Separation of glucooligosaccharides and polysaccharide hydrolysates by gradient elution hydrophilic interaction chromatography with pulsed amperometric detection

Commercial glucooligosaccharide mixtures (Polycose) and polysaccharide hydrolysates (acid and enzymatic) were fractionated by hydrophilic interaction chromatography and observed by pulsed amperometric detection. Seven peaks were observed when 625 ng of glucose oligomers in Polycose were fractionated. The between-run precision of retention times (n = 10, 100 μg, 15 peaks) ranged from a relative standard deviation (R.S.D.) of 0.09 to 0.40%; between-run precision of peak areas (n = 10) for the same separations had values that ranged from 2.66 to 14.4%. Injection-to-injection time was 48 min. When polysaccharide hydrolysates were fractionated using a gradient program capable of resolving all of the oligosaccharide species, dextran-derived -(1→6)- glucooligosaccharides were retained to a greater degree than amylose-derived -(1→4)-glucooligosaccharides, which were retained to a greater degree than β-(2→1)-fructooligosaccharides derived from inulin. Excluding the peaks that eluted before glucose or fructose, 25 to 35 peaks were observed after fractionation of the hydrolysates. Differences in elution profiles were observed between acid and enzymatic hydrolysis products of the same polysaccharide as well as between hydrolysis products of different polysaccharides. In conjunction with high-performance size-exclusion chromatography, the method demonstrated the effect of preheating starch before hydrolysis with isoamylase.     

Tertiary amines promoted synthesis of symmetrical 1,3-disubstituted ureas

Symmetrical 1,3-disubstituted ureas and cyclic ureas have been synthesized from corresponding isocyanates and diisocyanates by a new versatile, simple and quick method in the presence of tertiary amines at room temperature. The method under investigation has several advantages over the existing techniques, as it is simple to carry out; does not require complicated equipment; work-up is simple, as it does not use expensive chemicals. Moreover, the yields are almost quantitative. It has a potential for commercial applications in pharmaceutical chemistry.     

Characterization of methyl methacrylate grafting onto preirradiated biodegradable lignocellulose fiber by gamma-radiation

Gamma-radiation-induced graft copolymerization of methyl methacrylate onto natural lignocellulose (jute) fiber was carried out by the preirradiation method in an aqueous medium by using octylphenoxy-polyethoxyethanol as an emulsifier. The different factors that influenced the graft copolymer reaction process were investigated. In the case of radiation-dose-dependent grafting, samples irradiated in the presence of air produced up to 73% graft weight compared to 53% obtained in the case of irradiation in a nitrogen environment. By assuming Arrhenius reaction kinetics, the activation energy (E(a)) of the grafting reaction process was evaluated for different reaction temperatures. Moreover, the graft copolymer reaction was controlled by incorporating a homopolymer-inhibiting agent and three different chain-transfer agents in the reaction medium. The mechanical and thermal properties of jute fiber 'as received' and jute-graft-poly(methyl methacrylate) were also investigated. The results showed that the percentage of grafting with jute fiber has a significant effect on the properties. The kinetic parameters were evaluated from TGA thermograms by using Broido's method in the temperature range 240-350 degrees C. Scanning electron micrographs show that the structural changes on the surface of jute fibers were induced by graft copolymerization of methyl methacrylate monomer. Fiber-fiber surface friction was measured in terms of the average maximum load and the kinetic friction. SEM of jute-graft-poly(methyl methacrylate).     

Determination of Furosemide by Simple Diazotization Method in Pharmaceutical Preparations

A simple and rapid spectrophotometric method has been investigated for the determination of furosemide. The method is based upon simple diazotization reaction. The absorbance was measured at 480 nm. The method is optimized for acidity, amount of reagents required and heating time. The range of linearity was 0.4–10 μg mL^?1 of furosemide with molar absorptivity of 1.0 × 10⁴ l mol^?1 cm^?1. Standard deviation, coefficient of variance, limit of detection and limit of quantification were calculated using authentic standard of furosemide and were found to ± 0.0013,12.7%, 0.16 ppm and 0.52 ppm, respectively. The method was applied to various pharmaceutical preparations containing furosemide. The results of the investigated method for furosemide were compared with available official literature method. The results obtained by the proposed method agree well with the standard established method.     

Iodine binding by amylopectin and stability of the amylopectin–iodine complex

The iodine binding capacity (IBC) of amylopectin (AP, from potatoes) is determined to be around 0.38% (w/w) of the total AP in the solution. The mass of iodine bound comprises about 13.6% of the mass of AP involved with the complex, suggesting that with every four iodine atoms bound there are 23 anhydroglucose residues (AGU). Since our previous study indicates that four iodine atoms within the helix of 11 AGUs form a chromophore unit in the API complex, only 48% of the AGUs (11 out of 23) in the AP molecule are directly involved with the iodine. The heat of reaction for the API complex formation is determined to be around ?47 kJ/mol of I–I units bound and is significantly lower in magnitude than that of the amylose-iodine (AI) complex [Biopolymers, 31 , 57 (1991)]. A possible mechanism has been proposed for the formation of AI and API complexes with fixed compositions. © 1994 John Wiley & Sons, Inc.     

Rapid and easy identification of Illicium verum Hook. f. and its adulterant Illicium anisatum Linn. by fluorescent microscopy and gas chromatography

Illicium verum Hook. f. is used as an herbal tea to treat colic pain in infants. Reports suggest that Star anise herbal tea may be adulterated with Illicium anisatum Linn. A short and rapid method using microscopy and gas chromatography (GC) was developed to detect I. anisatum Linn., an adulterant in the powdered mixture of I. verum. Anatomical differences in the epicarp cells of I. verum and I. anisatum fruits were clearly defined as examined under fluorescent microscopy and scanning electron microscopy. A GC method was developed for quick identification of possible I. anisatum adulteration with I. verum.     

Synthesis of a novel, highly symmetric bis-oxa-bridged compound

A highly oxygenated, novel pentacyclic bis-oxa-bridged compound 8 was synthesized with remarkable efficiency starting from readily available tetrachloro-5,5-dimethoxyclopentadiene and 1,4-cyclohexadiene in three steps. The ruthenium-catalyzed oxidation of 2:1 bis-adduct 1 followed by a one-pot transformation of the resulting bis-alpha-diketone 3 furnished (after esterification) the title compound in an overall yield of 29.1%. The versatility of this simple method was further demonstrated with other norbornyl alpha-diketones to obtain the corresponding strained oxa-bridged derivatives.     

Anion-exchange initiation of reactions: Detection and spectrophotometric determination of aliphatic amines with 2,4-dinitrophenylhydrazine

The role of anion-exchange resin beads in the initiation of reactions of tertiary amines with 2,4-dinitrophenylhydrazine has been explored. This reagent has been used for the selective detection and determination of aliphatic amines. Radiochemical studies have been performed to show that the coloured species is adsorbed but not exchanged on ion-exchange beads. A model for the interaction is proposed.     

Rydberg states of the strontium ion

We report on the spectroscopy of highly excited strontium ions after resonant multistep laser excitation. The states observed belonged to then s (26≦n≦79),n d (25≦n≦83),n f (28≦n≦86) andn g (30≦n≦81) series of Sr⁺. A least squares fit has been applied to determine the quantum defects and their linear energy dependence in each series, together with the ionisation limit of Sr⁺. The analysis of our data lead to a revised value for this ionisation limit of 88 965.18±0.02 cm^?1, with respect to the ground state of the Sr⁺ ion. Analysis of the non core-penetratingn g states yielded experimental values for the dipole and quadrupole polarizability of Sr⁺⁺, which are in satisfactory agreement with previous calculations.     

HPTLC Method for Determination of 20-Hydroxyecdysone in Sida rhombifolia L. and Dietary Supplements

Naturally occurring 20-hydroxyecdysone is an important anabolic ecdysteroid. A simple thin-layer chromatography method to quantitate 20-hydroxyecdysone in methanolic extract of the whole plant material of Sida rhombifolia L. was developed. This method was successfully applied for quantitative evaluation of dietary supplements. The separation was achieved on glass TLC plates coated with silica gel 60F254, using chloroform: methanol (8:2 v/v) as developing solvent. Densitometric evaluation of 20-hydroxyecdysone was performed at 250 nm in reflectance/absorbance mode. The calibration was in the range of 200–1,000 ng spot^?1 and correlation coefficient for the calibration curve was >0.999. In addition, for six different Sida species unique fingerprints were obtained on the HPTLC plate.