Determination of Chlorinated Pesticides in Whole Blood

1973 ◽  
Vol 56 (5) ◽  
pp. 1173-1177
Author(s):  
Paula E Stretz ◽  
Henry M Stahr
Keyword(s):  
Sulfuric Acid ◽  
Whole Blood ◽  
Gas Liquid Chromatography ◽  
Chlorinated Pesticides ◽  
Blood Samples ◽  
Mean Values ◽  
Sulfuric Acid Method ◽  
Large Systematic Error ◽  
Good Agreement

Abstract Eight whole blood samples spiked with lindane, dieldrin, and p,p′-DDT at levels of 2.5, 12.6, 126, and 630 ppb each were sent to 11 collaborators for analysis. The method evaluated uses sulfuric acid to liberate the pesticides from the blood matrix. The pesticides are then extracted with 10% acetone in hexane. Pesticides were identified and quantitatively analyzed by gas-liquid chromatography, using an electron capture detector. Mean values at all levels are in good agreement with the spiking levels. However, statistical analysis of the data reveals a large systematic error. Further evaluation of the sulfuric acid method by comparison with other methods is recommended.

Microcoulometric Determination of Organochlorine Pesticides in Human Blood

1974 ◽  
Vol 57 (3) ◽  
pp. 595-603
Author(s):  
Francis D Griffith ◽  
Robert V Blanke
Keyword(s):  
Sulfuric Acid ◽  
Human Blood ◽  
Retention Time ◽  
Whole Blood ◽  
Industrial Chemicals ◽  
Chlorinated Pesticides ◽  
Human Whole Blood ◽  
Sulfuric Acid Method ◽  
Made In

Abstract Improvements in the microcoulometric halogen system allow analysis of as little as 1 ppb chlorinated pesticides with specificity and linearity. Modifications were made in the sulfuric acid method of extracting pesticides from human whole blood to obtain recovery of 24 pesticides and 7 industrial chemicals. Recovery data were tabulated. Retention time and response tables for OV-210 and SE-30/QF-1 columns were prepared for these compounds, using the microcoulometric detector.

scholarly journals Determination of 19 Psychoactive Substances in Premortem and Postmortem Whole Blood Samples Using Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry

Separations ◽  
2021 ◽  
Vol 8 (6) ◽  
pp. 78
Author(s):  
Sevasti Karampela ◽  
Jessica Smith ◽  
Irene Panderi
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Formic Acid ◽  
Whole Blood ◽  
High Performance ◽  
Tandem Mass ◽  
Psychoactive Substances ◽  
Blood Samples ◽  
Whole Blood Samples

An ever-increasing need exists within the forensic laboratories to develop analytical processes for the qualitative and quantitative determination of a broad spectrum of new psychoactive substances. Phenylethylamine derivatives are among the major classes of psychoactive substances available on the global market and include both amphetamine analogues and synthetic cathinones. In this work, an ultra-high-performance liquid chromatography-positive ion electrospray ionization tandem mass spectrometric method (UHPLC-ESI-MS/MS) has been developed and fully validated for the determination of 19 psychoactive substances, including nine amphetamine-type stimulants and 10 synthetic cathinone derivatives, in premortem and postmortem whole blood. The assay was based on the use of 1 mL premortem or postmortem whole blood, following solid phase extraction prior to the analysis. The separation was achieved on a Poroshell 120 EC-C18 analytical column with a gradient mobile phase of 0.1% formic acid in acetonitrile and 0.1% formic acid in water in 9 min. The dynamic multiple reaction monitoring used in this work allowed for limit of detection (LOD) and lower limit of quantitation (LOQ) values of 0.5 and 2 ng mL−1, respectively, for all analytes both in premortem and postmortem whole blood samples. A quadratic calibration model was used for the 12 quantitative analytes over the concentration range of 20–2000 ng mL−1, and the method was shown to be precise and accurate both in premortem and postmortem whole blood. The method was applied to the analysis of real cases and proved to be a valuable tool in forensic and clinical toxicology.

scholarly journals Simultaneous Determination of Cyclosporine A, Tacrolimus, Sirolimus, and Everolimus in Whole-Blood Samples by LC-MS/MS

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Mustafa Karapirli ◽  
Murat Kizilgun ◽  
Ozgur Yesilyurt ◽  
Husamettin Gul ◽  
Zeki Ilker Kunak ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Tandem Mass Spectrometry ◽  
Simultaneous Determination ◽  
Cyclosporine A ◽  
Whole Blood ◽  
Immunosuppressive Drugs ◽  
Tandem Mass ◽  
Blood Samples ◽  
Whole Blood Samples

Objectives. Cyclosporine A (CyA), tacrolimus (TRL), sirolimus (SIR), and everolimus (RAD) are immunosuppressive drugs frequently used in organ transplantation. Our aim was to confirm a robust sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determination of CyA, TRL, SIR, and RAD in whole-blood samples.Materials and Methods. We used an integrated online solid-phase extraction-LC-MS/MS system and atmospheric pressure ionization tandem mass spectrometry (API-MS/MS) in the multiple reaction monitoring (MRM) detection mode. CyA, TRL, SIR, and RAD were simultaneously analyzed in whole blood treated with precipitation reagent taken from transplant patients.Results. System performance parameters were suitable for using this method as a high-throughput technique in clinical practice. The high concentration of one analyte in the sample did not affect the concentration of other analytes. Total analytical time was 2.5 min, and retention times of all analytes were shorter than 2 minutes.Conclusion. This LC-MS/MS method can be preferable for therapeutic drug monitoring of these immunosuppressive drugs (CyA, TRL, SRL, and RAD) in whole blood. Sample preparation was too short and simple in this method, and it permits robust, rapid, sensitive, selective, and simultaneous determination of these drugs.

Development and validation of a dried blood spot–HPLC assay for the determination of metronidazole in neonatal whole blood samples

2010 ◽  
Vol 397 (2) ◽  
pp. 687-693 ◽  
Author(s):  
Maysa Faisal Suyagh ◽  
Godwill Iheagwaram ◽  
Prashant Laxman Kole ◽  
Jeff Millership ◽  
Paul Collier ◽  
...  
Keyword(s):  
Whole Blood ◽  
Dried Blood Spot ◽  
Hplc Assay ◽  
Blood Samples ◽  
Whole Blood Samples ◽  
Development And Validation ◽  
Blood Spot

Modified Automated Determination of 2,3-Diphosphoglycerate in Whole Blood

1972 ◽  
Vol 18 (9) ◽  
pp. 1001-1004 ◽  
Author(s):  
Kenneth F Atkinson
Keyword(s):  
Sample Size ◽  
Coefficient Of Variation ◽  
Whole Blood ◽  
Normal Range ◽  
Blood Samples ◽  
Automated Determination

Abstract A modification is described of the automated determination of 2,3-diphosphoglycerate (DPG) in blood [Grisolia, S., et al., Anal. Biochem. 31, 235 (1969)]. Modifications in the manifold result in a sensitive, noise-free, rapid system and the modifications in the preparations of the reagents ensure stability of the diluted standards and blood samples for at least three weeks. Samples are run at the rate of 60/h and sample size can be as small as 5 µl of whole blood. The coefficient of variation of the overall determination of automated DPG and manual hemoglobin is 3.6% and the SD is ±0.77 µmol/g Hb. The normal range is 14.6 ± 2.2 (SD) µmol/g hemoglobin.

X-Ray Spectroscopy in the Clinical Laboratory

1961 ◽  
Vol 7 (2) ◽  
pp. 115-129 ◽  
Author(s):  
Samuel Natelson ◽  
Bertrum Sheid
Keyword(s):  
Total Phosphorus ◽  
Whole Blood ◽  
Phosphorus Content ◽  
Clinical Laboratory ◽  
Total Iron ◽  
Mean Values ◽  
X Ray ◽  
Significant Difference ◽  
Wet Ashing

Abstract X-ray spectroscopy was applied to the determination of the total phosphorus content of serum and the iron content of whole blood (hemoglobin). Samples were placed on confined spots on paper, dried, then passed through the X-ray field. Concentration was then determined from the peaks as drawn on a recorder. A device is described that permits automatic assay of successive samples dried on paper without delays between readings. Samples are placed in the field and rapidly withdrawn at 30-sec. intervals, the response of the recorder serving as a measure of concentration. Results for total phosphorus in serum and total iron in whole blood were compared with those obtained by a wet ashing procedure. No significant difference with respect to both mean values and precision was observed except that total iron by the wet ashing procedure was more precise. However, the X-ray technic was adequate for clinical purposes. Hemoglobin levels calculated from whole-blood iron values demonstrated that bilirubin, red cell debris, leukocytes, and lipids interfered in the colorimetric but not in the X-ray procedure. A hemoglobinometer based on the X-ray spectroscopic technic may, therefore, yield results of greater clinical significance.

scholarly journals Detection of hepatitis B surface antigen in whole blood by coupled particle light scattering (Copalis™)

1997 ◽  
Vol 43 (9) ◽  
pp. 1764-1770 ◽  
Author(s):  
Michael J Benecky ◽  
Diane R Post ◽  
Susan M Schmitt ◽  
Manish S Kochar
Keyword(s):  
Hepatitis B ◽  
Surface Antigen ◽  
Whole Blood ◽  
Direct Detection ◽  
Hepatitis B Surface Antigen ◽  
Light Scatter ◽  
Blood Samples ◽  
Cell Components ◽  
Multiple Analytes

Abstract Coupled particlelight scattering (Copalis™) is a homogeneous immunoassay technology that permits simultaneous determination of multiple analytes in serum, plasma, or whole blood. Copalis differentiates monomeric latex microparticles from latex aggregates and cells on the basis of their unique light scatter properties. Copalis readily discriminates small (∼0.1 μm) differences in latex microparticle size. Therefore, multiple simultaneous assays are configured by the use of mixtures of different-size latex microparticles. The Copalis research immunoassay for hepatitis B surface antigen (HBsAg) is configured in a sandwich format where the extent of light scatter histogram broadening due to HBsAg-mediated binding of colloidal gold to latex provides the basis for antigen quantification. Simultaneous Copalis forward- and wide-angle light scatter measurements allow discrimination of latex microparticles from the cell components of whole blood. Consequently, direct detection of HBsAg in unprocessed whole-blood samples by Copalis is feasible.

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