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81.
Kazuo Koyama Takashi Hirao Akira Toriba Kazuichi Hayakawa 《Biomedical chromatography : BMC》2013,27(5):583-588
The quality of starch‐containing foods may be significantly impaired by contamination with very small amounts of α‐amylase, which can enzymatically hydrolyze the starch and cause viscosity loss. Thus, for quality control, it is necessary to have an analytical method that can measure low amylase activity. We developed a sensitive analytical method for measuring the activity of α‐amylase (from Bacillus subtilis) in starch‐containing foods. The method consists of six steps: (1) crude extraction of α‐amylase by centrifugation and filtration; (2) α‐amylase purification by desalting and anion‐exchange chromatography; (3) reaction of the purified amylase with boron‐dipyrromethene (BODIPY)‐labeled substrate, which releases a fluorescent fragment upon digestion of the substrate, thus avoiding interference from starch derivatives in the sample; (4) stopping the reaction with acetonitrile; (5) reversed‐phase solid‐phase extraction of the fluorescent substrate to remove contaminating dye and impurities; and (6) separation and measurement of BODIPY fluorescence by HPLC. The proposed method could quantify α‐amylase activities as low as 10 mU/mL, which is enough to reduce the viscosity of starch‐containing foods. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
82.
Yusuke Kawashima Mamoru Satoh Tatsuya Saito Takashi Matsui Fumio Nomura Hiroyuki Matsumoto Yoshio Kodera 《Biomedical chromatography : BMC》2013,27(6):691-694
We report a cyclic sample pooling technique devised in two‐dimensional liquid chromatography–electrospray ionization mass spectrometry (LC‐ESI‐MS) shotgun proteomics that renders deeper proteome coverage; we combined low pH reversed‐phase (RP) LC in trifluoroacetic acid in the first dimension, followed by cyclic sample pooling of the eluate and low‐pH RP‐LC in formic acid in the second dimension. The new protocol has a significantly higher resolving power suitable for LC‐ESI‐MS/MS shotgun proteomics. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
83.
Fujiko Iwasaki Hideyuki Nishiyama Noriko Manabe Masanori Yasui Noboru Matsumura 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1):429-430
Abstract Novel metal-carbene complexes (4) with a metallapentalene framework have been obtained from hypervalent diazadiselenathiapentalenes (3) by treating with Pt(PPh3)4, Pd(PPh3)4 and RhCl(PPh3)3. X-Ray investigations revealed that the central hypervalent sulfur atom in 3 was substituted by a metal atom to form M-Se bonds in the resultant metallapentalene framework. 相似文献
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Masahiro Ishino Kaoru Kinoshita Kunio Takahashi Takashi Sugita Motoo Shiro Kimiko Hasegawa Kiyotaka Koyama 《Tetrahedron》2012,68(41):8572-8576
Three novel diterpenes, phomactins K–M (1–3), were isolated from the cultures of an unidentified marine-derived fungus. The structures of 1–3 were elucidated from spectroscopic data (NMR, MS, IR), and the absolute configurations of 1, 2, and the relative configuration of 3 were determined by X-ray diffraction analysis. 相似文献
88.
The rate constant of the reaction of NO3 radical with CF3I was determined by a relative rate method using a Fourier transform infrared (FTIR) spectrometer smog chamber with a long path length gas cell. As a result, the upper limit of the rate constant was determined to be <2.2 × 10?18 cm3 molecule?1 s?1 in 100 Torr of total pressure at 298 K, which suggests that CF3I emitted into the atmosphere accumulates during night. The rate constant of the reaction of NO3 with I(2P3/2) was also measured using time‐resolved cavity ring‐down spectroscopy. The rate constant showed no pressure dependence in the range of 100–500 Torr of total pressure at 298 K and was determined to be (3.9 ± 1.0) × 10?11 cm3 molecule?1 s?1. The present result is different from the previous ones and is about half of that reported most recently. From this rate constant, it is likely that the reaction of NO3 radical with I(2P3/2) does not have a much influence on the loss of I(2P3/2) and the formation cycle of IO radical in the atmosphere. © 2012 Wiley Periodicals, Inc. Int J Chem Kinet 44: 649–660, 2012 相似文献
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(R)-Tetrahydrozerumbone 2, which has a powerful balmy fragrance, contains a stereogenic carbon at the C2 position and can be easily prepared from zerumbone 1, one of the most important materials displaying an NMRDOS character. The reduction of 2 gave two diastereomers of tetrahydrozerumbol 3, and the optically active (>99%ee) alcohols were obtained by a lipase-catalyzed stereoselective transesterification of each racemic alcohol. A barrier to this development is a long reaction time (about four weeks) and the need to separate the diastereoisomers. The desired (2R)-form of 3 was efficiently obtained by a lipase-catalyzed transesterification under optimized conditions using a diastereomeric mixture of racemic 3 as the starting material without separation of the diastereomers. Using this method, the reaction of other zerumbone derivatives is greatly improved. 相似文献
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