Method of extracting novocain from water solution
SUBSTANCE: method of Novocain extraction from water solutions includes the preparation of an aqueous salt solution of Novocain by its dissolution in a saturated solution of a salting-out agent, extraction and analysis of an equilibrium water phase, with the application as an extragent of a solvotrophic reagent solution in chloroform with the concentration of 10 wt %, for which purpose the aqueous salt solution of Novocain with pH 8.0±0.5 is prepared due to the application of a saturated ammonium sulphate solution as the salting-out agent and addition of an ammonium buffer solution, Novocain is extracted for 5-7 minutes with the solution of the solvotrophic reagent in chloroform with the ratio of volumes of the aqueous salt solution of Novocain and extragent of 5:1, then the aqueous saline phase is separated from the organic one and analysed by a method of UV-spectrophotometry at a wavelength of 291 nm, the concentration of Novocain in the water solution is found by means of a calibrating graph; the coefficient of distribution (D) and the degree of extraction (R, %) of Novocain is are calculated by formulae.
EFFECT: method for the extraction of Novocain from the water solution, which is characterised by expressiveness, makes it possible to realise the practically complete single extraction of Novocain from the aqueous salt solution and can be applied in the analysis of Novocain-containing water solutions.
The invention relates to analytical and pharmaceutical chemistry and can be used for the extraction of novocaine from aqueous media with the purpose of its further determination.
The closest in technical essence and the achieved effect is a method of extraction of novocaine from aqueous media with the use of chloroform without adding vicariates [Korenman Ya. I. distribution Coefficients of organic compounds. Guide. Voronezh: Publishing house of Voronezh state University. 1992. 336 p.]. The disadvantage of this method is the low distribution coefficient of novocaine (27,5) in the specified system.
The technical problem of the invention is to develop extraction systems with the aim of achieving a high coefficient of novocaine and almost complete extraction from aqueous solutions of chloroform with the use of allotropes reagent.
The technical result of the invention is to achieve a high distribution ratio of novocaine (up to 229,2), almost complete (98%) extract of novocaine from the aqueous solution with a solution of camphor in chloroform in the presence of ammonium sulfate.
Said technical result is achieved in that the extraction of novocaine from aqueous media involves the preparation of a solution of novocaine by dissolving in a saturated solution of vicariates, extraction and Ana�from the equilibrium water phase, the extractant solution using allotropes reagent in chloroform with a concentration of 10 wt. % why prepare a water-salt solution of novocaine with application as vicariates saturated solution of ammonium sulfate and add ammonia buffer solution, extracted with novocaine for 5-7 min with a solution allotropes reagent in chloroform in a volume ratio of water-salt solution of novocaine and extractant 5:1, separating the water-salt phase from the organic and analysed by UV-spectrophotometry at a wavelength of 291 nm, calibration chart to find the concentration of procaine in aqueous solution.
The implementation of the method is illustrated by the following example. Prepare a water-salt solution of novocaine, which has a pH of 8.0±0,5 due to the use as vicariates saturated solution of ammonium sulfate and add ammonia buffer solution, for which a portion of novocaine pharmacopoeial purity, taken on an analytical balance, placed in a chemical beaker 50 cm3was dissolved in a small volume (2-3 cm3) of distilled water, after complete dissolution of the sample (30-35 h) the solution was transferred to volumetric flask of 100 cm3, bring to mark with a saturated solution of ammonium sulfate, extracted with novocaine solution of camphor in chloroform, for this � received novocaine solution was added a solution of camphor in chloroform with a concentration of 10 wt. % when the volume ratio of water-salt solution of novocaine and extractant 5:1, is extracted on vibromaster before the establishment of the interfacial equilibrium (5-7 min). After stratifying system of water-salt phase is separated from the organic and analysed by UV-spectrophotometry. Measure the optical density of a water-salt solution on a UV spectrophotometer in a quartz cell with a thickness of the light-absorbing layer of 1 cm at a wavelength of 291 nm, build a calibration graph of optical density of water-salt solution from the concentration of novocaine, on schedule find the concentration of procaine in aqueous solution.
The distribution coefficient (D) and the degree of extraction of novocaine after extraction (R, %) is calculated according to the formulas:
where Caboutand Cin- concentration of novocaine in the organic and aqueous phases, µg/cm3; f - the ratio of the equilibrium volumes of aqueous and organic phases.
The organic phase is transferred 98% of novocaine from its original content in the analyzed solution, the distribution coefficient equal 229,2.
As you can see, the high distribution coefficient (229,2) and almost complete (98%) removal of novocaine solution of camphor in chloroform, when the volume ratio of water-salt solution and EXT�agent of 5:1 and use as vicariates of ammonium sulfate. The analysis duration 30-35 minutes.
When used as vysalivatel sodium chloride and lithium sulfate the degree of extraction of novocaine does not exceed 50% when the volume ratio of aqueous and organic phase is 10:1 and 15:1 the degree of recovery of less than 40%.
The proposed method of extraction of novocaine from aqueous media allows you to reach high values of distribution coefficient (up to 229,2) and almost complete (98%) extract of novocaine from water-salt solution, characterized by rapidity (analysis time 30-35 minutes) and can be applied in the analysis of aqueous media containing novocaine.
Method of extraction of novocaine from aqueous solutions, comprising preparing a water-salt solution of novocaine by dissolving in a saturated solution of vicariates, extraction and analysis of the equilibrium aqueous phase, characterized in that the extractant solution using allotropes reagent in chloroform with a concentration of 10 wt.%, why prepare a water-salt solution of novocaine with pH 8,0±0,5 due to the use as vicariates saturated solution of ammonium sulfate and add ammonia buffer solution, extracted with novocaine for 5-7 min with a solution allotropes reagent in chloroform in a volume ratio of water-salt solution of novocaine and extractant 5:1, further oteleuton-salt organic phase and analyzed by UV-spectrophotometry at a wavelength of 291 nm,
on the calibration chart to find the concentration of procaine in aqueous solution; calculate the distribution coefficient (D) and the degree of extraction (R, %) of novocaine by the formulas:
where Caboutand Cin- concentration of novocaine in the organic and aqueous phase after extraction, respectively, mg/cm3; f - the ratio of the equilibrium volumes of aqueous and organic phases.
SUBSTANCE: invention relates to analytical chemistry and can be used in a system for monitoring content of sodium thiosulphate in solutions. The method of determining sodium thiosulphate in solutions is characterised by adding an analysed sample into a reaction vessel containing a corresponding amount of photogenerated iodine, obtained by blowing with air for 1-2 minutes and irradiating the reaction mixture with a stabilised light source, the mixture consisting of 0.5 M potassium iodide solution, an acetate buffer solution with pH 5.6 and a sodium eosinate sensitising agent, by detecting change in current in a cell and upon achieving constant current, re-blowing the reaction mixture with air for 2-3 minutes and re-irradiating with the stabilised light source until achieving the initial amount of iodine in the vessel, measuring the iodine generation time spent on achieving the decrease thereof, determining the amount of sodium thiosulphate from a calibration curve from the change in current and generation time.
EFFECT: invention provides a simple method of determining sodium thiosulphate in solutions and avoids use of expensive equipment.
10 tbl, 5 dwg
SUBSTANCE: invention describes a method for lipoic acid measurement in biologically active additives by cathode voltammetry involving transferring a substance from a sample into a solution and taking voltammetric measurement; the cathode voltammetry is performed on a mercury-film electrode at potential -0.373 V of a relatively saturated silver-chloride electrode with borate buffer solution pH 9.18 at continuously current potential trace at 0.06 V/s with the determined lipoic acid content range from 4.5·106 to 1.1·10-3 mole/l.
EFFECT: improving sensitivity and expressivity of the method for measuring lipoic acid in tabletted BAAs by cathode voltammetry.
1 tbl, 1 ex, 3 dwg
SUBSTANCE: in agar plate which is in a Petri dish and inoculated with one of the fungal species of the genus Fusarium, circular holes are cut with the diameter of 8 mm, 0.05 ml of the working solution of the test preparation is applied into them, and placed in a thermostat at a temperature of 24.5-25.0°C, after 2-5 days depending on the type of fungus the diameter of the zone of growth inhibition of fungal mycelium is measured and the activity of the preparations is calculated according to the formula , and it is considered that when A=1 the fungicide is ineffective - the zone of growth inhibition is not formed (D=d), when A=2-3 the preparation activity is low, when A=4 it is average, and when A≥5 it is high.
EFFECT: invention provides accuracy of determining the activity of seed disinfectants and fungicides used in agricultural production.
SUBSTANCE: invention represents a method for preclinical study of cardiotropic antiarrhythmic drugs, involving determining the bioelectric parameters in isolated multicellular perfused preparations and measuring an action potential duration, differing by the fact that the isolated multicellular perfused preparations are presented by rat's pulmonary vein myocardium; the parameters are measured in three operation modes of the multicellular preparations; a resting potential is additionally measured; varying APD 90%, related APD 50%/APD 90%, a spontaneous shear velocity of the resting potential, the most positive membrane potential in the resting preparation, a spontaneous activity train repetition rate, spontaneous action potential train repetition and variability frequency, post-depolarisation number and intensity, as well as a shear membrane potential corresponding to the beginning of train activity are used to evaluate the signs of antiarrhythmic and arrhythmogenic action.
EFFECT: more reliable prediction of the antiarrhythmic action of the potential pharmacological agents and reduction of experimental phase time.
SUBSTANCE: invention relates to method of determining platelet resistance to acetylsalicylic acid (ASA) by impedance analysis of aggregation function of platelets in vivo, in which aggregation activity is analyses after incubation of biological material sample with ASA with application of aggregation inducer, and aggregation of platelets is induced by collagen in optimal concentration 2 mg/ml, and simultaneously with measurement of impedance determination of dynamics of platelet granules release is performed by luminescent method, where before carrying out aggregation samples are calibrated by means of adenosine triphosphate (ATP) standard, value of aggregation amplitude are determined in Ohms by obtained aggregatograms and obtained values are given points: values ≤6 correspond to 0 points, values 7-9 correspond to 1 point, values 10-12 correspond to 2 points, values >12 correspond to 3 points; after that, intensity of ATP release from platelet granules is determined in nmoles and obtained values are given points: values <0.5 correspond to 0 points, values 0.5-1.0 correspond to 1 point, values 1.0-1.5 correspond to 2 points, values 1.5 correspond to 3 points, and then resistance index (RI) is calculated by formula, value of IR parameter points to presence of aspirin-resistance of platelets.
EFFECT: carrying out fast complex diagnostics of platelet resistance to ASA with estimation of functional state of platelet granules before beginning treatment and possibility of preventing development of undesirable thrombotic or hemorrhagic complications.
2 dwg, 1 tbl, 2 ex
SUBSTANCE: claimed is application of fat emulsion for parenteral feeding as solvent for compounds which are poorly soluble in water. Fat emulsion contains in 1 l of solution: 30 g of refined soybean oil, 30 g of triglycerides with the average chain length, 25 g of olive refined oil, 15 g of purified fish oil.
EFFECT: obtaining solvent for compounds, poorly soluble in water, which makes it possible to determine parameters and spectrum of biological activity of novel compounds of chemical nature at the stages of pre-clinical and clinical tests, which does not change basic biological constants and possesses biological inertness.
2 tbl, 2 ex
SUBSTANCE: invention relates to biology, forensic and analytical chemistry and specifically to methods of determining procaine in blood plasma. The method comprises adding sodium fluoride to blood plasma containing procaine to achieve concentration of 10 mg/ml; treating the obtained mixture with acetone; separating the extract from the precipitate by filtering; evaporating acetone from the filtrate in an air current at room temperature; diluting the aqueous residue by adding water; saturating the obtained solution with ammonium sulphate; alkalising with an ammonium buffer solution to pH 9.0-9.5; extracting twice with portions of an organic extraction agent in the form of 30% camphor solution in methyl acetate, with ratio of the aqueous to the organic phase of 1:1 by volume; separating the organic extracts; combining; evaporating the solvent from the combined extract in an air current at room temperature; chromatographing the residue in a thin layer of silica gel STKH-1A on Sorbfil PTSKH-AF-A-UF plates, using a dichloromethane-ethanol mobile phase in ratio of 6:4 by volume; developing the chromatogram in UV light; eluting the analysed substance from the sorbent with a mixture of acetonitrile-methanol-0.025 M potassium dihydrogen phosphate solution with pH 3.0 in ratio of 10:10:90 by volume; chromatographing by HPLC method using a reversed-phase sorbent Nucleosil C18, a polar mobile phase acetonitrile-methanol-0.025 M potassium dihydrogen phosphate solution with pH 3.0 in ratio of 10:10:90 by volume and a UV detector; measuring optical density at wavelength 298 nm and calculating the amount of the analysed compound from the area of the chromatographic peak.
EFFECT: method improves sensitivity of determination.
3 tbl, 2 ex
SUBSTANCE: invention relates to analytical chemistry. The method is characterised by electrochemically concentrating benzoic acid on the surface of a graphite electrode for 90 s at electrolysis potential of (-0.500) V on a background of 0.1 mol/l sodium hydrogen phosphate, recording polarisation curves with linear potential sweep rate of 25 mV/s and determining concentration of benzoic acid from the peak height in potential range of 0.5-1.6 V relative to a silver chloride electrode.
EFFECT: method provides highly sensitive and rapid determination of benzoic acid in medicinal drugs.
3 ex, 6 tbl
SUBSTANCE: sample is applied on a paper filter, and standard calibration solutions of metronidazole in the concentration range of 10-100 mcl are radially applied on the same filter. The filter is processed with a developing agent containing 5% potassium hydroxide and acetone taken in ratio 2:1 and thermostated at 100°C until coloured spots are visible. A colour intensity of the sample spot is compared to the colour of the spot colour of the reference calibration solutions to determine the metronidazole concentration in the analysed sample.
EFFECT: method enables the fast and reliable monitoring of the metronidazole content and the timely correction of the therapeutic process.
SUBSTANCE: invention refers to medicine, namely to studying and analysing medical preparations, and can be used for standardising herbal raw materials. A method for identification and qualitative measurement of chlorophyll, carotinoids and hydroxycinnamic acids in a combination in great nettle leaves involves a 1-hour fractional extraction, 30 min each of the ground raw material having a particle size of 1.0 mm on a water bath at a temperature of 100°C with 70% ethanol in a ratio of the herbal raw material to the extractant of 1:100, the combination of the extracts and reduction to 100 ml with a solvent, dilution of the prepared solution in a ratio of 2:25 in 96% ethanol, measuring an optical density of the solution in relation to 96% ethanol at maximum absorption 328±1 nm, 442±1 nm and 667±1 nm, calculation of the total content of hydroxycinnamic acids equivalent to chlorogenic acid, carotinoids equivalent to violaxanthin and chlorophyll in the percentage equivalent to an absolute dry mass of the raw material by formulas.
EFFECT: method provides availability, simplicity, efficiency and low error of measurement.
3 dwg, 1 ex
SUBSTANCE: in order to extract iron (III) from water solutions diphenylguanidine (DPG) is applied as the first organic reagent. As the second organic reagent, salicylic acid (SA) is applied, and as solvent of organic phase chloroform is applied. In organic phase complex with molar component ratio DPG: Fe3+:SA, equal 1:1:1, is extracted. Process of iron (III) extraction is carried out at medium acidity pH=1.5-2.5 with the following detection of iron (III) by trimetric method.
EFFECT: invention makes it possible to increase selectivity and simplify process of extraction and detection of iron from water solutions.
2 cl, 5 dwg, 1 ex
SUBSTANCE: invention relates to method of purifying acidic salt solutions, in particular, those that are formed in complex processing of apatite with obtaining rare-earth metals concentrate (REM), from admixtures of phosphorus, fluorine and alkali metals. Method includes sedimentation of phosphorus, fluorine in form of phosphates and fluorides of calcium, and alkali metals in form of siliconfluorides, and before sedimentation of phosphates and fluorides of calcium and siliconfluorides of alkali metals acid is simultaneously with REM selectively extracted into organic extragent, with re-extraction of valuable component from organic extract, and after sedimentation of phosphates and fluorides of calcium and siliconfluorides of alkali metals acid is re-extracted from extract into water solution.
EFFECT: claimed method makes it possible to eliminate admixtures of phosphorus, fluoride and alkali metals, extract REM without loss and regenerate acid.
4 cl, 1 dwg, 4 ex
SUBSTANCE: invention relates to versions of composition for heat transmission. One of composition versions contains (i) from about 20 to about 90 wt % of R-1234yf; (ii) from about 10 to about 60 wt % of R-134a and (iii) from about 1 to about 20 wt % of R-32. Invention also relates to a number of versions of composition application.
EFFECT: composition has lower value of global warming potential and at the same time is characterised by productivity and energy efficiency.
56 cl, 7 dwg
FIELD: textiles, paper.
SUBSTANCE: invention relates to a multi-stage bubbling extractor and can be used in chemical, petrochemical, food, pharmaceutical and other industries. The multi-stage bubbling extractor comprises a vertical housing divided by partitions into sections-settlers with the mixing devices located inside, made in the form of two concentric pipes, the gas distribution nozzles with holes, nozzles for heavy fluid flow and overflow pipes for light fluid with holes. In each section-settler the outer pipe of the mixing device is mounted on the lower partition, and its upper edge is located at mid-height of the section-settler. The inner pipe of the mixing device is mounted with a gap to the lower partition, and in its upper end the holes are made for the gas discharge from the mixing device. The gas distribution nozzle is made in the form of an inverted cup with holes in the upper cover located above the lower edge of the inner pipe of the mixing device. The lower edge of the gas distribution nozzle is located below the holes for gas discharge from the mixing device of the underlying section-settler. In the web of the upper cover of the gas distribution nozzle concentrically to the mixing device the overflow pipe for light fluid is mounted, the lower edge of which is located below the holes for gas discharge from the mixing device of the underlying section-settler, and the holes in its upper part are located inside the nozzles for heavy fluid flow, the lower edge of which is located below the holes for gas discharge from the mixing device.
EFFECT: result is to increase technological capabilities of the extractor by using it for processing of fluid systems in which light fluid undergoes dispersion and heavy fluid is a continuous medium.
SUBSTANCE: method of obtaining vanadyl sulphate includes extraction from sulphuric acid of vanadium (IV) with undiluted di-2-ethylhexylphosphoric acid in the presence of sodium sulphate and further filtration under vacuum. Extraction is carried out with the ratio of water and organic phases equal (2.5÷3.0):1. After that, the organic phase is separated from the water phase, the organic phase is cooled to 0±0.5°C with an exposure at the said temperature for 20-30 min. After that, xylol is added to the organic phase with a ratio, equal to 1:(0.5÷1.0); the obtained product is washed with hexane.
EFFECT: invention makes it possible to increase the output of vanadyl sulphate trihydrate.
3 cl, 1 dwg, 4 ex
FIELD: process engineering.
SUBSTANCE: invention relates to fluid treatment. Proposed device comprises phase components feed and discharge means and tubular flow extraction chamber with fluid and carrier gas feed and discharge pipes. Extraction chamber is placed vertically in thermostat. It features hydrophilic inner surface and taper at top end aligned with capillary pipe so that a round slot is formed, or with funnel furnished with hollow cone secured so that a circular slot is formed between funnel surface and cone surface. Gas unions are arranged at acute angle to chamber axis while relative to chamber surface they are fitted tangentially. Method of extraction comprises feed of components into extraction chamber in countercurrent and discharge of carrier gas therefrom enriched in volatile components. Note here that tubular extraction chamber temperature is stabilised. Fluid flow forced into said chamber is converted into coaxial flow flowing over its concave surface in thin film while carrier gas flow is swirled in upward spiral. Mass exchange is executed at countercurrent of phase components or at stationary has phase.
EFFECT: increased extraction and higher sensitivity of analytic systems.
5 cl, 5 dwg
FIELD: process engineering.
SUBSTANCE: invention is intended for gas-fluid extraction. Proposed method comprises management of fluid and carrier gas flows, formation of phase interphase and mass exchange with subsequent separation of extracted fluid and carrier gas enriched in volatile components. Fluid axial flow incoming to the chamber is transformed into two coaxial flows separated by carrier gas. Extraction in analytical systems is carried in one step whereat fluid and gas phases migrate or in two steps. First, sample is forced via chamber at stationary gas phase normal or decreased pressure. Then, at concentration phase equilibrium, formed cloud saturated with volatile components of carrier gas vapour-gas mix is pushed from said chamber into analyser gas cell whereat carrier gas pressure equals barometric pressure. Device comprises flow-through tubular mass exchange chamber arranged vertically and having coaxial cavity with hydrophilic surface connected at top end with diverging coaxial slit.
EFFECT: higher degree of extraction, sensitivity and accuracy of these systems.
4 cl 7 dwg
FIELD: process engineering.
SUBSTANCE: invention can be used in radiochemical production for cleaning and separation of radioactive fluids, and in chemical, metallurgical and pharmaceutical industries. Rotary extractor comprises housing with mixing chamber, light phase discharge chamber and heavy phase discharge chamber with partition, rotor with separation chamber and conveying device, hydraulic lock and light phase discharge pipes and drive mounted at housing cover. Top part of heavy phase discharge chamber is equipped with the pocket secured to housing inner wall. Aforesaid partition arranged concentrically in gap between said pocket and drive is connected with housing cover. Partition bottom edge is located under pocket top edge while said cover is a turning design.
EFFECT: perfected design.
SUBSTANCE: method of mercury (II) extraction from chloride solutions includes extraction of mercury from a water phase into an organic component of a stratifying system water-antipyrine-organic acid. To provide quantitative concentration of mercury (II) in a hydrophobic melt of an organic phase of antipyrinum acetylsalicylate antipyrine and acetylsalicylic acid in a molar ratio 1:1 are used. In the course of the process heating on the water bath to a temperature of 90°C for 20-30 minutes, intensive shaking up and mixing are carried out. Sediment of the organic phase represents a mercury concentrate and can be used as an analytic sample.
EFFECT: invention makes it possible to reduce antipyrinum consumption.
1 dwg, 2 tbl
SUBSTANCE: extractor includes a vertical housing separated by partition walls into settling sections which are fitted with mixing devices in form of concentric inner, outer and cone-shaped pipes, gas-distribution nozzles with openings, mounted coaxial to the pipes, overflow pipes mounted in the partition walls. The upper edge of the cone-shaped pipe lies in the middle of the height of the settling section with spacing from the lower edge of the outer pipe. The inner pipe is placed with spacing from the lower partition wall. The upper edge of the gas-distributing nozzle lies higher than the lower edge of the inner pipe.
EFFECT: high efficiency of the extraction process.
FIELD: petrochemical industry; devices for a liquid by a liquid extraction.
SUBSTANCE: the invention is pertaining to the field of petrochemical industry, in particular, to a device for a liquid by a liquid extraction. The invention is dealt with a multiplate device for realization in a vertical column of multistage an extraction of a liquid by a liquid using a counterflow principle. The device contains: plates, and each plate after a fine setting in a column takes a horizontal position and is supplied with a seal ring, which adjoins the inside surface of the column; a perforated working area; a chordal up-going channel located on one side of a plate and a vertical bead retaining a liquid and surrounding the working area of the plate and spaced apart from the plate periphery closer to its center. The height of the upward directed bead is sufficient to retained a heavy liquid on a working area of the plate preventing is appearance on the edge of the plate, where a leakage downwards is possible because of availability of a gap between the edge of the plate and then inside surface of the wall of the column. The invention ensures more efficient prevention of the heavy liquid leakages through the tightness along the edge of the plate.
EFFECT: the invention ensures more efficient prevention of the heavy liquids leakages through the sealing-in along the edge of the plate.
6 cl, 5 dwg