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PubMed1992

Development and evaluation of analytical methodology for the determination of aflatoxins in palm kernels.

A rapid, simple and reproducible method for the simultaneous estimation of aflatoxins AFB1, AFB2, AFG1 and AFG2 in palm kernel samples has been developed by optimizing the sample preparation, solvent extraction, sample clean-up and quantification procedures. The aflatoxins are extracted from a slurried palm kernel sample with an acetone-water (80 + 20, v/v) mixture and the crude extract is cleaned up by solid-phase extraction using a phenyl bonded phase cartridge. The extract is passed through the cartridge with a water-methanol (93 + 7) mixture. Subsequent elution of the aflatoxins retained on the cartridge is achieved with a 3 ml aliquot of chloroform. The aflatoxin content of the eluate is quantified using a bi-directional high-performance thin-layer chromatography procedure. A critical evaluation of the proposed method was carried out by statistical comparison with the British Standard Method. The proposed procedure was shown to be more efficient and precise. Consistent recoveries of over 90% were achieved from spiked palm kernel extracts and detection limits were found to be 3.7, 2.5, 3.0 and 1.3 micrograms kg-1 for AFB1, AFB2, AFG1 and AFG2 aflatoxins, respectively.

Aflatoxins↗

PubMed2005

Analysis of perchlorate in human urine using ion chromatography and electrospray tandem mass spectrometry.

Because of health concerns surrounding widespread exposure to perchlorate, we developed a sensitive and selective method for quantifying perchlorate in human urine using ion chromatography coupled with electrospray ionization tandem mass spectrometry. Perchlorate was quantified using a stable isotope-labeled internal standard ((18)O(4)-perchlorate) with excellent assay precision (coefficient of variation <5% for repetitively analyzed quality control material). Analytical accuracy was established by blind analysis of certified proficiency testing materials prepared in synthetic urine matrix; calculated amounts deviated minimally from true amounts, with percent differences ranging from 2% to 5%. Selective chromatography and tandem mass spectrometry reduced the need for sample cleanup, resulting in a rugged and rapid method capable of routinely analyzing 75 samples/day. The lowest reportable level (0.025 ng/mL) was sufficiently sensitive to detect perchlorate in all human urine samples evaluated to date, with a linear response range from 0.025 to 100 ng/mL. This selective, sensitive, and rapid method will help elucidate any potential associations between human exposure to low levels of perchlorate and adverse health effects.

Adult↗

PubMed2000

Development and validation of a near infrared method for the analytical control of a pharmaceutical preparation in three steps of the manufacturing process.

A near infrared diffuse reflectance spectroscopy (NIRS) procedure for the quantitative control analysis of the active compound (otilonium bromide) in a pharmaceutical preparation in three steps of the production process (blended product, cores and coated tablets) and a methodology for its validation are proposed. The analytical procedure is composed by two consecutive steps. First, the sample is identified by comparing its spectrum with a second derivative spectral library. If the sample is positively identified, the active compound is quantified by using a previously established partial least squares (PLS) calibration model. The procedure was validated by studying repeatability, intermediate precision, accuracy and linearity. To this end, an adaptation of ICH (International Conference on Harmonisation) validation methodology to an NIR multivariate calibration procedure is proposed. The relative standard error of prediction (RSEP) was < or = 1% and the suitability of the procedure for control analysis was confirmed by the results obtained analysing new production samples produced over a three-month period.

Calcium Channel Blockers↗

PubMed1998

Determination of lamotrigine in biologic materials by a simple and rapid liquid chromatographic method.

Lamotrigine (LTG), a newly introduced antiepileptic drug, appears to have potential therapeutic advantages for the treatment of patients with partial-onset seizures. Increasing clinical application and research of LTG demand a simpler and more rapid analytical procedure to determine LTG concentration in body fluids and tissues. The authors have developed an effective one-step procedure for sample preparation followed by high-performance liquid chromatography (HPLC) to quantitate LTG in plasma, urine, and brain tissues. Body fluids and brain homogenates were treated with cold acetonitrile to precipitate protein. The samples were fractionated on a 250 x 4.6 mm C18 reversed-phase column with an isocratic mobile system consisting of potassium phosphate buffer, acetonitrile, and methanol (70:16:14). The method had a LTG detection limit of 0.02 microg/ml in plasma and 0.03 microg/ml in urine. The coefficients of variation were <2.7% for intraday and 4.2% for interday analyses. The recovery of LTG added to plasma, urine, and brain homogenate ranged from 98% to 100%. The method was applied to a clinical study to determine plasma and urine concentrations of LTG in subjects receiving a single oral dose of LTG. The calculated pharmacokinetic parameters were comparable to those previously reported. The method proved to be simple, fast, reproducible, and useful in clinical investigation and monitoring of LTG concentrations.

Acetonitriles↗

PubMed2005

Determination of ropivacaine in human plasma using highly selective molecular imprint-based solid phase extraction and fast LC-MS analysis.

A method for determining ropivacaine in human plasma using highly selective molecular imprint-based solid phase extraction and LC-MS analysis was developed. The imprinted extraction material was prepared using a structural analogue of ropivacaine as the template. The efficient sample cleanup achieved allowed single MS mode operation and analytical separation under isocratic conditions with a total separation time of less than two minutes. The absence of ion suppression was confirmed for both the m/z of ropivacaine and the m/z of the internal standard. The solid phase extraction protocol was optimised for elution of ropivacaine in a small volume of aqueous-rich solvent suitable for injection into a reversed phase LC-MS system. The final method measured trace levels of ropivacaine in human plasma with a limit of quantification of 2.5 nmol/L and interassay accuracy and precision of 101.7-104.4% and 2.1-7.2%, respectively.

Amides↗

PubMed2000

Extraction of polychlorinated dibenzo-p-dioxins and dibenzofurans from solid samples using the Randall technique.

This study deals with a new sample extraction technique which minimizes pollution in analytical laboratories whilst reducing sample preparation time and cost. The device uses the Randall technique for solid sample extraction, performed by immersion of the sample in boiling solvent. The fast solubilization operated by the hot solvent leads to a sharp reduction in extraction time. This method was tested for the extraction of polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) from different solid matrices using toluene as extractant, and compared with the conventional Soxhlet. The reduction in the extraction times (from 48 to 2 h) with an efficiency similar to or higher than that afforded by the conventional Soxhlet technique indicates the suitability of this method.

Benzofurans↗

PubMed1998

Automated free-solution isotachophoresis: instrumentation and fractionation of human serum proteins.

An automated free-solution isotachophoresis system (FS-ITP) for preparative fractionation of biopolymers is described, operated in a batch mode. The dimension of the separation chamber allows an up to 1200-fold higher sample load compared to separation in capillaries of 180 microm inner diameter as used in analytical capillary isotachophoresis (C-ITP). The preparative capacity of the system is within the milligram range. The method is fully compatible with analytical C-ITP, which is essential for preparative-scale isotachophoresis with regard to optimization of electrolyte systems and the search for suitable spacers. As a model application the fractionation of human serum proteins is reported. The collected fractions were analyzed by C-ITP and agarose gel electrophoresis.

Blood Proteins↗

PubMed2004

Simultaneous speciation of mercury and butyltin compounds in natural waters and snow by propylation and species-specific isotope dilution mass spectrometry analysis.

A robust method has been developed for simultaneous determination of mercury and butyltin compounds in aqueous samples. This method is capable of providing accurate results for analyte concentrations in the picogram per liter to nanogram per liter range. The simultaneous determination of the mercury and tin compounds is achieved by species-specific isotope dilution, derivatization, and gas chromatography-inductively coupled plasma mass spectrometer (GC-ICP-MS). In derivatization by ethylation and propylation, reaction conditions such as pH and the effect of chloride were carefully studied. Ethylation was found to be more sensitive to matrix effects, especially for mercury compounds. Propylation was thus the preferred derivatization method for simultaneous determination of organomercury and organotin compounds in environmental samples. The analytical method is highly accurate and precise, with RSD values of 1 and 3% for analyte concentrations in the picogram per liter to nanogram per liter range. By use of cleaning procedures and SIDMS blank measurements, detection limits in the range 10-60 pg L(-1) were achieved; these are suitable for determination of background levels of these contaminants in environmental samples. This was demonstrated by using the method for analysis of real snow and seawater samples. This work illustrates the great advantage of species-specific isotope dilution for the validation of an analytical speciation method-the possibility of overcoming species transformations and non-quantitative recovery. Analysis time is saved by use of the simultaneous method, because of the use of a single sample-preparation procedure and one analysis.

Hydrogen-Ion Concentration↗

PubMed1999

Use of X-ray crystallography for the characterization of single crystals grown in steroid containing transdermal drug delivery systems.

Target of the study was to characterize crystals which had grown in steroid-containing matrix patches during short-term storage and to thereby establish a rationale for the inhibition of crystal formation in those patches in general. Matrix type transdermal drug delivery systems (TDDS) containing either 2.2% gestodene or 3.3% estradiol were free of crystals directly after their production. However, crystals of up to 800 microns in length grew during 3 months of storage at ambient temperature. The application of several analytical methods did not help to identify the crystals. This was mainly due to the fact that the adhesive matrix surrounding the crystals could not be fully removed in the course of sample preparation with routine laboratory methods and thus impaired DSC, FTIR microscopy and hot stage polarized microscopy. However, within X-ray diffractometry, the residual amorphous patch matrix did not hamper the measurement of the crystals. Thus, they were identified as estradiol hemihydrate and gestodene form I, respectively. These results suggest that steroid-containing matrix TDDS should be stabilized against drug recrystallization e.g. by the addition of suitable crystallization inhibitors. Furthermore, systems containing estradiol may be stabilized by efficient removal water.

Administration, Cutaneous↗

PubMed2002

Identification of incurred sulfonamide residues in eggs: methods for confirmation by liquid chromatography-tandem mass spectrometry and quantitation by liquid chromatography with ultraviolet detection.

Two complementary methods for identifying and measuring sulfonamide residues in eggs were developed for use in surveying eggs for potential drug residues. The first method uses liquid chromatography-tandem mass spectrometry (LC-MS-MS) to confirm the presence of sulfonamide residues in eggs. During its validation the limit of confirmation was estimated to be 5-10 ng/g (ppb) depending on the drug. Also, a method for measuring residue level by liquid chromatography with ultraviolet detection (LC-UV) was validated using the same extraction procedure as the confirmatory method. The determinative method was validated over the 50-200 ppb range. Samples were prepared by homogenizing whole egg, extracting with acetonitrile, and cleaning up with a C(18) solid-phase extraction cartridge. For confirmation, analytes were separated by gradient LC on a C(18) column, ionized by electrospray ionization (ESI), and detected by MS-MS with an ion trap mass spectrometer. For determination, analytes were separated by a different gradient LC procedure and detected by UV at 287 nm. Fifteen drugs were dosed individually in laying hens, and residues of parent drug and/or metabolites were found in eggs for all the drugs. Validation was based on repetitive analyses of control samples, control samples fortified at 100 ppb sulfonamides, and samples of blended incurred eggs.

Animals↗

PubMed2001

Isotope dilution gas chromatography/mass spectrometry method for the determination of methionine sulfoxide in protein.

We have developed a new technique for quantifying methionine sulfoxide (MetSO) in protein to assess levels of oxidative stress in physiological systems. In this procedure, samples are hydrolyzed with methanesulfonic acid (MSA) in order to avoid the conversion of MetSO to methionine (Met) that occurs during hydrolysis of protein in HCl. The hydrolysate is fractionated on a cation exchange column to remove the nonvolatile MSA from amino acids, and the amino acids are then derivatized as their trimethylsilyl esters for analysis by selected ion monitoring-gas chromatography/mass spectrometry. The limit of detection of the assay is 200 pmol of MetSO per analysis, and the interassay coefficient of variation is 5.8%. Compared to current methods, the SIM-GC/MS assay avoids the potential for conversion of Met to MetSO during sample preparation, requires less sample preparation time, has lower variability, and uses mass spectrometry for sensitive and specific analyte detection.

Collagen↗

PubMed2003

Thorium concentration in Pakistani diet.

To evaluate radiation doses due to ingestion of thorium activity by members of the public, baseline analytical data on thorium concentration in a typical Pakistani diet was generated. Food samples were collected from major districts/ cities of the country using the market basket method, and typical daily diets were prepared. Thorium concentration was determined by instrumental neutron activation analysis. It was found to vary from 1.6 ng g(-1) to 12 ng g(-1). The median value was 4.6 ng g(-1). This leads to median daily thorium intake of 2.7 microg d(-1). The geometric mean was 2.6 microg d(-1), which was 13% less than the ICRP value. Based on these measurements the average intake of 232Th activity was 10 mBq d(-1), and the average annual and committed effective doses for adults were estimated to be 8.8 x 10(-7) Sv y(-1) and 4.4 x 10(-5) Sv, respectively.

Diet↗

PubMed2001

Development and validation of a sensitive analytical method for the simultaneous determination of buprenorphine and norbuprenorphine in human plasma.

A sensitive, specific, and robust capillary gas chromatography-mass spectrometry method has been developed and validated for simultaneous determination of buprenorphine and its active metabolite, norbuprenorphine, in human plasma. Sample preparation involved a clean-up procedure using a Bond Elut Certify cartridge followed by derivatization with pentafluoropropionic anhydride. Separation was carried out on a HP-1 fused silica capillary column using helium as the carrier gas. Selected ion monitoring was used in the electron impact mode. Excellent linearity was found between 0.10 and 20.0 ng/ml with a limit of quantitation of 0.05 and 0.10 ng/ml for buprenorphine and norbuprenorphine, respectively. Interday and intraday assay precisions (%CV) and accuracies were within 15.0% for buprenorphine and norbuprenorphine, respectively. Recoveries were quantitative and concentration-independent. This method will be applied to pharmacokinetic/pharmacodynamic/bioequivalence studies of buprenorphine in humans.

Analgesics, Opioid↗

PubMed1993

Simple and rapid method for the determination of the diastereomers of difenacoum in blood and liver using high-performance liquid chromatography with fluorescence detection.

A rapid and sensitive high-performance liquid chromatographic method for the analysis of cis and trans diastereomers of the anticoagulant rodenticide difenacoum has been described. The methodology demonstrates potential for the analysis of diastereomers of related 4-hydroxycoumarin anticoagulants. Separations were achieved by reversed-phase chromatography on a Zorbax ODS column with gradient elution using acetonitrile-water, modified with 0.1% acetic acid, as the mobile phase. Detection of the analytes was effected by fluorescence at excitation and emission wavelengths of 310 and 390 nm, respectively. Sample preparation from both plasma and liver has been simplified to reduce preparation time and manipulation. The minimum detectable concentration of each diastereomer was 5 ng/ml. Recoveries of 100% were obtained from plasma and 93% from liver tissue. This method has been used for the investigation of the pharmacokinetics of difenacoum diastereomers in rats, and for investigation of unexplained hypoprothrombinaemic events encountered clinically.

4-Hydroxycoumarins↗

PubMed1998

Solvent-free method for the determination of polynuclear aromatic hydrocarbons in waste water by solid-phase microextraction-high-performance liquid chromatography with photodiode-array detection.

Solid-phase microextraction (SPME) has rapidly been established among the practical alternatives for sample preparation for gas chromatography. Nevertheless polynuclear aromatic hydrocarbons (PAHs) are more effectively monitored by high-performance liquid chromatography (HPLC), but initially, there was no simple way to introduce analytes extracted by SPME into an HPLC system. A SPME-HPLC interface was developed by Supelco, which enables one to take advantages of the time and solvent savings offered by SPME. In the present work six PAHs from the European Union directives: fluoranthene, benzo[b]fluoranthene, benzo[k]fluoranthene benzo[a]pyrene, benzo[ghi]perylene, indeno[1,2,3-cd]pyrene were evaluated after optimization of a sample preparation method with a 100-micron poly(dimethylsiloxane) fiber. Repeatability, reproducibility, correlation coefficients, linearity, recoveries and limits of detection where determined and are indicated.

Chromatography, High Pressure Liquid↗

PubMedDate not supplied

Spectrofluorimetric determination of acetaminophen with N-bromosuccinimide.

A simple, sensitive, and selective method for determination of acetaminophen based on its oxidation using N-bromosuccinimide (NBS) to produce a highly fluorescent product. Optimization of reaction variables was carried out concerning NBS concentration, pH, temperature, reaction time, and stability time. Under optimal analytical conditions, the fluorescent intensity was measured at lambda emission. 442 nm (excitation at lambda 330 nm). The linearity range is 120-800 ng/mL with lower detection limit of 33.6 ng/mL acetaminophen. The method was applied successfully to the determination of the compound in pharmaceutical preparations, with average recovery of 100.3 +/- 2%. The method was also applied successfully to the determination of the drug in spiked plasma samples, with an average recovery of 101.2 +/- 1%. Interference effects of some compounds, present in combination with acetaminophen, were studied and the tolerance limits of these compounds were determined.

Acetaminophen↗

PubMed2004

Analysis of the Fusarium mycotoxins fusaproliferin and trichothecenes in grains using gas chromatography-mass spectrometry.

A method is described using gas chromatography-mass spectrometry (GC-MS) for the simultaneous detection of the Fusarium mycotoxins fusaproliferin and seven trichothecenes from grains. Sample purification of the raw extract was carried out with commercial solid phase extraction columns, and the recovery of the more polar analytes was increased by rinsing the column with acetonitrile. A significant matrix effect was found for the analysis of fusaproliferin and trichothecenes; thus, the calibrants should be prepared in a blank matrix. The response was linear in the range used. The mean recovery for fusaproliferin was 60.4 or 62.9%, depending on the spiking level. With respect to the trichothecenes, the recovery was generally higher (70.2-125.3%). The method proved to be repeatable for the analysis of fusaproliferin and trichothecenes. The limit of detection for fusaproliferin in the blank matrix mixture was 50 microg/kg, and that for trichothecenes was 5-15 microg/kg. Thirty-eight Finnish grain samples were analyzed for fusaproliferin and trichothecenes with the method developed. Fusaproliferin was not detected in any of the samples. The mean levels of deoxynivalenol, 3-acetyldeoxynivalenol, nivalenol, HT-2 toxin, and T-2 toxin in Finnish grain samples were 272, 17, 150, 40, and <20 microg/kg, respectively.

Edible Grain↗

PubMed1996

Simultaneous determination of coumarin, 7-hydroxycoumarin and 7-hydroxycoumarin glucuronide in human serum and plasma by high-performance liquid chromatography.

A HPLC method was developed for the determination of the metabolites of coumarin and 7-hydroxycoumarin in plasma and serum. Separation was based on gradient elution of 7-hydroxycoumarin glucuronide, 7-hydroxycoumarin, coumarin and finally 4-hydroxycoumarin (which is used as an internal standard). Standards, prepared in plasma or serum, and samples were treated with trichloroacetic acid, mixed and centrifuged. The supernatant was removed and analyzed by reversed-phase high-performance liquid chromatography on a C18 column. The limit of detection was 50 ng/ml for 7-hydroxycoumarin and 200 ng/ml for coumarin and 7-hydroxycoumarin glucuronide. The linear range was 0.5-100 micrograms/ml for each of the analytes. The percentage relative standard deviation about the mean measured concentrations were all below 10%. There was no statistical difference between the standard curves prepared in plasma or serum. The method developed was applied to the determination of each of the three compounds in serum, after the administration of 7-hydroxycoumarin, and in plasma after the administration of coumarin. The concentrations of total 7-hydroxycoumarin in the serum samples were also determined by another HPLC method and the results were compared. There was no statistical difference between the results determined.

Chromatography, High Pressure Liquid↗