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Biochemical investigations
ABSTRACTS
127
nique is greatly accelerated by simultaneous exposure of the system to a silent electrical discharge. Co” y-rays were far less useful for increasing tritium incorporation. &If-absorption correction (1959). A new correction sample is reported.
for carbon-14 R. W. Hendler, Science, 130, 772-77 factor that is linearly related to the thickness of the
Biochemical
Investigations
Dt,termination of ethanol in jingtirtip quantities of blood, L. A. Williams, R. A. Linn, and B. Zak, C2in. Chim. Acta, 3,169-72 (1958). A Conway cell for isothermal distribution containing CrzOi= is used for determination of 25-400 pg. EtOH. Crz07= is treated with Bmcine and read at 425 or 350 mp. Separation and preliminary characterization of oligowhycins A, B, and C, 8. Masamune, J. Am. Chem. Sot., 80,6092-95 ( 1958). Oligomycin complex (2-4 Mg.) is separated by paper chromatography into three components. Immunochemical studies on blood groups. XXI. Chromatographic examination of constituents split from blood group A, B, and O(H) substances and from type XIV pneumococcal polysaccharide by Clostridium tertium enzymes, G. Schiffman, C. Howe, and E. A. Kabat, J. Am. Chem. Sot.; 80,6662-70 (1958). Modifications of Whistler-Durso chromatographic and ParkJohnson procedures for reducing sugars for use with 2-10 pg. sugar are completely described. Qu.antitative determinations of free lysine in urine by two-dimensional paper chromu,tographs, L. F. Kerley, J. Lab. Clin. Med., 53, 149-55 (1959). Quantitative determination of free lysine in urine by an Eel scanner on two-dimensional paper chromatograms is described. The standard is run on the same paper. An improvement of the method jar determination of plasma and urine hemoglobin, T. R. Johnson, J. Lab. Clin. Med., 53,49598 (1959). A modification of the Dacie pipet is described for the measurement of small volumes of plasma or urine permitting the use of the benxidine method for microhemoglobinometry without preliminary dilution. A micromethod for serum iron determinations, W. Woodruff, J. Lab. Clin. Med., 53, 95!&57 (1959). A micromodification of Ramsey’s method is described. Standard deviations of variation between duplicates is 3.8 pg./100 ml. A .simplijied method for the deferminations of citric acid, E. Beutler and M. K. Y. Yeh, J. Lab. Clin. Med., 54, 125-31 (1959). Citric acid is converted to pentabromoacetone and a color developed with a thiourea-borax reagent. Quantities det,ermined lie between 10 and 2000 pg.
128
ABSTRACTS
A microcolorimetric method for the determination of sorbitol, mannitol, and glycerol in biologicjluids, J. M. Bailey, J. Lab. Clin. Med., 54,158-62 (1959). A micromethod for sorbitol, mannitol, and glycerol involves periodate oxidations followed by colorimetric determination of the HCHO formed. The method is applicable to 5-50 pg. material. Glucose and other blood serum components do not interfere. The determination of copper in blood serum with lead diethyldithiocarbamate, I. Dezsii and T. Fiilijp, Mikrochim. Acta, 1959, 592-95. As little as 0.3 pg./ml. Cu may be determined, and iron as well as the other cations present in serum do not interfere. Paper chromatography of small amounts of vasopressins and oxytocins, H. Heller and K. Lederis, Nature, 182,1231-32 (1958). A method is described for preparation of 0.7 pg. or more arginine-vasopressin or 0.02 pg. or more oxytocin. DetectimL of hemoglobin, ha?moglobin-haptogloin complexes and other substances with peroxidase aetiv-ity after zone electrophoresis, J. A. Owen, H. J. Silberman, and C. Got, Nature, 182,1373 (1958). o-Dianisidine reagent has been found accurate A description is given of the for as little as 5 X lOA pg./cm.* of hemoglobin. preparation and use on the electrophoretic strips. Rapid specific method for the determination of aldosaccharides in body jluio?s, E. Hultman, Nature, 183,108-109 (1959). Glucose (10-400 pg.) in blood or urine is determined calorimetrically by reaction with o-toluidine. A rapid m&o-quantitative method for estimating serum calcium, T. A Harper, Nature, 183,232-33 (1959). Microgram quantities of calcium are estimated by treatment mrith alkaline murexide-ammonium purpurate in a spectrophotometric method to accuracy within f 1%. Micro-volume drop-plate assay of antibiotics, M. R. S. Iyengar, Nature, 183, 684 (1959). Spotting 0.4-1.6 ~1. quantities of antibiotic solutions directly on the assay plate by a microsyringe gives an assay with error in the range of the conventional cup-plate assay method. A source of error in microbiological assays attributable io a bacterial inhibitor in distilled water, S. A. Price and L. Gare, Nature, 183,838-40 (1959). Proper cleaning procedures eliminate difficulties in folic acid assays involving use of Streptococcus aecalis R. Identification of barbiturates, A. S. Curry, Nature, 183, 1052 (1959). A reliable spectrophotomet.ric method for total barbiturate concentration in 5-10 ml. blood is detailed. Direct determination of drug concentrations in biological fuids by polarography, P. 0. Kane, Nature, 183,1674 (1959). 2-Ethyl-Pthiocarbamidopyridine (1314 TH) MICROCHEMICAL
JOURNAL,
VOL.
IV,
ISSUE
1
ABSTRACTS in small concentrations (0.1-5.0 pg./ml.) can be determined directly raphy since this compound has a well-defined polarographic wave.
129 by polarog-
Structure of melanocyte-stimulating hormone from the human pituitary gland, J. I. Harris, Nuture, 184,167-69 (1959). A description of the procedures used in identification of amino acids and polypeptides in 4-5-mg. samples is given. Determination of magnesium in blood serum by atomic absorption spectroscopy, J. B. Willis, Nature, 184, 186-87 (1959). Magnesium in serum can be determined directly by use of the atomic absorption method without ashing and dilution with wa,ter containing 1% d&odium salt of ethylenediamine tetraacetic acid. Estimation of microgram quantities of iron in culture medium, using bathophenanthroline, P. A. Seamer, Nature, 184, 636-37 (1959). A detailed description is given of a calorimetric method suitable for determining 2-3 pg. iron with an accuracy within f1.5%. Microbiological determination of antibiotics in the Swiss Pharmawpia, M. Vuilleumier and L. Anker, Pharm. Acta Helv., 33,621-33 (1958). A general method for the microbiological assay of antibiotics based upon the use of Sarcina lutea is described. Ra:pid micromethod for the evaluation of alkaline serum phosphatases, P. Kesselman, Rev. asoc. btiguim. arg., 23,9&94 (1958). A standardized procedure is proposed for the determination of both alkaline and acidic serum phosphatases. Micromethod for determination of blood galadose by means of glucose oxidase (notatin) and anthrone, G. Spdergaard, &and. J. Clin. & Lab. Invest., 10, 203-10 (1958). Notatin removes glucose, Ba(OH)2-ZnS04 removes proteins, and the remaining galactose is determined calorimetrically with anthrone. Inhibition of enzymatic synthesis of pantothenate by 2,3-dichloro-isobutyrate, J. L. Hilton, Science, 128,1509-10 (1959). Inhibition of enzymatic synthesis of pantothenate is followed by measuring the rate of CO, liberation from bicarbonate buffer at pH 8 and 30” and is carried out in Warburg vessels containing a 5% CO2 atmosphere. Measurement of precipitin reactions in the millimicrogram protein-nitrogen range, D. Click, Stience, 128,162s26 (1958). Interaction of 10 ~1. antigen solution and 10 ~1. antiserum gives over 1 ml. solution for spectrophotometric determination of protein-nitrogen. Four dyes are compared for dye-binding of the protein. Analysis of gas in biological fluids by gas chromatography, L. H. Ramsey, Science, 129,90&901 (1959). A combination of vacuum extraction and gas ehromatography allows reproducible determinations of small quantities of permanent gases in biological fluids. Demonstration is given of oxygen tension in 1 ml. human plasma.
130
ABSTRACTS
Isotope dilution method for assay of inayylutinable erythrocytes, K. C. Atwood and S. L. Scheinberg, Science, 129,963-64 (1959). The true inagglutinable proportion of cells can be found by successive agglutinat,ions of a labeled population in the presence of unlabeled carrier cells. Free p-hydroxy-r-aminobutyric acid in brain, K. Ohara, Science, 129, 1225-26 (1959). @Hydroxy-r-aminobutyric acid was shown to exist in the brain of mice, rabbits, cattle, and humans by comparing the patterns obtained in paper chromatography and high-potential paper electrophoreeis of prepared extracts with those obtained with synthetic acid. Use of phosphorus-32 in microassay for nucleic acid synthesis in Escherichia coli, P. Hanawalt, Science, 130, 386-U (1959). A rapid means of determining less than 1 pg. ribonucleic acid and deoxyribonucleic acid in bacterial cultures is described. A modified Schmidt-Thannhauser procedure is applied to microquantities of Pa2 labeled cells collected on a membrane. Identi$cation Hendershott flavanone is point, paper
of a growth inhibitor from extracts of dornkant peach$ower buds, C. H. and D. R. Walker, Science, 130,798-99 (1959). 5,7,4’-Trihydroxyisolated and identified by infrared and ultraviolet spectra, melting chromatography, and activity in the bioassay test.
A nkicrowlorimetric method for the determination of antimony in biological material, C.-K. Ho, C.-C. Kung, S.-y. Wang, and L. Li, Sheng Li Hsueh Pao, 21, 167-73 (1957). The sample is digested, later extracted and red color formed with Rhodamine B is measured spectrophotometrically.
Inorganic Microsynthesis Diphenylacetylene derivatives of iron carbonyl, G. N. Schrauzer, J. Am. Chem. Sot., 81, 5307-10 (1959). The conversion of 72-100 mg. iron carbonyl complexes by thermal decomposition and by base is described. Substituted carbonyl compounds of chromium, molybdenum, tungsten, and mangarzese, E. W. Abel, M. A. Bennett, and G. Wilkinson, J. Chem. Sot., 1959, 232327. Complexes of the type L,M(CO)I, where M is (Cr, MO, W), and L represents various N, P, As, and Sb donor compounds have been synthesized in decigram quantities. Phosphine complexes of di- and trivalent chromium, K. Isslieb and H. 0. FrShlich, 2. anorg. u. allgem. Chem., 298, 84-99 (1959). Preparation of CrC& [P(C&H&]2 from 300 mg. CrCl* and 300 mg. P(C2H& in anhydrous benzene is described. (See specifically p. 98). On the action of halogenates on vanadium(IZZ) oxide in aqueous solution, T. Kuusinen, 2. anorg. u. &gem. Chem., 298,194-201(1959). Investigation of theprodMlCROCHEMICAL
JOURNAL,
VOL.
IV,
ISSUE
1
127
nique is greatly accelerated by simultaneous exposure of the system to a silent electrical discharge. Co” y-rays were far less useful for increasing tritium incorporation. &If-absorption correction (1959). A new correction sample is reported.
for carbon-14 R. W. Hendler, Science, 130, 772-77 factor that is linearly related to the thickness of the
Biochemical
Investigations
Dt,termination of ethanol in jingtirtip quantities of blood, L. A. Williams, R. A. Linn, and B. Zak, C2in. Chim. Acta, 3,169-72 (1958). A Conway cell for isothermal distribution containing CrzOi= is used for determination of 25-400 pg. EtOH. Crz07= is treated with Bmcine and read at 425 or 350 mp. Separation and preliminary characterization of oligowhycins A, B, and C, 8. Masamune, J. Am. Chem. Sot., 80,6092-95 ( 1958). Oligomycin complex (2-4 Mg.) is separated by paper chromatography into three components. Immunochemical studies on blood groups. XXI. Chromatographic examination of constituents split from blood group A, B, and O(H) substances and from type XIV pneumococcal polysaccharide by Clostridium tertium enzymes, G. Schiffman, C. Howe, and E. A. Kabat, J. Am. Chem. Sot.; 80,6662-70 (1958). Modifications of Whistler-Durso chromatographic and ParkJohnson procedures for reducing sugars for use with 2-10 pg. sugar are completely described. Qu.antitative determinations of free lysine in urine by two-dimensional paper chromu,tographs, L. F. Kerley, J. Lab. Clin. Med., 53, 149-55 (1959). Quantitative determination of free lysine in urine by an Eel scanner on two-dimensional paper chromatograms is described. The standard is run on the same paper. An improvement of the method jar determination of plasma and urine hemoglobin, T. R. Johnson, J. Lab. Clin. Med., 53,49598 (1959). A modification of the Dacie pipet is described for the measurement of small volumes of plasma or urine permitting the use of the benxidine method for microhemoglobinometry without preliminary dilution. A micromethod for serum iron determinations, W. Woodruff, J. Lab. Clin. Med., 53, 95!&57 (1959). A micromodification of Ramsey’s method is described. Standard deviations of variation between duplicates is 3.8 pg./100 ml. A .simplijied method for the deferminations of citric acid, E. Beutler and M. K. Y. Yeh, J. Lab. Clin. Med., 54, 125-31 (1959). Citric acid is converted to pentabromoacetone and a color developed with a thiourea-borax reagent. Quantities det,ermined lie between 10 and 2000 pg.
128
ABSTRACTS
A microcolorimetric method for the determination of sorbitol, mannitol, and glycerol in biologicjluids, J. M. Bailey, J. Lab. Clin. Med., 54,158-62 (1959). A micromethod for sorbitol, mannitol, and glycerol involves periodate oxidations followed by colorimetric determination of the HCHO formed. The method is applicable to 5-50 pg. material. Glucose and other blood serum components do not interfere. The determination of copper in blood serum with lead diethyldithiocarbamate, I. Dezsii and T. Fiilijp, Mikrochim. Acta, 1959, 592-95. As little as 0.3 pg./ml. Cu may be determined, and iron as well as the other cations present in serum do not interfere. Paper chromatography of small amounts of vasopressins and oxytocins, H. Heller and K. Lederis, Nature, 182,1231-32 (1958). A method is described for preparation of 0.7 pg. or more arginine-vasopressin or 0.02 pg. or more oxytocin. DetectimL of hemoglobin, ha?moglobin-haptogloin complexes and other substances with peroxidase aetiv-ity after zone electrophoresis, J. A. Owen, H. J. Silberman, and C. Got, Nature, 182,1373 (1958). o-Dianisidine reagent has been found accurate A description is given of the for as little as 5 X lOA pg./cm.* of hemoglobin. preparation and use on the electrophoretic strips. Rapid specific method for the determination of aldosaccharides in body jluio?s, E. Hultman, Nature, 183,108-109 (1959). Glucose (10-400 pg.) in blood or urine is determined calorimetrically by reaction with o-toluidine. A rapid m&o-quantitative method for estimating serum calcium, T. A Harper, Nature, 183,232-33 (1959). Microgram quantities of calcium are estimated by treatment mrith alkaline murexide-ammonium purpurate in a spectrophotometric method to accuracy within f 1%. Micro-volume drop-plate assay of antibiotics, M. R. S. Iyengar, Nature, 183, 684 (1959). Spotting 0.4-1.6 ~1. quantities of antibiotic solutions directly on the assay plate by a microsyringe gives an assay with error in the range of the conventional cup-plate assay method. A source of error in microbiological assays attributable io a bacterial inhibitor in distilled water, S. A. Price and L. Gare, Nature, 183,838-40 (1959). Proper cleaning procedures eliminate difficulties in folic acid assays involving use of Streptococcus aecalis R. Identification of barbiturates, A. S. Curry, Nature, 183, 1052 (1959). A reliable spectrophotomet.ric method for total barbiturate concentration in 5-10 ml. blood is detailed. Direct determination of drug concentrations in biological fuids by polarography, P. 0. Kane, Nature, 183,1674 (1959). 2-Ethyl-Pthiocarbamidopyridine (1314 TH) MICROCHEMICAL
JOURNAL,
VOL.
IV,
ISSUE
1
ABSTRACTS in small concentrations (0.1-5.0 pg./ml.) can be determined directly raphy since this compound has a well-defined polarographic wave.
129 by polarog-
Structure of melanocyte-stimulating hormone from the human pituitary gland, J. I. Harris, Nuture, 184,167-69 (1959). A description of the procedures used in identification of amino acids and polypeptides in 4-5-mg. samples is given. Determination of magnesium in blood serum by atomic absorption spectroscopy, J. B. Willis, Nature, 184, 186-87 (1959). Magnesium in serum can be determined directly by use of the atomic absorption method without ashing and dilution with wa,ter containing 1% d&odium salt of ethylenediamine tetraacetic acid. Estimation of microgram quantities of iron in culture medium, using bathophenanthroline, P. A. Seamer, Nature, 184, 636-37 (1959). A detailed description is given of a calorimetric method suitable for determining 2-3 pg. iron with an accuracy within f1.5%. Microbiological determination of antibiotics in the Swiss Pharmawpia, M. Vuilleumier and L. Anker, Pharm. Acta Helv., 33,621-33 (1958). A general method for the microbiological assay of antibiotics based upon the use of Sarcina lutea is described. Ra:pid micromethod for the evaluation of alkaline serum phosphatases, P. Kesselman, Rev. asoc. btiguim. arg., 23,9&94 (1958). A standardized procedure is proposed for the determination of both alkaline and acidic serum phosphatases. Micromethod for determination of blood galadose by means of glucose oxidase (notatin) and anthrone, G. Spdergaard, &and. J. Clin. & Lab. Invest., 10, 203-10 (1958). Notatin removes glucose, Ba(OH)2-ZnS04 removes proteins, and the remaining galactose is determined calorimetrically with anthrone. Inhibition of enzymatic synthesis of pantothenate by 2,3-dichloro-isobutyrate, J. L. Hilton, Science, 128,1509-10 (1959). Inhibition of enzymatic synthesis of pantothenate is followed by measuring the rate of CO, liberation from bicarbonate buffer at pH 8 and 30” and is carried out in Warburg vessels containing a 5% CO2 atmosphere. Measurement of precipitin reactions in the millimicrogram protein-nitrogen range, D. Click, Stience, 128,162s26 (1958). Interaction of 10 ~1. antigen solution and 10 ~1. antiserum gives over 1 ml. solution for spectrophotometric determination of protein-nitrogen. Four dyes are compared for dye-binding of the protein. Analysis of gas in biological fluids by gas chromatography, L. H. Ramsey, Science, 129,90&901 (1959). A combination of vacuum extraction and gas ehromatography allows reproducible determinations of small quantities of permanent gases in biological fluids. Demonstration is given of oxygen tension in 1 ml. human plasma.
130
ABSTRACTS
Isotope dilution method for assay of inayylutinable erythrocytes, K. C. Atwood and S. L. Scheinberg, Science, 129,963-64 (1959). The true inagglutinable proportion of cells can be found by successive agglutinat,ions of a labeled population in the presence of unlabeled carrier cells. Free p-hydroxy-r-aminobutyric acid in brain, K. Ohara, Science, 129, 1225-26 (1959). @Hydroxy-r-aminobutyric acid was shown to exist in the brain of mice, rabbits, cattle, and humans by comparing the patterns obtained in paper chromatography and high-potential paper electrophoreeis of prepared extracts with those obtained with synthetic acid. Use of phosphorus-32 in microassay for nucleic acid synthesis in Escherichia coli, P. Hanawalt, Science, 130, 386-U (1959). A rapid means of determining less than 1 pg. ribonucleic acid and deoxyribonucleic acid in bacterial cultures is described. A modified Schmidt-Thannhauser procedure is applied to microquantities of Pa2 labeled cells collected on a membrane. Identi$cation Hendershott flavanone is point, paper
of a growth inhibitor from extracts of dornkant peach$ower buds, C. H. and D. R. Walker, Science, 130,798-99 (1959). 5,7,4’-Trihydroxyisolated and identified by infrared and ultraviolet spectra, melting chromatography, and activity in the bioassay test.
A nkicrowlorimetric method for the determination of antimony in biological material, C.-K. Ho, C.-C. Kung, S.-y. Wang, and L. Li, Sheng Li Hsueh Pao, 21, 167-73 (1957). The sample is digested, later extracted and red color formed with Rhodamine B is measured spectrophotometrically.
Inorganic Microsynthesis Diphenylacetylene derivatives of iron carbonyl, G. N. Schrauzer, J. Am. Chem. Sot., 81, 5307-10 (1959). The conversion of 72-100 mg. iron carbonyl complexes by thermal decomposition and by base is described. Substituted carbonyl compounds of chromium, molybdenum, tungsten, and mangarzese, E. W. Abel, M. A. Bennett, and G. Wilkinson, J. Chem. Sot., 1959, 232327. Complexes of the type L,M(CO)I, where M is (Cr, MO, W), and L represents various N, P, As, and Sb donor compounds have been synthesized in decigram quantities. Phosphine complexes of di- and trivalent chromium, K. Isslieb and H. 0. FrShlich, 2. anorg. u. allgem. Chem., 298, 84-99 (1959). Preparation of CrC& [P(C&H&]2 from 300 mg. CrCl* and 300 mg. P(C2H& in anhydrous benzene is described. (See specifically p. 98). On the action of halogenates on vanadium(IZZ) oxide in aqueous solution, T. Kuusinen, 2. anorg. u. &gem. Chem., 298,194-201(1959). Investigation of theprodMlCROCHEMICAL
JOURNAL,
VOL.
IV,
ISSUE
1