Abstract DL-Valine was resolved completely by a solvent extraction system with continuous sample feeding process called countercurrent fractional (CFE). The two-phase contained n-butanol and water copper(II) complex of N-n-dodecyl-L-hydroxproline as resolving reagent. upper (alcohol-rich) phase the lower (water-rich) proceeded in segmented columns countercurrently; D-isomer recovered phase, while L-isomer phase. optical purity enantiomers obtained consistently 99.5% or higher. extracted...

Abstract The new prototype of the cross-axis coil planet centrifuge (X-axis CPC) fabricated in our laboratory provides various improvements over original unit such as ambient temperature control, good visibility rotary frame and substantial reduction torque by a round transparent case, direct motor shaft coupling to stabilize system, ease belt tension adjustment using idler pulleys. capability system was demonstrated separation stable proteins with polymer phase pair eccentric assembly...

The present studies have been conducted to investigate the cause of an unusually broad peak ovalbumin obtained by countercurrent chromatography (CCC) reported earlier [K. Shinomija et al., J. Chromatogr., 644 (1993) 215]. A series CCC experiments using our prototype cross-axis coil planet centrifuge revealed that commercial products were classified into two groups: group formed peaks at pH 7.0 and 5.8, while B showed a relatively sharp single in range pH. Electrophoresis indicated consisted...

Abstract Commercial D,L-kynurenine was resolved by high-speed countercurrent chromatography using a cross-axis coil planet centrifuge. The separation performed with an aqueous-aqueous polymer phase system composed of 10% (w/w) polyethylene glycol 8000 and 5% dibasic sodium phosphate containing 6% bovine serum albumin as chiral selector. lower phosphate-rich mobile eluted the L-enantiomer first followed D-enantiomer. peak resolution 0.94 for 2.5 mg sample. completed within 3.5 h.

Abstract Sugars and their p-nitrophenyl (PNP) derivatives were separated by high-speed countercurrent chromatography using a cross-axis coil planet centrifuge (cross-axis CPC) equipped with pair of eccentric assemblies. A polar two-phase solvent system composed 1-butanol/acetic acid/water (4:1:5) was used for the separation sucrose fucose, glucuronic acid (lactoid form) galacturonic acid, while 1-butanol/ethanol/water (4:1:4) free lactoid forms acid. PNP-sugar such as neutral sugars, uronic...

Abstract Proteins were separated using a cross-axis coil planet centrifuge equipped with two different types of coiled columns, i.e., toroidal and eccentric assemblies. An aqueous-aqueous polymer phase system composed 12.5% (w/w) polyethylene glycol 1000 dibasic potassium phosphate was used for the separation cytochrome C, myoglobin ovalbumin. The assemblies 1 mm ID tubing yielded partition efficiency 170 theoretical plates at peak. A slightly higher obtained from same diameter. highest 450...

ABSTRACT Effect of elution modes on protein separation was investigated using cross-axis coil planet centrifuge (cross-axis CPC) with two different types coiled columns, i.e., eccentric and toroidal assemblies. Myoglobin lysozyme were separated an aqueous two-phase solvent system composed 12·5% (w/w) polyethylene glycol 1000 dibasic potassium phosphate. The substantial effect observed by the coil, while negative result given at coil. Using higher peak resolution proteins attained tail to...

The countercurrent chromatographic separation of isoflavones from a crude soybean extract was performed with various two‐phase solvent systems, using two different types the coil planet centrifuge (CPC) cross‐axis CPC and type‐J multilayer CPC. overall results indicated that separates daidzin genistin an ethyl acetate/ethanol/water (4:2:7) system at purity over 97 near 100%, respectively, while resolves these compounds in much longer elution time acetate/1‐butanol/water (2:1:3) system....

ABSTRACT A newly fabricated spiral column assembly was first applied to the countercurrent chromatographic separation of proteins using cross-axis coil planet centrifuge (cross-axis CPC). The performed by a set stable such as cytochrome C, myoglobin, and lysozyme with an aqueous–aqueous polymer phase solvent system composed 12.5% (w/w) polyethylene glycol (PEG) 1000–12.5% dibasic potassium phosphate. Three sets left-handed single-layer columns different IDs (1.0, 1.5, 2.0 mm) were employed...

Abstract A novel non-isotopic receptor binding technique for the detection of benzodiazepines is described. benzodiazepine labeled with europium chelate was prepared and employed as a ligand, time-resolved measurements long lifetime fluorescence allowed avoidance interference due to proteins in preparation. Experimental results demonstrate sigmoid inhibition curve, ligand inhibited by comparable concentrations unlabeled drug. The proposed assay may provide simple procedure measurement...

Various aliphatic dicarboxylic acids were separated by countercurrent chromatography using cross-axis coil planet centrifuge (cross-axis CPC) equipped with a pair of eccentric assemblies mounted in an off-center position. Partition coefficients these samples optimized adjusting the volume ratio polar two-phase solvent system composed methyl t-butyl ether/1-butanol/acetonitrile/aqueous 0.1% trifluoroacetic acid. Maleic acid and fumaric at 5:0:0:5 lower aqueous phase mobile, while tartaric...

Countercurrent chromatographic separation of hippuric acid (HA) and related compounds was performed using the cross-axis coil planet centrifuge equipped with a pair eccentric assemblies mounted in an off-center position. Partition coefficients HA set were determined on polar two-phase solvent system composed methyl t-butyl ether, 1-butanol, acetonitrile aqueous 0.1% trifluoroacetic at various volume ratios. The optimal ratio 1 : 0 successfully used to resolve p-amino HA, p-methyl...

The spectrophotometric determination of various drugs having a carboxyl function is described. method involves flow injection and specific detection carboxylic acids based on the formation 2-nitrophenyl-hydrazide derivatives mediated by water-soluble carbodiimide. Using this system, linear calibration range spanned three orders magnitude from 125 pmol to 200 nmol both hydrophilic hydrophobic could be determined easily at sampling rate 100 per hour. A number drug preparations were also...

We investigated the effect of a noncompetitive N-methyl-D-aspartate (NMDA) receptor antagonist, (+)-5-methyl-10, 11-dihydro-5H-dibenzo[a, d]cyclohepten-5, 10-iminehydrogen maleate (dizocilpine, MK-801), on hippocampal norepinephrine release in morphine-treated rats order to clarify relationship between NMDA receptors and development morphine dependence. Naloxone hydrochloride injected subcutaneously (s.c.) into morphine-dependent rats, induced an immediate increase release, which was...

Countercurrent chromatographic separation of water-soluble vitamins, such as riboflavin sodium phosphate, cyanocobalamin, riboflavin, pyridoxine hydrochloride, and thiamine nitrate was performed using the cross-axis coil planet centrifuge equipped with a pair eccentric assemblies at off-center position. The solvent system used in present studies prepared by adding 1.5% 1-octanesulfonic acid salt, an ion-pair reagent, to polar two-phase composed 1-butanol aqueous 0.15 M monobasic potassium...

Countercurrent chromatography (CCC) of proteins was performed by the cross-axis coil planet centrifuge (cross-axis CPC) using polyethylene glycol (PEG) - dextran biphasic systems. A pair eccentric assemblies mounted at two different positions (off-center and central) on rotary frame. The best separation obtained from a two-phase solvent system composed 4.0% (w/w) PEG 8000 5.0% T500 in 5 mM potassium phosphate buffer (pH 7.0) 3 M sodium chloride upper PEG-rich phase as mobile phase....

Abstract Vitamins were resolved by high-speed countercurrent chromatography using a cross-axis coil planet centrifuge equipped with eccentric assemblies. A two-phase solvent system composed of 1-butanol/ethanol/aqueous 0.15 M monobasic potassium phosphate (8:3:8) was used for the separation water-soluble vitamins such as thiamine nitrate, pyridoxine hydrochloride, and nicotinamide, while 2,2,4-trimethyl pentane (isooctane)/methanol (1:1) fat-soluble calciferol, vitamin acetate,...

A simple and rapid liquid chromatographic method is described for the determination of barbaloin (aloin, 10-D-glucopyranosyl-1,8-dihydroxy-3-(hydroxymethyl)-9(10H)-anthraceno ne) in foods. Barbaloin extracted with water from foods containing aloe extract cleaned up on a disposable cartridge by using methanol-water (55 + 45) as eluant. The eluted separated chromatography YMC A-302 column (50 50) mobile phase, detected at 293 nm. Recoveries added to levels 0.05 0.50 mg/g were 94.4-100%. Assay...

Abstract Countercurrent chromatographic separation of proteins by the cross-axis coil planet centrifuge was maximized selecting suitable polymer phase system and revolution speed. Polymer systems composed polyethylene glycol (PEG) 1000 several inorganic salts were examined to determine partition coefficient values (K) for various proteins. The overall results indicated that 12.5% (w/w) PEG dibasic potassium phosphate yielded K most except cytochrome C apo-transferrin which may be separable...

A new technique of on-line electrochemical derivatization using glassy carbon column electrode as a reactor is established. Materials eluting from separation are converted in the to form fluorescent or intensely UV-absorbing products, products being monitored by suitable detector. An example use this detection homovanillic acid (HVA) urine. HVA applied (Hitachi #3011-N, 250×4mm i.d.) HPLC and derivatized dimer (2, 2-dihydroxy-3, 3-dimethoxybiphenyl-5, 5-diacetic acid) oxidation reactor. The...

毒キノコのベニテングタケに含有され,中枢神経系に作用するイソキサゾール化合物のイボテン酸とムッシモールの高速液体クロマトグラフィーによる分析法を検討した。カラムはアミノプロピル基を化学結合したShim-pack P NH2-10/S2504を用い,0.01Mリン酸塩緩衝液(pH4.5)-メタノール(30:70)を移動相とし,220nmで検出した。陰イオン交換樹脂及びアルミナを積層したシリカゲルカラムによる前処理を行うことにより混在物の影響もなく,精度良くイボテン酸,ムッシモールの同時定量が可能である。