Commercial Syrup Research Articles

Simultaneous Determination of dl-Methylephedrine Hydrochloride and Dihydrocodeine Phosphate in Antitussive Syrups by High Performance Liquid Chromatography

A method for the simultaneous determination of dl-methylephedrine hydrochloride (ME-H) and dihydrocodeine phosphate (DC-P) in antitussive syrups by using high performance liquid chromatograph (HPLC) was described. A sample solution for HPLC was prepared as follows. A sample syrup was poured into cation exchange resin column (Amberlite CG 50 NH4 type, 1 cm i.d.×8 cm). After washing the column with water, ME-H and DC-P were eluted with 0.1 N HCl. The eluate was alkalized and extracted with chloroform. The chloroform solution was evaporated to dryness and the residue was dissolved in methanol containing acetaminophen as an internal standard. An aliquot of the sample solution was injected into HPLC equipped with UV-254 nm detector. dl-Methylephedrine and dihydrocodeine were separated on a styrene-divinyl benzene copolymer column (4 mm i.d.×15 cm) by using ammonia-methanol (1 : 99, v/v) as a mobile phase. By washing the cation exchange resin column sufficiently, influence of caffeine on the recovery of DC-P was removed. This procedure was found to be applicable to almost all commercial syrups and to give satisfactory accuracy.

High Pressure Liquid Chromatographic Determination of Antihistamine-Adrenergic Combination Products: Collaborative Study

A reverse phase high pressure liquid chromatographic method in which ion-pairing is used for the determination of combinations of pseudoephedrine hydrochloride with triprolidine hydrochloride or chlorpheniramine maleate in syrups and tablets was collaboratively studied by 8 laboratories. Collaborators were supplied with 12 samples including synthetic and commercial syrup formulations and commercial tablet composites. Mean recoveries of pseudoephedrine hydrochloride and triprolidine hydrochloride from synthetic syrup formulations were 100.5 and 99.6%, respectively. Mean recoveries of pseudoephedrine hydrochloride and chlorpheniramine maleate from synthetic syrups were 98.8 and 100.5%, respectively. Mean coefficients of variation for syrups and tablets ranged from 1.68 to 3.07% for pseudoephedrine hydrochloride, from 2.92 to 3.85% for triprolidine hydrochloride, and from 1.34 to 2.15% for chlorpheniramine maleate. The method has been adopted official first action.

Efficacy of Instant Glucose-Reply

In a study using normal volunteers, we demonstrated a failure of direct oral absorption of glucose from instant glucose. Absorption of tritium-labeled glucose through the buccal mucosa was also not observed. The free glucose content of this preparation was found to average only 143 milligrams of glucose per gram of instant glucose. Since instant glucose is manufactured using a commercial corn syrup base, the bulk of carbohydrates in this preparation was thought to consist of disacharides and oligosaccharides. Thus, it was concluded that the only likely mechanism by which glucose could be absorbed in sufficiently large quantities to reverse hypoglycemic coma in diabetic subjects would involve first intestinal hydrolysis and then absorption. We are indebted to Dr Rosenbaum and his colleagues for providing their experience using instant glucose at the Cleveland diabetic camp. Since most carbohydrate in instant glucose is disaccharides and oligosaccharides, which require disaccharidases for hydrolysis

Reverse Osmosis of Glucose Syrups

AbstractThe paper presents data on the osmotic pressure of glucose syrup fractions obtained by reverse osmosis fractionation of a 43% D.E. commercial glucose syrup and membrane performance at different starting solids contents. Details regarding the production of glucose syrup fractions in the range 15–80% D.E. are given. The fractions produced consist of a narrower spectrum of sugars than is found in a commercial syrup of the same D.E. and thus offer new types of syrup to the industrial user of glucose syrups. Reverse osmosis and ultrafiltration seem to offer the only feasible economic means for obtaining specialised sugars from glucose syrups.

Selected physical properties of glucose syrup fractions produced by reverse osmosis

SummaryA series of glucose syrup fractions in the range 15‐67 D.E. were produced by reverse osmosis. Specific rotation, average molecular weight and solubility rate were determined for each fraction. Similarly, these parameters were determined for a series of commercially produced glucose syrups and the data for both series subjected to a statistical analysis to establish any differences between the series for a particular property.No significant differences were established either for specific rotation or solubility rate but a significant difference was established between the average molecular weight of a fraction and a commercial syrup of the same D.E.The glucose syrup fractions were later found to contain relatively large amounts of inorganic salts and, after demineralization, specific rotation and average molecular weight were redetermined. A significant difference was established between fractions before and after demineralization for both these properties, thus showing the importance of demineralization when measuring these parameters.

Human Urinary Excretion of Piperazine Citrate from Syrup Formulations

A modified colorimetric method using Folin’s amino acid reagent was used for the quantitative determination of piperazine in human urine. Comparative urinary excretion trials were carried out on five subjects using two different piperazine citrate syrup formulas. Within each individual, the percentage and pattern of excretion of piperazine citrate after oral administration of a newly developed syrup formula, equivalent to 3.5g. piperazine hexahydrate, compared favorably with a commercial syrup sample taken in this investigation as a standard.

Urinary Excretion of Ephedrine in Man without pH Control following Oral Administration of Three Commercial Ephedrine Sulfate Preparations

In a feasibility study, 25-mg. single oral doses of ephedrine sulfate, in the form of a commercial syrup and two commercial capsules, were administered in crossover fashion to three nonsmoking male subjects. Urinary pH was not controlled, but adequate urinary flow rates were maintained by regulated water intake. Urinary excretion of ephedrine was measured over a 48-hr. period by a GC method. There were no significant differences in average amounts of ephedrine excreted during any of the 11 sampling intervals, in average peak excretion rates, nor in average times of occurrence of the peak excretion rate. There were insufficient subjects used in this preliminary study to form definite conclusions about differences between or among dosage forms. The urinary excretion data were adequately described by the two-compartment open model with first-order absorption and lag time. The average elimination half-life of ephedrine was 5.99hr. estimated from the β-values obtained by exponential fitting. Average urinary pH was 6.30 (95 of the 99 samples fell within 5.32 to 7.28). The data provided little, if any, evidence of significant relationships between deviations of observed from theoretical excretion rates of ephedrine and urinary pH, urinary excretion rates of ephedrine and urinary pH, or excretion rates of ephedrine and urinary flow rates.

The occurrence of abscisic acid in inhibitors B1 and C from immature fruit of Ceratonia siliqua L. (carob) and in commercial carob syrup

The presence of abscisic acid in the inhibitors B1 and C from immature carob fruit, whole and minus seed, has been established by thin-layer and gas chromatography and by combined gas chromatography-mass spectrometry. Abscisic acid has been identified in commercial carob syrup by the same means. Most, if not all, of the growth inhibitory activity in these fractions is accounted for as abscisic acid by quantitative gas chromatography as the methyl ester. Trimethylsilylation of abscisic acid with bis (trimethylsilyl) acetamide in pyridine gives two isomeric tris(trimethylsilyl) derivatives.

A Liquid with Unusually High Sound Velocity

During a study of the effect of molecular structure on sound velocity in liquids, a liquid was found in which the velocity of sound is 3000 meters/second at 20°C, as measured by a 3-Mc ultrasonic interferometer. Previously the highest value known was less than 2000 meters/second, for glycerine. The new liquid is a viscous concentrated aqueous solution of sorbitol, prepared by heat dehydration of the commercial syrup “Arlex.” Sorbitol was selected for study, even though it is a solid, because its chemical structure is that of a double glycerine molecule. Concentrated sorbitol solutions also show a dispersion of sound velocity with frequency in the megacycle range (reminiscent of the behavior of polyisobutylene as described by Mason) and absorption coefficients many times larger than that of glycerine.

ANALYSIS OF STARCH SYRUP

Examination of a number of starch syrups revealed wide differences in content of non-carbohydrates: water, 17.4 to 28.7%; protein 0.05 to 1.0%; ash 0.2 to 1.6%, sodium chloride 0.1 to 0.7% and sulphur dioxide 0 to 340 p.p.m. The commercial wheat syrups examined had high protein and salt contents, and a sample prepared by direct acid hydrolysis also contained an appreciable amount of ammonium chloride. Maximum absorption by storage color was observed at 3500 to 4500 Å; this region is therefore suitable for routine color measurements. Steinhoff's empirical copper acetate procedure for the direct determination of dextrose was found to be strongly influenced by heat treatment, total salt, and copper concentration; it was not improved by changing the composition of the reaction mixture. Moisture data obtained by vacuum oven and toluol distillation methods showed close agreement on syrups of widely different dextrose equivalent value; an improved stirring device is described for the incorporation of syrup and dispersing agent in either of these procedures.

SUGAR PRODUCTION BY WHITE AND YELLOW BIRCHES

White and yellow birch trees produced an abundance of sap, but the yield of sugar was on the average only about one-third that of the sugar maple. Results indicate that yellow birch sap contains invert sugar with small amounts of sucrose, and that white birch sap contains a mixture of fructose and invert sugar. Syrups prepared from white and yellow birch saps by concentrating 100 times were similar in taste and appearance to commercial corn syrup.

THE PREPARATION OF CRYSTALLINE LACTIC ACID

On account of its importance in intermediary metabolism, lactic acid was among the first compounds chosen in our plan, which we have described in a previous communication (1), to augment the available data on the free energies of formation of substances significant in biological chemistry. It was necessary for this purpose to obtain pure crystalline lactic acid, free of water, anhydride, and lactide. The only description in the literature of the preparation of crystalline lactic acid is that of Krafft and Dyes (2). Table I shows that the product obtained by their method contains relatively large quantities of anhydro impurities. The subject of the present communication is the description of a method which yields the active isomers of lactic acid in a crystalline state, free of water, anhydride, and lactide, supplemented by the description of two methods of separating the active forms from the commercial syrup (1). Lactic acid commercially available at present either is in the form of the U.S.P. syrup, which usually exhibits a low optical activity corresponding to the excess it happens to contain, which is variable, of one or the other optical isomer, or is the expensive zinc sarcolactate. The methods described below now make it possible to obtain easily and quickly and at low cost large quantities of both active isomers in a relatively high degree of purity.