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One hundred sixty-six isolates of Fusarium spp. from domestic cereal grains, feed, and other sources were examined for their ability to produce zearalenone on autoclaved moist rice grains. They belonged to the following species (number of producers/number tested): F. roseum (9/28), F. roseum (Culmorum) (3/4), F. roseum (Gibbosum) (2/5), F. roseum (Avenaceum) (1/2), F. roseum (Scirpi) (0/1), F. tricinctum (1/4), F. tricinctum (Sporotrichiella) (0/7), F. lateritium (1/1), F. episphaeria (0/2), F. moniliforme (0/3), F. oxysporum (0/12), F. rigidiusculum (0/4), F. solani (0/4), F. splendens (0/1), F. nivale (0/2), and Fusarium spp. (15/86). Zearalenone was isolated from molded rice by ethanol extraction and purified by column chromatography. Selected isolates of F. roseum M-3-2 and F. roseum (Gibbosum) A-O-2 produced 50 to 100 mg of zearalenone per kg of rice. Increased yields (250 to 407 mg/kg of rice) were obtained by F. roseum M-3-2 when the substrate was supplemented with 1% peptone.

The 1H–2H exchange in 2H2O solutions, at 25 °C, of the basic pancreatic trypsin inhibitor and of insulin has been studied by infrared and proton magnetic resonance spectroscopy. Under identical conditions of pH the exchange in the peptide groups of the inhibitor is considerably slower than the exchange in the peptide groups of insulin, indicating that the interior regions of the inhibitor molecules are less accessible to the solvent than those of the insulin molecules. The experimental results are expressed in terms of the probabilities of local conformational changes of the proteins, by which the peptide groups are exposed to the solvent, and in terms of the corresponding changes in standard free energy. The data is taken as an illustration of the range of distributions of values of these parameters, typical of globular proteins.

A nonaxenic sewage culture metabolized 1,1-diphenylethylene by two different pathways involving hydration to form 2,2-diphenylethanol and oxidation and fission of one of the benzene rings to form atropic acid. Five different bacterial strains which grew on 1,1-diphenylethylene were isolated; all were gram-negative rods comprising the genera Pseudomonas, Acetomonas, and Acinetobacter. A fungal isolate, Cladosporium, which used diphenylethylene as a sole carbon source, was also obtained from the same enrichment procedure.

A method is described for the synthesis of labeled ethidium (3,8-diamino-5-ethyl-6-phenyl phenanthridinium) bromide. Based on benzoic acid, the radioactive precursor used, the yield is 15% of a compound that is indistinguishable from authentic ethidium bromide in its absorption spectra (uv, visible, ir), Chromatographie behavior, and mutagenic effectiveness in the induction of respiration-deficient cell lines in baker's yeast.

When Pseudomonas C12B is grown on nutrient broth to the stationary phase, cell extracts contain two secondary alkylsulphatases (S1 and S2) active towards potassium decan-5-yl sulphate but not towards potassium pentan-3-yl sulphate and one primary alkylsulphatase (P1) active towards sodium dodecan-1-yl sulphate (sodium dodecyl sulphate). When 10mm-sodium hexan-1-yl sulphate is included in the nutrient broth an additional primary alkylsulphatase (P2) is produced. The S1, S2, P1 and P2 enzymes are also present in extracts of cells grown on broth containing the commercial detergent Oronite, together with an additional secondary alkylsulphatase (S3) active towards pentan-3-yl sulphate as well as decan-5-yl sulphate. The P2 primary alkylsulphatase can be induced by a number of primary and secondary alkyl sulphate esters but the induction of the S3 enzyme appears to be a more specific and complex process. Studies on the ability of different fractions separated from Oronite to act as inducers suggest that the combination of a long-chain secondary alkyl sulphate(s) and a long-chain secondary alcohol(s) is responsible for the appearance of the S3 enzyme. Potassium hexadecan-2-yl sulphate or potassium tetradecan-2-yl sulphate, in combination with either hexadecan-2-ol or tetradecan-2-ol, can serve as inducers for the enzyme. Some characteristics of these specific inducer systems have been elucidated.

The isolation, purification, and identification of di-(1-phenylisopropyl)methylamine, present in illicit samples of methamphetamine, are described. The identity of the substance was confirmed by synthesis. It is commonly present in amounts ranging between 3 and 15% relative to methamphetamine.

The glycosaminoglycans of root dentine from permanent human teeth were studied. The tissue was digested with papain and the glycosaminoglycans were precipitated with cetylpyridinium chloride and recovered by centrifugation. A small quantity of keratan sulphate was recovered from the supernatant after fractionation on cetylpyridinium chloride and Ecteola-cellulose. The cetylpyridinium chloride-precipitated glycosaminoglycans were studied by infra-red spectrophotometry, cetylpyridinium chloride cellulose chromatography and electrophoresis on cellulose acetate. Individual hexosamines were determined on an autoanalyzer. The results indicate that chondroitin-4-sulphate is the major glycosaminoglycan and that chondroitin-6-sulphate, hyaluronic acid, dermatan sulphate and a nonsulphated galactosaminoglycan are also present in minor quantities.

In this study an endotoxic substance was extracted from the cells ofCryptococcus neoformans and the physicochemical and biological properties of this substance (Cr-ET) were investigated. In comparison with endotoxin of gram-negative bacteria, the lethality of Cr-ET for mice and chick embryos was low and such biological activities were weak as the pyrogenic effect on rabbits and effects on the leucocyte count and blood sugar level in rabbits. Skin reactions (both primary and Shwartzman reactions) were elicited in rabbits by relatively large dose of Cr-ET. Unlike bacterial endotoxin, hyperreactivity to Cr-ET was not induced in mice by prior infection with BCG.

1-(S)-Hydroxy-2-(S, S)-valylamido-cyclobutane-l-acetic acid was isolated from a fermentation broth of an unidentified Streptomyces species X-1092. The structure was determined by single crystal X-ray diffraction analysis of the p-bromophenylcarbamyl derivative. The substance inhibits the growth of gram-positive microorganisms in a chemically defined medium but growth inhibition is partially reversed by L-cysteine.

A C-nucleoside analog of cordycepin, 6-amino-8-(3-deoxy-β-D-erythro-pentofuranosyl)purine (6), has been synthesized. 3-Deoxy-2,5-di-O-(p-nitrobenzoyl)- β-D-erythro-pentofuranosyl bromide reacted with mercuric cyanide in nitromethane to give 2,5-anhydro-4-deoxy-3,6-di-O-(p-nitrobenzoyl)-D-ribo-hexononitrile which, after acid hydrolysis and removal of the protecting groups, afforded 2,5-anhydro-4-deoxy-D-ribo-hexonic acid. Reaction of this acid with 4,5,6-triaminopyrimidine gave the corresponding amide, which was pyrolyzed to give compound 6. The mass- and n.m.r.-spectral data for the synthesized analog are quite similar to those of the natural antibiotic.

A technique is presented for applying infrared gas analysis to the determination of alcohol in liquid samples. The sample is incubated in a water bath and its gas phase directly introduced into the determination cell of the analyzer by means of a circuit tube.

Infrared methods permit detection of CO within tissue under nearly physiological conditions. The CO stretch bands exhibit frequencies, band widths and intensities characteristic of the particular binding site with areas related to concentrations. For small volumes (

A new metabolite, KD16-U1, has been isolated from the culture of Streptomyces filipinensis. The structure of the metabolite elucidated in this paper has been found to be closely related to shikimic acid.

Pilot whale head oil (blackfish head oil, raw) was analyzed by means of IR spectroscopy, NMR, thin layer chromatography, and gas liquid chromatography-mass spectrometry. The oil consisted of hydrocarbons (mainly pristane) (3%); waxes and cholesterol esters (9%); triglycerides (87%) (i.e. non-11%, mono-19% and di-57% isovalero triglycerides) and cholesterol and diglycerides (1%). By mass spectrometry, the diisovalero triglycerides were shown to be mainly symmetrical. Fatty acids were isobranched or normal (only traces of anteiso acids were found), saturated, or monounsaturated. Isovaleric acid predominated (54 mole % fatty acids), the rest having 10–18 carbon atoms. A 5-carbon fatty acid was the only acid found in the waxes. The alcohol composition qualitatively resembled that of the fatty acids, but major quantitative differences were present. This rules out direct interconversion of all fatty acids and alcohols. The possible role of these lipids in ultrasound transmission is discussed.

The pulmonary toxicity of mold-damaged sweet potatoes has recently been ascribed to a “lung edema factor” which is produced in the roots in response to microbial infection. We now present data suggesting that this toxic principle comprises a group of at least four closely related compounds: 4-ipomeanol (1-(3-furyl)-4-hydroxy-1-pentanone), the isomeric 1-ipomeanol (1-(3-furyl)-1-hydroxy-4-pentanone). the corresponding diketone, ipomeanine (1-(3-furyl)-1,4-pentanedione), and the diol, 1,4-ipomeadiol (1-(3-furyl)-1,4-pentanediol). Isolation and purification of the compounds was accomplished using a combination of column chromatography, preparative gas chromatography, and high pressure liquid chromatography. Structures were initially determined from infrared, nuclear magnetic resonance, and mass spectra. Synthetic procedures for the compounds were devised in order to confirm the assigned structures and to provide an efficient source of the toxins for biological studies. All of these 1,4-dioxygenated-1-(3-furyl)-pentanes arc acutely toxic to the lungs of experimental animals, characteristically producing pulmonary edema and congestion, following a latent period of several hours after dosing. Mice receiving lethal doses of the toxins usually die within 24 h, and pathological findings are seen most often only in the lungs. However, mice initially surviving near-lethal doses of the toxins, particularly 1-ipomeanol and 1,4-ipomeadiol, may show evidence of nephrotoxicity within 1–3 days. The latter observation suggests that pathological responses other than lung damage should also be considered as possible features of moldy sweet potato toxicity.

A simple and sensitive method for the assay of hepatic microsomal epoxide hydrolase activity by using safrole oxide (SAFO) as the substrate is described. It involves differential extraction of the unreacted substrate with n -hexane from the incubation medium containing the reaction product, safrole glycol (SAFG) followed by measurement of absorbancy at 288 nm of the separated hexane layer. A stoichiometric relationship between the SAFO disappearance and SAFG formation was confirmed in the enzymatic reaction.

Low-frequency Raman and far-infrared spectra of polyglycine, poly-L-alanine, and poly-L-valine have been measured. The Raman spectra exhibit an intense band near 100 cm−1 for these homopolypeptides. Lattice calculations of the polyglycines are used to assign the intense Raman band to a rotary lattice mode. For homopolypeptides in the β conformation, an infrared band is observed whose frequency varies inversely with the square root of the mass of the peptide repeating unit. This infrared band is assigned to the hydrogen bond stretching lattice vibration.

Conductometric and spectrophotometric (covering the visible, UV, and IR ranges) studies as well as microanalyses of uranyl complexes with tetracycline revealed the existence of the 1:1 complex species. The mean stability constant of the 1:1 complex, as determined spectrophotometrically, amounted to 1.2 × 105. This finding permits the use of the procedure for the microdetermination of tetracycline using UO2+2ion or vice versa.

Evidence of an interaction between the water-soluble phosphated nonylphenolethoxylate (PNE) and the oil-soluble phosphated fatty alcohol ethoxylate (PFE) could not be obtained when the two compounds were mixed in the anhydrous state. However, measurements of refractive index, interfacial tension, density and viscosity of aqueous solutions of the two surfactants showed anomalies which were at a maximum when they were present in an approximately equal ratio by weight. Thin-layer chromatography confirmed the anomalous properties of mixtures of the two compounds and it is suggested that these result from the formation of a complex material involving PNE, PFE and water.

A pseudomonad has been isolated from sewage, which can utilize 3-chlorobenzoic acid as a sole carbon source. In cells grown on benzoate the enzymes of the β-ketoadipic acid pathway are present. Considerable enzymic activities for chlorinated substrates were found in benzoate grown cells only for the oxygenation of 3-chlorobenzoate and the dehydrogenation of 3- and 5-chloro-3,5-cyclohexadiene-1,2-diol-1-carboxylic acid. 3-Chlorobenzoate grown cells show additional high activities for the turnover of 3- and 4-chlorocatechols and chloromuconic acids.

A new fluorometric method for analysis of citric acid in blood and plasma was established, where the citric acid react with o -aminothiophenol in 35% phosphoric acid solution, at 125°C, for 15 hr. The fluorescent substance was extracted by ethylacetate and measured with excitation at 415 nm and emission at 450 nm. Only 0.05 ml of human blood or plasma is required.

The use of explosives in breaking offences, and in some techniques in the investigation of their use is described.

N-Acetyl-proline-methylamide (APMA) was synthesized by the mixed anhydride method and investigated by IR. spectroscopy and chemical relaxation measurements. The temperature-induced variation of the IR. absorption bands of the internally hydrogen bonded (b) and of the extended, unbonded (e) species at 3330 and 3450 cm−1 respectively, were used to evaluate the molar absorptivities, a(b) = 280 and a(e) = 50 l/mol · cm, the equilibrium constant K = 0.70, and the molar enthalpy of reaction ΔH = − 2280 ± 60 cal/mol. The entropy was estimated to be in the range − 8 to − 9 e.u. The reaction rates of this conformational transition were measured by the chemical dipole field effect. The relaxation time of the rate process is τ = 2.7 · 10−9s, the rate constant for the formation of the hydrogen bond k(b) is 2.2 · 108 s−1, and that for the unfolding accompanied by the breakage of the amide hydrogen bond k(e) is 1.5 · 108s−1.

A technique to measure transmitted infrared radiation from minute biological systems is described. Infrared color film was exposed by radiation transmitted through bacterial colonies. The resultant photographic image was unique for each species of bacteria examined and spectral analysis of the image provided differential light emission patterns which could be quantitated. A formula for developing numerical comparisons among bacterial colonies was provided. The results of this numerical procedure gave quantitative relationships for the total infrared data from each microbial colony and made possible the differential identification of ten species of medically significant bacteria.

1. 1. Cellular lipids of an alcoholophilic bacterium Lactobacillus heterohiochii which is known to produce unusually long chain (C 20 –C 30 ) fatty acids (Uchida K., (1974) Biochim. Biophys. Acta 348, 86–93) were studied with special attention to the distribution of the long-chain acids. 2. 2. Homogenization or disruption of the cells before solvent extraction was found to be necessary for adequate recovery of the cellular lipids. 3. 3. The major lipid constituents were cardiolipin (22%), phosphatidylglycerol (21%), diglycosyldiglyceride (19%), free fatty acid (15%) and, in addition, ethylester of fatty acid (7%). 4. 4. The unusually long chain acids were scarcely located in the neutral lipids, but were esterified exclusively to the phospholipids and the glycolipid in essentially equal concentrations. 5. 5. The significance of the biological membrane containing polar lipids with unusually long acyl chains was given attention in view of the alcoholophilic nature of this bacterium.

Conformational studies of a series of oligopeptides (from the tripeptide to the octadecapeptide) with the repeating sequence L-norvalyl-glycyl-L-proline and a polytripeptide with this sequence are reported. By means of chiroptical techniques, unordered conformations are found for all oligopeptides in water, trifluoroethanol, and ethylene glycol and for the water-insoluble polymer in trifluoroethanol. In ethylene glycol the polymer assumes a collagen-like structure. Infrared studies indicate that all the oligomers, in contrast to the polymer, are unordered in the solid state.

The diffractometric method has more advantages than the camera technique for X-ray diffraction analysis of the crystalline components of human dental calculus. With the use of this crystallographic method and infrared absorption techniques, it was found that the magnesium content of human dental calculus is the result of partial substitution of magnesium for calcium in whitlockite, and that the carbonate content is the result of substitution in apatite.

Amberlite XAD-2 was used to extract bile acids from urine or diluted serum of patients with hepatobiliary diseases. Columns containing Sephadex LH-20 were then used to sepa- rate the sulfated and nonsulfated bile acids. Thin-layer chroma- tography of the sulfated bile acid fraction obtained from urine revealed several spots with RF values different from those of the taurine or glycine conjugates. According to thin-layer chromato- graphic mobilities, gas-liquid chromatographic analyses, in- frared spectra, and elementary analysis of the sulfated material, one of these sulfated bile acids was identified as glycochenodeoxy- cholic acid monosulfate, and the others were presumed to be taurochenodeoxycholic acid sulfate and glycocholic acid sulfate. A large amount of bile acid sulfate was found in urine of pa- tients with hepatobiliary diseases. They accounted for 35.5- 93.3% of total urinary bile acids and consisted of both di" and trihydroxycholanoic acids, with chenodeoxycholic acid as the major acid. Sulfated bile acids were also found in serum, and accounted for 1.8-21.2% of the total bile acids. Only dihydroxycholanoic acids (mainly chenodeoxycholic) were identified.

Thermoluminescence has been observed in tooth enamel, dentine and bone, and is apparently related to the inorganic part of the tissue. Activation energies, mostly below 1 eV, have been estimated for the process leading to the photon emission, and a spectral analysis has been attempted. The underlying mechanisms are thought to be connected to fundamental properties of calcified tissues, and a study of the luminescence is expected to add to the general knowledge of biological hard tissues.

1. 1. The digestive gland of the sea hare Aplysia californica was shown to contain a number of halogenated natural products. Aplysin, debromoaplysin, laurinterol, pacifenol, johnstonol and pacifidience, all derived from the metabolites bolites of the alga Laurencia pacifica , were isolated after chromatography on silica. 2. 2. Two new halogenated monoterpenes, 3,7-dimethyl-1,8,8-tribromo-3,4,7-trichloro-1,5-octadiene and 7-chloro-3,7-dimethyl-1,4,6-tribromo-1-octen-3-ol, were isolated after chromatography on florisil. 3. 3. Examination of extracts of local red algae revealed that the monoterpenes were from Plocamium coccineum var. pacificum . 4. 4. Experiments revealed that the chemical constituents of the digestive gland depended on the algal diet of the individual Aplysia .

The synthesis and complete characterization of certain hitherto unreported copper(II) complexes of β-phenethylamine and mescaline are described. The nature of the bonding in, and the structures of, these complexes are deduced on the basis of electronic and infrared spectral data, mass spectra, and molar conductivity measurements.

The polymerization kinetics and optical rotatory properties of AnBm polypeptides have been studied, where A = D,L-Tyr, D,L-TyrZ, D,L-LysZ, L-AspOBzl, or L-Asp-ONBzl, and B = D,L-GluOR (R = Me or Bzl). In most cases where An and Bm prefer the same helix sense, the polymerization of A N-carboxyanhydride (initiated by Bm in dioxane) shows first order kinetics and produces a monotonic change in optical rotation, while if opposite helix senses are preferred, the kinetics are multiphasic and the change in rotation reverses direction after the addition of several residues. The rotation change in the latter case is interpreted to mean that the helix in the A block is initially induced to take the nonpreferred sense, as originally suggested by Doty and Lundberg from similar observations on (D-GluOBzl)n-(L-GluOBzl)m. It is found here that the CD spectra for the latter polymer show the sign changes required by this hypothesis. The optical rotation curves and CD spectra for (D,L-Tyr)n-(L-GluOBzl)20 suggest, by analogy, that (L-Tyr)n prefers the same helix sense as (L-GluOBzl)n. However, it is found that the opposite conclusion is equally consistent with the data if one considers the effects of possible changes in side-chain conformation on these data in accordance with the calculated CD spectra of Chen and Woody. The optical rotation curves for (D-GluOBzl)n-(L-GluOBzl)20, (D-Tyr)n-(L-GluOBzl)20, and (L-Tyr)n-(L-GluOBzl)20 are all found to be consistent with a two-state equilibrium model in which the A block initially takes on an induced conformation and has an increasing tendency to revert to its preferred conformation as n increases. It is concluded that in both D-Tyr and L-Tyr the side-chain and/or the backbone conformation is induced by the neighboring L-GluOBzl block, and the data do not distinguish which type of change is occurring. These results are discussed in connection with other observations bearing on the helix sense of (L-Tyr)n.

A method has been developed for the determination of 2,4-dihydroxy-1,4(2H)-benzoxazin-3-ones, which occur in corn (Zea mays L.) plants as glucosides. The method involves freezing and thawing of corn tissue samples to allow enzyme-catalyzed cleavage of the glucosides, fragmentation, extraction of the released aglycons, removal of chlorophyll, conversion of the 2,4-dihydroxy-1,4(2H)-benzoxazin-3-ones to the more stable 2(3)-benzoxazolinones, extraction of the 2(3)-benzoxazolinones, and quantitative ir measurement of the 2(3)-benzoxazolinones in methylene chloride solution. The amount of 2(3)-benzoxazolinone calculated as 6-methoxybenzoxazolinone (MBOA) obtained from B37 × B14 single-cross corn was found to be 1.56 mg 50 g fresh weight (10 samples; SD 0.16 mg). For synthetic samples, the precision of the method is that of the reproducibility of the spectrophotometer used. Depending upon the spectrophotometer used, a detection limit of 0.03–0.06 mg MBOA 50 g fresh tissue was observed.

Oriented films of bacteriophage DNAs of low and intermediate (G + C) content and of different chemical composition were investigated by infrared linear dichroism: PBS1, DNA (28% G + C, uracil replaces thymine), T4, DNA (34%, G + C, glucosylated), T4* DNA (34% G + C, unglucosylated), T5, DNA (39% G + C). None of these phage DNAs exhibit a transition to a predominantly pure A form when relative humidity is lowered. At lower relative humidity, the infrared dichroism of the 1230-cm-1 band changes to mainly parallel orientation with respect to the DNA axis. The pattern of the tansition as a function of relative humidity indicates the presence at low relative humidity of a well-defined form for which the O2–O3 line of the phosphate group was found to be directed approximately at 52°C with respect to the helix axis. This allows one to assign the lower-humidity form of these phage DNAs as a predominant C-like form. The comparison of T4 with T4* DNA indicates that glucosylation has no effect on conformational properties of phage DNAs, and particularly on the absence of the B to A structural change. The replacement of the thymine by uracil in DNA of PBS1, has not affected the structural properties of the B form at high humidity nor the absence of the main A form at lower humidity; the transition from the B form to a predominant C-like form was observed.

The human serum high-density lipoprotein sub-class of hydrated density 1.125–1.21 g/ml (HDL3) has been shown by preparative isoelectric focusing to consist of at least twelve different subpopulations having reproducible isoelectric points, at 25 °C, ranging from 3.8 to 7.4. Some of the components had isoelectric points identical to those observed for the components of human serum high-density lipoprotein sub-class of hydrated density 1.063–1.125 g/ml (HDL2). The recombined components were indistinguishable from native HDL3 either by analytical ultracentrifugation or by agarose gel electrophoresis. When the HDL3 fractions were combined, all the pooled fractions contained protein, cholesterol and phospholipid but in different amounts. The fractions also differed in their sedimentation coefficients and in their ultraviolet and infrared spectra Polyacrylamide gel electrophoresis of the delipidated fractions showed that the proteins were not uniformly distributed. These data suggest that HDL3 consists of several discrete lipoprotein subspecies some of which may be different from those in HDL2.

2-Phenethyl alcohol (2-PEA) and 2-phenyllactic acid (2-PLA) were isolated from the culture filtrates of Candida species grown in media containing peptone or phenylalanine as nitrogen source. These compounds were characterized by comparing their UV, IR, and NMR spectral properties with authentic samples. Candida species differed markedly in their production of 2-PEA and 2-PLA. Experiments using [14C]-phenylalanine indicated that both 2-PEA and 2-PLA are synthesised from L-phenylalanine. A pathway for the biosynthesis of 2-PEA from L-phenylalanine has been proposed.

Gas liquid chromatographic analysis of the fatty acid methyl esters from eggs ofDermacentor andersoni Stiles (Ixodidae) revealed the presence of significant quantities (15% total fatty acids) of an unidentified component with a retention time between C18∶3−C22∶0 fatty acids. Smaller amounts of the unidentified component (ca. 5% total fatty acid) also were detected in host rabbit serum. Purified, the unidentified component's methyl ester collected from the tick eggs by preparative gas liquid chromatography was partially identified and characterized by chemical and spectroscopic analyses. The evidence suggests that the unidentified component is a methyl branched C15 tricarboxylic acid containing two vicinal carboxylic acid groups. Biosynthesis of the unidentified component by the tick is under investigation.

Summary Studies on infrared spectra revealed that β-structured polypeptide in the outer membrane of Escherichia coli was stable in dodecylsulfate solution but almost disappeared when it was heated in the presence of dodecylsulfate. The heating of the outer membrane alone did not cause decrease but somewhat increase of β-structured polypeptide. Such an increase was significant when the cytoplasmic membrane was heated in the absence of dodecylsulfate. The result was consistent with the observation that the mobility of outer membrane protein in acrylamide gel was altered when it was heated in the presence of dodecylsulfate.