Quantification of anti-fertility compound-Diosgenin concentration in the fenugreek seeds aqueous extract (FSA)

Introduction: This study aims to build a standardization method for preparation of effective powder from FSA and to quantify diosgenin in FSA. Methodology: One kg of FS were used in this study. Setting: BMS, KOM and KOP, IIUM Kuantan campus. FS were washed with distilled water to exclude any foreign matter, and were then air dried. FS-powder were put in distilled water in a ratio of 1 g of powder in 20 ml of distilled water and were shaken at room temperature for 24 hours. Ten mg of hydrolyzed extract sample was diluted in 10 ml volumetric flask with methanol for 15 minutes. Chromatographic estimation was performed using an equilibrated reverse phase Eclipse XDB-C18 column (particle size 5 µg, 4.6 mm x 150 mm). Results: One gram of FSA extract was hydrolyzed to produce sapogenins and 46.6% was recovered. A calibration curve that was constructed based on five dilutions of diosgenin standard at concentrations of 2, 5, 10, 20, 30 and 50 ppm produced a linear graft (r = 0.999). The concentration of diosgenin in FSA extract as calculated using the regression analysis was found to be 29.66 µg/ml, 13.81 % w/w on dried weight basis. Conclusion: Preparation and standardization of effective powder from FSA are the corner stone of many scientific researches in IIUM and Malaysia. Diosgenin is available in the FSA in adequate concentration. The adequate amount of diosgenin in the FSA will guide us to do further study in the way of preparation of a natural product that can be used in the field of reversible anti-fertility therapy.

Effect of pH, Anions and Acids on the Extraction of Zinc (II) from Aqueous media using Acetylacetone Solutions of Sulphamethoxazole

The challenge of heavy metal contaminations have been remediated to a certain level by the application of several methods of their extractions from aqueous media. Solvent extraction of zinc (II) ions from buffered aqueous solutions into acetylacetone solution of sulphamethoxazole as a function of pH and concentration of anionic substances and certain mineral acids were investigated in this work. The aqueous medium was prepared by dissolving 1.0995g of ZnSO4.7H2O in 250 ml volumetric flask to form 1000mg/L solution. 50mg/L working concentration was prepared from the 1000mg/L by dilution method. The organic phase is 0.5 M Sulfamethoxazole solution prepared by dissolving 12.664g of the salt in 100 ml acetylacetone. 2 ml each of aqueous and organic phases were taken with micro pipette and transferred into a set of 20 ml extraction bottle and the mixture was agitated mechanically for about 30 minutes. The mixture was allowed to settle and separate into two layers. 1 ml of the aqueous phase was taken, diluted and analysed for Zn (II) ions using atomic absorption spectrophotometer at a wavelength of 213.9. The results obtained on studying the effect of pH showed that Zn (II) ion was quantitatively extracted between pH of 7.0 to pH 8.0. The highest percentage extraction 85.37% was observed at pH 8.0 in acetylacetone solution of sulphamethoxazole. Increase in pH above 8.0 resulted in a steady decrease in the extraction of Zn (II). Studies on the effect of anions showed significant extractions which changes as the anions concentrations increased. All studies on mineral acids also showed significant extractions and increase in the concentrations of the acids affected the percentage extraction. Generally Zinc (II) ions can be extracted quantitatively in mild acids and anions concentrations when buffered from slightly acidic pH ranges of 6.0 to slightly alkaline pH values of 8.5.

Correlations of soybean yield with soil porosity and bulk density of an Oxisol

ABSTRACT The spatial variability of soil physical attributes is important to indicate management practices that best suit agricultural areas. This study aimed to analyze spatial correlations between soybean grain yield and soil mass-volume relationships, in order to select which attribute is correlated with yield, as well as to evaluate the spatial variability of soil attributes and yield components of this crop, in an Oxisol under no-tillage system. The soil attributes analyzed (0.0-0.10 m and 0.10-0.20 m) were the following ones: soil bulk density (paraffin-coated clod and volumetric ring methods), particle density (volumetric flask and modified volumetric flask methods) and total porosity. The soybean yield components were evaluated as it follows: grain yield, number of pods per plant, number of grains per pod, mass of 100 grains, grain mass per plant, plant population and plant height. The total soil porosity, calculated by the relations between the bulk density (volumetric ring method) and particle density (volumetric flask), in the 0.10-0.20 m layer, was the best indicator of soybean grain yield under no-tillage conditions.

Quantitative determination of glycine in pharmaceutical formulations by reaction with 2,3-dichlor-1,4-naphthoquinone reagent

Glycine has been reported to be determined by different techniques including titrimetric methods, VIS spectrophotometry. Some of the proposed methods require inaccessible reagents, others – difficult in execution or offered only for substances. That is why, feasibility of developing new, simple, valid methods for the glycine quantitative determination in medical forms is not in doubt. This paper presents a new, simple and accurate VIS spectrophotometric method for determining of glycine in pharmaceutical formulation using 2,3-dichlor-1,4-naphthoquinone as a reagent. Pharmaceutical preparations: capsules of Doppel Herz, 0,50 g (Queisser Pharma Gmbh & Co, Germany); powder in packets Medichronalum-Darnitsa, 7,00 g (Pharmaceutical company «Darnitsa», Ukraine); tablets of Glycin («Biotiki», Russia).and Glicised («Arterium», Ukraine), 0,10 g. Analytical balance (ABT-120-5DM); UV-VIS spectrophotometer (Specord 200); water bath (Memmert WNB 7-45). The aliquot part (0,1200‒0,2000 g) of the glycine is put into a 25,00 ml volumetric flask, add 7,00 ml water and filled to the mark with DMF. The amount of 1,00 ml of the resulted solution is poured into a 25,00 ml volumetric flask, then treated with 2,50 ml of 1% solution of the 2,3-dichlor-1,4-naphthoquinone and mixed up. A received solution is heated up for 15 minutes on the water-bath under temperature of 95 °С, then is cooled down and filled to the mark with the DMF. Absorbance of the test solution is measured at 470 nm against the background of the compensation solution that does not contain any test solution. Defined minimum calculated by common method is 3,20 mcg/ml. Experimentally determined glycine optimal reaction conditions with the 2,3-dichlor-1,4-naphthoquinone as the basis for the development of spectrophotometric methods for glycine quantitative determination in the 4 drug dosage forms. The analytical method was optimized and validated by establishing the linearity (in the range of 5,00‒8,00 mg/100 ml), the correlation coefficient (r = 1,000), precision and the accuracy. Thus, the peculiarity of the developed method consists in it’s enhanced sensitivity in comparison with other available methods of quantitative determination. The developed method is simple and useful for routine analysis of glycine in pharmaceutical formulations and in-process quality control.

Analysis of Chemical Composition of Different Irreversible Hydrocolloids

Irreversible hydrocolloids (IR) is a dental impression material commonly used in Brazilian and European dental practice because it is inexpensive, easy to handle, has good reproductive detail and is comfortable for the patient. This research aimed to analyze the chemical composition of eight different IRs for dental use. A sample of 0.2 g was weighed and transferred to a Teflon beaker moistened with drops of distilled or deionized water; 5 mL of nitric acid was added until total solubility of the sample; the solution was transferred to a 100 mL volumetric flask, the volume was filled with distilled or deionized water and homogenized. Thirty-five chemical elements were found: Lithium, Beryllium, Boron, Sodium, Magnesium, Aluminum, Silicon, Phosphorus, Potassium, Titanium, Manganese, Cobalt, Nickel, Vanadium, Zinc, Rubidium, Arsenic, Iron, Copper, Strontium, Yttrium, Zirconium, Niobium, Molybdenum, Ruthenium, Cadmium, Tin, Antimony, Barium, Lanthanum, Cerium, Mercury, Lead, Thorium and Uranium. Only one of the samples contained no Nickel, Antimony and Lead; and Arsenic and Uranium were found in 2 samples. This study provided evidence of high toxicity of the IR brands, pointing out the need for better quality control of this product, in order to prevent health damage in dentists, prosthesis technicians and patients.

SINTESIS α-PINENE MENJADI α-TERPINEOL MENGGUNAKAN KATALIS H2SO4 DENGAN VARIASI SUHU REAKSI DAN VOLUME ETANOL

This study is intended to explore the optimum temperature reaction and volume of ethanol in the synthesis of α-pinene to α-terpineol. Turpentine oils that is used in this study contains α-pinene by 79.05%. In this study the variables used is the reaction temperature (60º, 70º, and 80ºC) and the volume of ethanol (105, 115, 125, 135 and 145 mL). Synthesis is done during 4 hours using a three-neck flask, condenser, hot plate, a magnetic stirrer, and a thermometer with a stirring speed of scale 7(350-700 rpm). After that, the results is neutralized to pH 7 using NaOH 5% then it is diluted with ethanol in 250 mL volumetric flask. Synthesized samples were analyzed by Gas Chromatography method. In this study, the highest concentration of α-terpineol obtained 57.05% with yield 67,79% at temperature reaction 70oC and the volume of ethanol is 135 mL.

Determination of Ergotamine Tartrate in Tablets by Liquid Chromatography with Fluorescence Detection

A method is presented for the liquid chromatographic (LC) determination of ergotamine tartrate in tablets that is applicable even in the presence of other ingredients such as phenobarbital, belladonna alkaloids, and caffeine. The sample is transferred to a volumetric flask, a small volume of formic acid is added to dissolve and stabilize the ergotamine, and the solution is diluted to volume with methanol. The solution is mixed and filtered through paper. The LC system consists of a Rheodyne injector fitted with a 20 μL loop and a C,18 reverse phase column; the mobile phase is acetonitrile-water-triethylamine (700 + 300 + 0.5). Ergotamine tartrate is determined fluorometrically at an excitation wavelength of 250 nm and an emission wavelength of 430 nm. Recovery studies were conducted at the 0.3 and 1.0 mg levels. Average recoveries were 99.6 and 100.8%, respectively; relative standard deviations (RSDs) were 1.08 and 2.21%, respectively. Some commercial preparations containing ergotamine tartrate in combination with other ingredients were also analyzed. The RSDs for 5 determinations of each of 2 ground composites were 0.09 and 0.34%.

Sampling of Insecticides from Pressurized Cans: Collaborative Study

Seven laboratories collaboratively studied 3 methods for sampling water-based insecticides in pressurized cans. Method 1 was a direct sampling method where the sample was collected continuously from an aerosol outlet into the solvent, using a U-shaped sampling assembly. Method 2 was an indirect method, in which the sample was collected in the solvent from an open can after the propellent was discharged under frozen conditions. Method 3 was an extension of Method 1, where ≥3 samples were collected continuously from an aerosol outlet into the solvent through a U-shaped sampling assembly. The solvent, which contained the active ingredient, was concentrated and transferred to a suitable volumetric flask for gasliquid chromatographic (GLC) analysis. The means of the analytical results for Methods 1 and 3 did not show a significant difference at the 95% confidence level. However, a significant difference was found at the 95% confidence level for the mean value for Method 2 compared with the means for Methods 1 and 3. Methods 1 and 3 have been adopted as official first action for sampling pressurized cans containing aerosols.