High performance liquid chromatographic separation of monoacylglycerol enantiomers on a chiral stationary phase

High performance liquid chromatographic separation of monoacylglycerol enantiomers as di-3,5-dinitrophenylurethane derivatives was carried out on a chiral stationary phase, N-(S)-2-(4-chlorophenyl)isovaleroyl-D-phenylglycine chemically bonded tov-aminopropyl silanized silica. Complete separation of the urethane derivatives of racemic monoacylglycerols with saturated acyl groups of C₁₂−C₁₈ was achieved using a stainless steel column (25 cm long) packed with the 5μ particles, an isocratic elution at ambient temperature with a mixture of hexane/ethylene dichloride/ethanol as a mobile phase, and a UV detector. Thesn-1 enantiomers were eluted ahead of the correspondingsn-3 enantiomers. Complete separation of thesn-2 isomers from the corresponding enantiomers and partial separation of the enantiomer homologues differing by two acyl carbons also were observed.     

Oxochloromolybdenum(V)tetraphenylporphyrin complex-containing polymer as a phosphate ion exchanger

Summary Oxochloro(5,10,15,20-tetraphenylporphyrinate)molybdenum (V) was physically entrapped into poly (styrene) by lyophilizing a benzene solution including both complex and polymer. The functional ability of the obtained complex-containing resin to adsorb H₂PO₄ ^– from an aqueous solution was investigated in the presence of various anions. It was found that the selectivity of the resin for H₂PO₄ ^– is superior to those of conventional anion exchangers.     

Effects of coal blending on the reduction of PM10 during high-temperature combustion 2. A coalescence-fragmentation model

A coalescence-fragmentation model has been developed to predict the behaviors of coal mineral particles during the combustion of pulverized bituminous coals or coal blends. Based on the computer-controlled scanning electron microscope (CCSEM) characterization of coal minerals, the particle size distributions (PSDs) and mineral species of ash particles can be simulated. In particular, the interactions among excluded minerals (mainly referring to the excluded Ca-bearing-species and Fe-bearing-species) and included minerals are accounted for in this model. The PSDs and the mineral species of ash particles are derived from the coalescence and fragmentation of coal mineral particles. Based on this proposed model, both of the predicted PSDs and the mineral species of ash particles are in good agreement with their corresponding experimentally measured values. And the comparisons further demonstrate that the combined effects of coalescence of included minerals and fragmentation of excluded minerals have direct impacts on the ash-forming process. In addition, for the coals rich in excluded Ca- and/or Fe-bearing-species, the interactions among included minerals and excluded minerals are another important mechanism governing ash formation for high-rank coals.     

Efficient production of L‐lactic acid by Crabtree‐negative yeast Candida boidinii

Industrial production of L ‐lactic acid, which in polymerized form as poly‐lactic acid is widely used as a biodegradable plastic, has been attracting world‐wide attention. By genetic engineering we constructed a strain of the Crabtree‐negative yeast Candida boidinii that efficiently produced a large amount of L ‐lactic acid. The alcohol fermentation pathway of C. boidinii was altered by disruption of the PDC1 gene encoding pyruvate decarboxylase, resulting in an ethanol production that was reduced to 17% of the wild‐type strain. The alcohol fermentation pathway of the PDC1 deletion strain was then successfully utilized for the synthesis of L ‐lactic acid by placing the bovine L ‐lactate dehydrogenase‐encoding gene under the control of the PDC1 promoter by targeted integration. Optimizing the conditions for batch culture in a 5 l jar‐fermenter resulted in an L ‐lactic acid production reaching 85.9 g/l within 48 h. This productivity (1.79 g/l/h) is the highest thus far reported for L ‐lactic acid‐producing yeasts. DDBJ/EMBL/GenBank nucleotide database with Accession Nos. AB440630 and AB440631. Copyright © 2009 John Wiley & Sons, Ltd.     

Stereospecific analysis of triacyl-sn-glycerols by chiral high-performance liquid chromatography

A method for the stereospecific analysis of triacyl-sn-glycerols by high-performance liquid chromatography (HPLC) on a chiral column is described. Triacyl-sn-glycerols were partially degraded with ethyl magnesium bromide, and the monoacylglycerols produced were separated as 1- and 2-monoacylglycerol fractions by thin-layer chromatography on boric acid-impregnated silica gel plates. The 1-monoacylglycerols were resolved intosn-1 andsn-3 monoacylglycerol fractions by HPLC on a chiral column (Sumichiral OA-4100) after derivatization with 3,5-dinitrophenyl isocyanate. Fatty acid methyl esters obtained from the original triacyl-sn-glycerols, 1- and 2-monoacylglycerol fractions, andsn-1 andsn-3 monoacylglycerol fractions were analyzed by gas chromatography on open-tubular columns. Stereospecific acyl distributions in triacyl-sn-glycerols were calculated from the data. The acyl distributions of several oils were obtained. The method is rapid, simple and gave reproducible results.     

Gas chromatographic separation of wax esters based on the degree of unsaturation

The wax esters of sperm whale head oil have been characterized by gas-liquid chromatography on an APOLAR 10C column according to their carbon number and number of double bonds. The novel technique permits the direct quantitative analysis of saturated and unsaturated wax esters.     

Micro method for stereospecific analysis of triacyl-sn-glycerols by chiral-phase high-performance liquid chromatography

A procedure for micro stereospecific analysis of triacyl-sn-glycerols (TGs) by high-performance liquid chromatography (HPLC) on a chiral column is presented. TGs were partially hydrolyzed with ethyl magnesium bromide, and total products were immediately converted to 3,5-dinitro-phenylurethane derivatives. Each of the 1- and 2-monoacylglycerol (MG) derivatives was isolated by HPLC on a silica column. The 1-MGs were resolved intosn-1 andsn-3 MG fractions by HPLC on a Sumichiral OA-4100 column (Sumitomo Chemical, Osaka, Japan). Fatty acid methyl esters obtained from thesn-1,sn-2 andsn-3 MG fractions were analyzed by gas-liquid chromatography on a capillary column. Analyses of standard TGs showed that, even with 1 mg of sample, accuracy was comparable to that obtained with 100-mg samples. Applying this procedure to the stereospecific analysis of 5 mg of jujube pulp, TGs revealed the positional distribution of the (n-5) series of monounsaturated fatty acids they contained. Honored Student Award Address presented at the 83rd AOCS Annual Meeting held in Toronto, Canada, May 10–14, 1992.     

Force sensorless robust tracking servo system suppressing periodic disturbance and sudden disturbance for optical disk system

This paper proposes a new force sensorless robust tracking servo system, which detects and suppresses both the periodic disturbance and the sudden disturbance without force sensor. The proposed system estimates both the periodic disturbance and the sudden disturbance and the sudden disturbance by using a new sudden disturbance observer and the memory of tracking error. In the proposed system, the influence of sudden disturbance is suppressed by the proposed sudden disturbance observer. On the other hand, the influence of periodic disturbance is suppressed by means of ZPET feed‐forward servo system. The experimental results point out that the proposed tracking servo system has a precise tracking response against both the periodic disturbance and the sudden disturbance. © 2008 Wiley Periodicals, Inc. Electr Eng Jpn, 166(1): 82–90, 2009; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/eej.20614     

Excitation density dependence of luminescence spectrum of electron-hole plasma in diamond

Time-resolved band edge luminescence spectrum in IIa diamond has been measured with the 5th harmonics of a pulsed YAG laser (5.82 eV) and an ICCD image intensifier of 5 ns gate width at 290 K. The time-resolved luminescence spectrum is decomposed into three components of free exciton (FE), excitonic complex (EC) and electron-hole plasma (EHP). The decay times of the FE and EC luminescence are 45 and 27 ns, respectively and that of the EHP luminescence has been seen to be shorter than the gate width, 5 ns. The low energy onset of the EHP luminescence spectrum has been observed to decrease with increasing excitation density and attains the onset of the electron-hole drop luminescence spectrum at the excitation density of 0.6 J/cm², at which the electron-hole pair density is 1.2 × 10²⁰ cm^? 3. Furthermore, the excitation density dependences of the FE, EC and EHP luminescence intensities are explained with the percolation theory.     

Processing of ethanol fermentation broths by Candida krusei to separate bioethanol by pervaporation using silicone rubber‐coated silicalite membranes

BACKGROUND: Pervaporation employing ethanol‐permselective silicalite membranes as an alternative to distillation is a promising approach for refining low‐concentration bioethanol solutions. However, to make the separation process practicable, it is extremely important to avoid the problems caused by the adsorption of succinate on the membrane during the separation process. In this work, the pervaporation of an ethanol fermentation broth without succinate was investigated, as well as the influence of several fermentation broth nutrient components. RESULTS: Candida krusei IA‐1 produces an extremely low level of succinate. The decrease in permeate ethanol concentration through a silicone rubber‐coated silicalite membrane during the separation of low‐succinate C. krusei IA‐1 fermentation broth was significantly improved when compared with that obtained using Saccharomyces cerevisiae broth. By treating the fermentation broth with activated carbon, bioethanol was concentrated as efficiently as with binary mixtures of ethanol/water. The total flux was improved upto 56% of that obtained from the separation of binary mixtures, compared with 43% before the addition of activated carbon. Nutrients such as peptone, yeast extract and corn steep liquor had a negative effect on pervaporation, but this response was distinct from that caused by succinate. CONCLUSION: For consistent separation of bioethanol from C. krusei IA‐1 fermentation broth by pervaporation, it is useful to treat the low nutrient broth with activated carbon. To further improve pervaporation performance, it will be necessary to suppress the accumulation of glycerol. Copyright © 2009 Society of Chemical Industry