Blood ether analysis

New Method for Blood Ether Analysis Fifth Annual Gas Chromatogr. Inst.,... 

The new lipid occurred only in the plasma hpids of newborns and was not present in membrane hpids of red cell membranes or platelets. Total lipids were extracted from plasma and from red blood cell membranes and platelets. A total lipid profile was obtained by a three-directional PLC using silica gel plates and was developed consecutively in the following solvent mixtures (1) chloroform-methanol-concen-trated ammonium hydroxide (65 25 5, v/v), (2) chloroform-acetone-methanol-ace-tic acid-water (50 20 10 15 5, v/v), and (3) hexane-diethyl ether-acetic acid (80 20 1, v/v). Each spot was scraped off the plate a known amount of methyl heptadecanoate was added, followed by methylation and analysis by GC/MS. The accmate characterization of the new lipid was realized using NMR technique. 

Calcium-selective electrodes have long been in use for the estimation of calcium concentrations - early applications included their use in complexometric titrations, especially of calcium in the presence of magnesium (42). Subsequently they have found use in a variety of systems, particularly for determining stability constants. Examples include determinations for ligands such as chloride, nitrate, acetate, and malonate (mal) (43), several diazacrown ethers (44,45), and methyl aldofuranosides (46). Other applications have included the estimation of Ca2+ levels in blood plasma (47) and in human hair (where the results compared satisfactorily with those from neutron activation analysis) (48). Ion-selective electrodes based on carboxylic polyether ionophores are mentioned in Section IV.B below. Though calcium-selective electrodes are convenient they are not particularly sensitive, and have slow response times. 

Dialysis units provided highly efficient means for increasing selectivity in a dynamic system by placement in front of a lithium-selective electrode constructed by incorporating 14-crown-4 ether 3-dodecyl-3 -methyl-1,5,8,12-tetraoxacyclotetradecane into a PVC membrane that was in turn positioned in a microconduit circuit by deposition on platinum, silver or copper wires. The circuit was used to analyse undiluted blood serum samples by flow injection analysis with the aid of an on-line coupled dialysis membrane. For this purpose, a volume of 200 pL of sample was injected into a de-ionized water carrier (donor) stream and a 7 mM tetraborate buffer of pH 9.2 was... 

Blood, urine and histopathological analysis of rats and beagle dogs exposed by inhalation to 6-73.5 mg/m phenyl glycidyl ether for three months did not reveal any treatment-related effect. This compound caused skin irritation and corneal injury in rabbits and hair loss in rats. Its sensitizing potential in guinea-pigs is low (lARC, 1989). 

Halogenated acyl derivatives of steroids have been applied in order to increase sensitivity of the analysis. It follows from a comparison of the ECD responses of haloacetates of steroids that the highest sensitivity can be obtained with the aid of monochloro-acetates [351]. Brownie et al. [352] applied them in the analysis of testosterone in blood. The method involves the extraction of blood plasma with diethyl ether, purification by TLC and derivatization. GC analysis is performed only after a preliminary separation on a thin layer. Preparation of the derivatives is carried out by treating a dried extract with... 

For the determination of papaverine in the blood of rats and dogs, Mussini and Harzo developed a method based on the extraction of the alkaloid with diethyl ether from 2 ml blood, after basification with sodium hydroxide, back extraction with hydrochloric acid and extraction with diethyl ether (after adjustment of the pH to 10). To the dried residue a solution of the internal standard (penfluridol) was added and the gas chromatographic analysis carried out on a packed column with 3 % OV-17 on Gas Chrom Q at 290°C, and a 83Ni electron-capture detector. The sensitivity of the method was 10 ng/ml blood. 

To omit unconventional instrumentation that was not suitable for routine analysis, as proposed by De Graeve et al.88, Bellia et al.81 developed a quite simple method to determine papaverine in blood samples, using conventional flame ionization or a nitrogen-phosphorus detector. The internal standard, strychnine, was added to the sample prior to extraction, which was carried out with toluene after basification, back extraction with acetic acid and extraction of the liberated base with diethyl ether. The gas chromatography was done on a packed column with 2 % 0V-101 at 275°C. To minimize the adsorption effects, the column was silanized by in situ injection and by injection of a concentrated solution of papaverine and the internal standard prior to routine analysis. Precision and accuracy of the method is shown in Table 14.13. 

The first reported method of analysis for halo-thane in blood was by turbidimetric measurement. Halo-thane was extracted from blood with petroleum ether. 

Control groups were fed commercial chow (Purina) or a complete diet prepared of purified components (8). The mineral mixture in this latter diet could be prepared without iron, copper or zinc so that these mineral elements could be added in controlled amounts as supplements in the form of ferrous sulfate, copper sulfate, or zinc carbonate. Under ether anesthesia, blood was removed from the abdominal aorta with a 1.5 inch, 22 gauge needle attached to a 10 ml syringe containing dried heparin. Aliquots were taken for hemoglobin, hematocrit, red cell counts and plasma analysis. The liver was removed, weighed, frozen and saved for analysis. 

A similar concept was used for other environmental applications, for example, phenoxy acids, sulfonureas, phenolic compounds, and other environmentally important persistent pollutants [68, 76, 141, 143, 155-166]. Also, in the same manner, several drugs were enriched and determined in body fluids such as urine [144-146, 167-172] or blood [147, 156, 157, 173, 174]. A very advanced apphcation of SLM for analytical purposes, where transport process was based on simple diffusion with pH adjustment of aqueous phase, is the extraction of the basic drug, bambuterol, for pretreatment of plasma samples before analysis with capfflary zone electrophoresis (CZE) [147]. Bambuterol was used as a model substance in a separation system, where either 6-undecanone or a mixture of di- -hexyl ether (DHE) and tri- -octylphosphine oxide (TOPO) was used as membrane phase. It was possible not only to achieve a very low hmit of detection ( 50 nmol/1) but also to ensure the removal of salts from the sample. It helped to obtain the low ionic strength of the blood plasma samples and permitted subsequent sample stacking in the caphlary electrophoresis step. 

In oases of death firom ether the odor is generally well marked in the clothing and surroundings, and especially on opening the thoracic cavity. In the analysis it is sought for in the blood and lungs at the same time as chloroform (q. v. j. 

Other solvents may be used instead of acetonitrile ether [74] or ether/heptane [75], and ethyl acetate is popular because of its good solvent x>wer for aromatic compounds. The following papers describe the analysis of drugs or metabolites from blood or cerebrospinal fluid, where the substance if first extracted, usually by a solvent extraction step, dried down and then derivatized [76-79]. 

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