The analysis of solutions of epinephrine and norepinephrine
01 Aug 1955-Journal of the American Pharmaceutical Association (Elsevier)-Vol. 44, Iss: 8, pp 507-514
TL;DR: In this article, a method of analysis is described which is applicable to solutions of epinephrine and norepinephrine, such as Epinephrine injection U.S. P. and levarterenol bitartrate injection N. N. R.
Abstract: A method of analysis is described which is applicable to solutions of epinephrine and norepinephrine, such as epinephrine injection U. S. P. and levarterenol bitartrate injection N. N. R. The method depends on the quantitative conversion of the substances into O3, O4, N‐triacetyl derivatives which may be extracted into chloroform, weighed, identified, and examined polarimetrically for the determination of stereo‐chemical composition. Excellent recoveries of the physiologically potent l‐isomer are obtained, and results of analyses of solutions of epinephrine show very good agreement with potencies determined by the U. S. P. XIV dog bioassay. By supplementing the method with partition chromatography of the acetylation product, the norepinephrine in a solution of U. S. P. epinephrine may be quantitatively isolated as its triacetyl derivative and determined colorimetrically after deacetylation and oxidation to noradrenochrome.
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TL;DR: A gas chromatographic method using electron capture detection is described for the estimation of those catecholamines and their metabolites which possess one or two free alcoholic hydroxyl groups and has been successfully applied to the detection and estimation of free 4‐hydroxy‐3‐methoxyphenylethylene glycol and free 3,4‐dihydroxyphenylthylene Glycol in hypothalamic brain tissue.
Abstract: 1. A gas chromatographic method using electron capture detection is described for the estimation of those catecholamines and their metabolites which possess one or two free alcoholic hydroxyl groups. It is based on acetylation of phenolic hydroxyl and primary and secondary amino groups in aqueous solution, extraction into a water immiscible solvent and esterification of alcoholic hydroxyl groups with heptafluorobutyric anhydride.2. The method has been successfully applied to the detection and estimation of free 4-hydroxy-3-methoxyphenylethylene glycol (MOPEG) and free 3,4-dihydroxyphenylethylene glycol (DOPEG) in hypothalamic brain tissue.3. Although it was possible to measure noradrenaline and normetanephrine by the same method in pure solution, crude tissue extracts could not be used, despite their suitability for estimating the glycol metabolites.
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TL;DR: In this article, the optimal conditions for the reaction of alkyl chloroformates with epinephrine and norepinephrine in aqueous solution have been evaluated.
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TL;DR: Mass spectral characterization of derivatized serotonin using electron and positive or negative chemical ionization indicates that electron ionization mass spectrometry is useful for serotonin assay in most biological fluids and tissues, but that electron capture negative chemical Ionization is required for samples containing less than 1-2 ng (cerebrospinal fluid).
Abstract: A gas chromatographic mass spectrometric assay for serotonin (5-hydroxytryptamine) has been developed. Serotonin is acylated in homogenized biological media, efficiently extracted into ethyl acetate, and further derivatized with pentafluoropropionic anhydride. Mass spectral characterization of derivatized serotonin using electron and positive or negative chemical ionization indicates that electron ionization mass spectrometry is useful for serotonin assay in most biological fluids and tissues, but that electron capture negative chemical ionization is required for samples containing less than 1-2 ng (cerebrospinal fluid). An assay limit of 10 pg per sample has been established. Examples of applications for the assay of serotonin in human platelets, rat spinal cord, and monkey cerebrospinal fluid are presented.
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TL;DR: The Pharmacopeia of the United States of AmericaFifteenth Revision, Fifth Revision is published.
Abstract: The Pharmacopeia of the United States of America Fifteenth Revision. (U.S.P. 15.) Pp. lii + 1178. (New York: United States Pharmacopeial Convention, Inc., 1955. Distributed by Mack Publishing Company, Easton, Pa.) 10 dollars.
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