunction with GC and flame ionization detector. The linear ranges were two to four orders of magnitude, and the RSD values were below 7% for all analytes. The novel fiber was applied to determine volatile alcohols and fatty acids in wine samples. The volatile-free wine prepared in this work was used to assure similar chemical environment for analytes in both calibration solutions and in real wine samples, thus compensating for possible matrix interferences. The established internal standard method using 4-methyl-2-pentanol as internal standard showed satisfactory accuracy and precision.

Alcohols↗
PubMed2000

Alpha spectrometry sample preparation using selectively adsorbing thin films

Several years ago, Switzerland introduced limits for natural radionuclides in food, e.g. 1 Bq/l for 226Ra or 10 Bq/l for the sum of 238U and 234U in drinking water. To make enforcement by regional (cantonal) laboratories more attractive, simplified analytical methods had to be offered, at least for drinking water. A first step has been the development of radium adsorbing sheets. A 20 mm x 20 mm MnO2 film on a polyamide substrate adsorbs more than 80% of the radium present in a 100 ml water sample within 6 h. The film is thin enough to allow for high resolution alpha spectrometry. A second step now under way is to produce thin films, which selectively adsorb uranium. Actually, an ion exchange resin with diphosphonic and sulfonic acid groups is used for this purpose. Although not yet very thin, these films make possible energy resolutions far better than with any liquid scintillation alpha spectrometry method. Adsorption efficiencies are more than 80% after 20 h exposition to a 100 ml water sample (20 mm x 20 mm sheet). A third step is to have a system that measures radionuclide concentrations in water on-line. A prototype is presented where radionuclides are adsorbed on a film in contact with the water. A Si-detector placed on the other side of the film support counts the alphas passing through.

Journal Article↗
PubMed2000

A RIA combined with SPE for the determination of a dual D2-receptor and beta2-adrenoceptor agonist, AR-C68397XX, in human plasma.

A radioimmunoassay has been developed for the determination of AR-C68397XX, a dual D2-receptor and beta2-adrenoceptor agonist, in human plasma. The method incorporates solid phase sample extraction and is suitable for the determination of the analyte at pg ml(-1) concentrations. The antiserum was raised in Suffolk cross sheep following primary and booster immunisations with an immunogen prepared by conjugating a carboxyphenylmethyl derivative of AR-C68397XX, to bovine serum albumin. The radioligand was prepared by the 125I-labelled iodination of a derivative of AR-C68397XX. The solid phase extraction procedure, using octadecyl sorbent, was introduced to remove matrix interferences in the plasma and to enhance method sensitivity. The calibration range is 20-500 pg ml(-1), using 0.5 ml of undiluted human plasma sample.

Adrenergic beta-2 Receptor Agonists↗
PubMed2003

Element speciation definitions, analytical methodology, and some examples.

This paper gives definitions related to element speciation and the reasons for the need for speciation. The problems focused on, involve sampling, sample preparation and storage, as well as changes in species information that occur during the use of various separation technologies. However, the potential and advantages of the separation methods in element speciation are also discussed. In addition, problems arising during element detection that are attributable to analytes or mobile-phase composition are outlined, as well as the pronounced advantages of detection by inductively coupled plasma-mass spectrometry (ICP-MS). The combination of the various separation systems with element- or molecule-specific detectors creates problems especially in element speciation. These difficulties are described along with recent developments for overcoming them or for improving their coupling efficiency. Finally, several elements for which the issue of speciation is important are discussed, with examples from some recent publications on arsenic, selenium and iodine speciation.

Environmental Monitoring↗
PubMed1997

Analysis of perillic acid in plasma by reversed-phase high-performance liquid chromatography with ultraviolet detection.

A simple and sensitive isocratic high-performance liquid chromatographic (HPLC) method with UV detection for the quantitation of perillic acid, a major circulating metabolite of perillyl alcohol and d-limonene, in plasma is described. Sample preparation involved protein precipitation and subsequent transfer and dilution with 10 mM NaHCO3. The mobile phase consisted of acetonitrile (36%) and 0.05 M ammonium acetate buffer pH 5.0 (64%). Separations were achieved on a C18 column and the effluent monitored for UV absorption at the analytes' respective UVmax. Separation was excellent with no interference from endogenous plasma constituents. This method was found suitable for quantifying drug concentrations in the range of 0.25 to 200.0 micrograms/ml using a 0.05-ml plasma sample, and was used to study the plasma pharmacokinetics of perillic acid in mice.

Animals↗
PubMed1996

Sensitive gas chromatographic method for determination of mercapturic acids in human urine.

A method was developed for sensitive determination of the specific benzene metabolite S-phenylmercapturic acid and the corresponding toluene metabolite S-benzylmercapturic acid in human urine for non-occupational and occupational exposure. The sample preparation procedure consists of liquid extraction of urine samples followed by precolumn derivatization and a clean-up by normal-phase HPLC. Determination of analytes occurs by gas chromatography with electron-capture detection. With this highly sensitive method (detection limits 60 and 65 ng/l, respectively) urinary S-phenylmercapturic and S-benzylmercapturic acid concentrations for non-occupationally exposed persons (e.g. non-smokers) can be measured precisely in one chromatographic run. Validation of the method occurred by comparison with a HPLC method we have published recently.

Acetylcysteine↗
PubMed1998

Quantitation of N-ethyl-3,4-methylenedioxyamphetamine and its major metabolites in human plasma by high-performance liquid chromatography and fluorescence detection.

A HPLC method has been developed for the analogue of Ecstasy MDE and its major metabolites N-ethyl-4-hydroxy-3-methoxyamphetamine (HME) and 3,4-methylenedioxyamphetamine (MDA) in human plasma. In the course of our investigations we found that the methylenedioxyamphetamines and HME exhibit fluorescence at 322 nm. Therefore the detection could be carried out with a fluorescence (FL) detector. Solid-phase extraction was used for sample preparation and yielded high recovery rates greater than 95%. The limit of quantitation for MDE and its metabolites in the extracts was between 1.5 and 8.9 ng/ml and the method standard deviations were less than 5%. This sensitive, rapid and reliable analytical method has been used successfully in the quantitation of the substances in plasma samples obtained from 14 volunteers in two clinical studies after p.o. administration of 100 to 140 mg MDE*HCI. The maximum plasma concentrations were 235-465 ng/ml (MDE), 67-673 ng/ml (HME) and 7-33 ng/ml (MDA), respectively. Pharmacokinetic parameters have been investigated using the plasma concentration curves.

3,4-Methylenedioxyamphetamine↗
PubMed2004

Hydrophilic interaction chromatography combined with tandem-mass spectrometry to determine six aminoglycosides in serum.

A specific and automated method was developed to quantitate the aminoglycosides amikacin, gentamicin, kanamycin, neomycin, paromomycin, and tobramycin simultaneously in human serum. Samples were prepared with an automated solid phase extraction (SPE). The hydrophilic interaction chromatography (HILIC) was used for separation of analytes from endogenous compounds and baseline separation. The aminoglycosides were detected with electrospray ionisation tandem mass spectrometry (ESI-MS-MS). Using a volume of 500 microl biological sample the lower limits of quantification were 100 ng/ml or better. The described HILIC-MS-MS method is suitable for therapeutic drug monitoring and for clinical and pharmcokinetical investigations of the aminoglycosides.

Aminoglycosides↗
PubMed2000

Automated sample preparation of Roxifiban tablets: transfer of a manual method to an automated workstation.

Automation offers obvious advantages for the preparation of tablets prior to analysis by HPLC including unattended operation, minimization of human intervention and an electronic audit trail. However, significant effort has to be put in up front to develop and validate an automated method, particularly if it is required to closely follow an existing manual method. Here, method transfer for Roxifiban, a fibrinogen receptor antagonist, will be discussed. A Zymark tablet processing workstation II (TPWII) was used for all automated sample preparations. Manual methods for composite assay, content uniformity, weight variation and degradation products testing of a tablet formulation were transferred to the TPWII. The method involved weighing of the sample, disintegration of the dosage form by homogenization, extraction of the analyte in the homogenate solution, filtration of the homogenate, dilution of the filtrate and transfer to autosampler vials. Obstacles to a quick transfer included limitations in the volume capabilities of the TPWII, poor analyte solubility and achieving proper conditioning of the transfer lines and filter. After resolving these issues, a validated method was achieved. Spiked recoveries were from 99.4 to 101.1% (RSD's <0.5%). A cross-validation between automated and manual assay methods was compared by Westlake analysis giving a 0.7% calculated interval at the 95% confidence level. Carryover was 0.07% after 20 sample preparations at the highest tablet strength.

Amidines↗
PubMed2003

Separation, identification, and characterization of microorganisms by capillary electrophoresis.

The use of capillary electrophoresis (CE) for the analysis, identification, and characterization of microorganisms has been gaining in popularity. The advantages of CE, such as small sample requirements, minimal sample preparation, rapid and simultaneous analysis, ease of quantitation and identification, and viability assessment, make it an attractive technique for the analysis of microbial analytes. As this instrumental method has evolved, higher peak efficiencies have been achieved by optimizing CE conditions, such as pH, ionic strength, and polymer additive concentration. Experimental improvements have allowed better quantitation and more accurate results. Many practical applications of this technique have been investigated. Viability and identification of microbes can be accomplished in a single analysis. This is useful for evaluation of microbial analytes in consumer products. Diagnosis of microbe-based diseases is now possible, in some cases, without the need for culture methods. Microbe-molecule, virus-antibody, or bacteria-antibiotic interactions can be monitored using CE, allowing for the screening of possible drug candidates. Fermentation can be monitored using this system. This instrumental approach can be adapted to many different applications, including assessing the viability of sperm cells. Progress has been made in the development of microelectrophoresis instrumentation. These advances will eventually allow the development of small, dedicated devices for the rapid, repetitive analyses of specific microbial samples. Although these methods may never fully replace traditional approaches, they are proving to be a valuable addition to the collection of techniques used to analyze, quantitate, and characterize microbes. This review outlines the recent developments in this rapidly growing field.

Animals↗
PubMed2006

Mass spectrometric quantitation of C-reactive protein using labeled tryptic peptides.

Given the extensive efforts applied toward proteomics and research in biomarkers, methods for the simultaneous measurement of proteins, peptides, metabolic intermediates, hormones, etc. in a complex sample may be required in the foreseeable future. Assays based on mass spectrometric detection may be suitable for meeting the demands of such complex samples with sensitivity and specificity. An analytical method for the quantitation of C-reactive protein (CRP), a well-known marker of inflammation, is described. Exact quantities of two synthetic (13)C-labeled CRP tryptic peptides were added as internal standards directly to the sample prior to chemical treatment, trypsinization, and liquid chromatography/mass spectrometry quantitation. C-reactive protein levels based on isotopic response ratios were measured. Intact C-reactive protein was spiked into blank rat urine for chemical and enzymatic treatment, producing linear response ratios of labeled to unlabeled peptides. For rigorous quantitation, standard curves, and quality control samples were prepared in rat urine with highly purified labeled and unlabeled peptides over the 50 pg-5 ng/muL concentration range. Using the same chemical and enzymatic treatment used for digestion of intact CRP, data from these samples demonstrated excellent analytical performance. The method was successfully applied toward the quantitation of urinary C-reactive protein from a study of drug-induced nephrotoxicity.

Amino Acid Sequence↗