The method of analysis of liquid preparations based on vegetable raw materials
(57) Abstract:Use: the method can be used for analysis of multicomponent elixirs, balms, tinctures, and other dosage forms based on vegetable raw materials. The inventive method of analysis of liquid preparations based on vegetable raw materials includes removing the volatiles by distillation of the original sample with steam and their subsequent determination by GLC, and after removing volatiles spend their concentration by extraction with an organic solvent having a boiling point not more than 60oC, for example diethyl ether, followed by dehydration using a chemical agent resulting extract and its evaporation at a temperature not exceeding 70oC to stop the distillation of solvent vapours. The operation of the concentration of volatile substances is carried out to reduce the amount of leaf concentrate in relation to the volume of the original sample, at least 100 times. 1 C. p. F.-ly. The invention relates to the field of analytical chemistry and can be used for analysis of multicomponent elixirs, balms, tinctures and other liquid dosage forms based on vegetable raw materials, such as, for Oprea chemistry has a large Arsenal of physico-chemical methods, to allow the analysis of complex multicomponent mixtures. For the identification of trace substances present in the analyzed mixtures are the most convenient methods of chromatography.However, application of these methods, in particular, for analysis of extracts from vegetable raw materials is limited by the inability in most cases to carry out a direct analysis of the components of mixtures by chromatography and requires the preliminary preparation of the sample for analysis.While there are no universal methods of analysis, and each time you must select the specific techniques of sample preparation.The known method of gas chromatographic analysis of heterogeneous multicomponent liquid compositions  including the selection of the initial sample, the introduction of solvent or solvent mixture, separating nerastvorimaya part of the sample, the introduction of secondary samples in the form of a solution in the node input chromatograph, gas chromatographic separation and analysis of volatile components.The disadvantage of this method is the use of solvents, which leads to loss of sensitivity analysis due to the large dilution and introduction to the sample of volatile components, the attraction of volatile components in organic solvents and kontsentrirovanie defined components by passing them through the cartridge with a reversed-phase sorbent, and their subsequent determination by chromatography.However, application of this method is limited due to the narrow specificity of the sorbent used and the complexity of the analysis of preparations containing a wide range of volatile compounds.In addition, in this method is the loss of part of the designated component as a result of their binding to the sorbent, which is critical at very low concentrations of the compounds included in the composition of the analyzed extracts.Closest to the claimed is a method of analysis of oil extracts from vegetable raw materials with the addition of camphor and essential oils (the "Viton"), which is selected as a prototype 
The method includes removing the volatile components by distillation of the original sample with water vapor and their subsequent determination by the method of gas-liquid chromatography (GLC). The content of volatile components in the composition of the essential oils judge the authenticity of the analyzed drug.However, this method is applicable for determining the authenticity of herbal extracts on the content of volatile components at relatively high concentrations.Task C other liquid medicines based on vegetable raw materials with a low content of ingredients by identifying a wide range of characteristic volatile substances.The essence of the invention is that the method of analysis of extracts from plant material includes removing the volatiles by distillation of the original sample with water vapor and their subsequent determination by GLC, and after removing volatiles spend their concentration by extraction with an organic solvent having a boiling point not more than 60oC followed by dehydration using a chemical agent resulting extract and its evaporation at a temperature not exceeding 70oC to stop the distillation, solvent vapor, and the operation of the concentration of volatile substances is carried out to reduce the amount of leaf concentrate in relation to the volume of the original sample at least 100 times.A particular case of the use of an organic solvent for extraction is the use of diethyl ether.New in comparison with the prototype is that after removing volatiles spend their concentration by extraction with an organic solvent having a boiling point not more than 60oC, followed by dehydration using a chemical agent resulting extract and its evaporation at a temperature not Bo is carried out to reduce the amount of leaf concentrate in relation to the volume of the original sample, at least 100 times.Also new is that for the extraction of the analyzed substances using diethyl ether.Removing the volatile substances from the analyzed extract distillation method of the original sample with water vapor allows you to select a wide range of characteristic substances to facilitate their subsequent separation and identification by GLC.For using the GC for analysis of the extracts with a low content of the investigated components carry out the concentration of the extracted volatiles.Conduct the concentration of volatile substances by extraction with an organic solvent, followed by dehydration using a chemical agent obtained extraction and evaporation before the termination of the distillation vapors of the solvent provides the transfer of volatile substances in the final concentrate.When this extraction with an organic solvent having a boiling point not more than 60oC and carrying out the evaporation at a temperature not exceeding 70oC to stop the distillation of solvent vapours provide a soft, gentle concentration process, which eliminates loss substances.
="ptx2">Operations concentration to reduce the amount of leaf concentrate in relation to the volume of the original sample, at least 100 times allows you to reach the level concentrations for each of the defined volatile substances to the detection limit of the GLC.The method is as follows.Selected for the analysis of the original sample extract is placed in a distillation flask equipped downward fridge, add equal amount of water, bring the mixture to boiling and distilled, the distillate.Next, carry out the concentration determined volatile substances.The resulting distillate is placed in a separating funnel and extracted with an organic solvent having a boiling point of no more than 60oC, for example, diethyl ether.In the case of the analysis of hydro-alcoholic extracts suitable after organic extraction solution before drying and evaporation to wash the resulting extract to remove the alcohol.Next, the resulting extract dehydrated chemical agent, such as anhydrous sodium sulfate.Then, the sample is transferred into a flask with reflux condenser and evaporated on a water bath of this series of operations the concentration of volatile substances, the volume of concentrate relative to the volume of the original sample was reduced to less than 100 times, repeat the cycle of operations concentration until then, until it reaches the desired ratio of these volumes.Next, perform a GC analysis of the obtained concentrate volatile compounds by known methods.Examples of the method.Example 1.Carried out analysis of the elixir, which is an aqueous-alcohol extract of a mixture of 24 species of medicinal plant raw materials with the addition of Apple juice, honey, caramel and sugar syrup, to determine its authenticity on the composition of the volatile fraction.The study elixir contains the following herbal ingredients: fruit of the Siberian cedar, bilberry leaf, rhizome and roots of Rhodiola rosea, wild rose hips, the fruit of the black chokeberry, rhizome licorice, chamomile flowers, herb oregano, bearberry leaf, fruit cherry, rhizomes with roots of Siberian ginseng, herbs St. John's wort flowers of the hawthorn, hawthorn, sage leaves, plantain leaves, yarrow herb, rhizome with the roots of Rhaponticum safrolovidnaya, the roots of tormentil, the fruits of coriander seed, chaga, herb wormwood, the roots of the peony.A number of these herbal ingredients in the study elixir of sostavlyalo and water to 1000 ml.For the specified elixir criterion of authenticity is the presence of the following substances in the volatile fraction of this drug: cineole, linalool, camphor, benzoic acid, cinnamic aldehyde, cinnamic alcohol, eugenol, palmitic acid, ethyllinoleate and esters of high molecular weight saturated alcohols, the number of which shall not be less than five.For the analysis took 100 ml of elixir, was added 100 ml of water and boil the mixture for 1 hour.Received 120 ml of distillate (solution A).100 ml of solution And successively was extracted with diethyl ether three portions of 50 ml each.The combined extract washed twice with distilled water (100 ml each to remove the alcohol, and then the combined extract were dried for 2 hours over 30 g of anhydrous Na2SO4.Then dehydrated extract was transferred into a flask and evaporated on a water bath at a temperature of 50-55oC before the termination of the distillation vapor diethyl ether, the volume of residue in the flask was 3 ml, which corresponded to the reduction of the volume of the original sample is approximately 30 times.Continued the process of concentration.To the resulting ostogo ether in 10 ml.The combined ether extract was dried over 1 g anhydrous Na2SO4for 15 minutes and then was evaporated as described above until the volume in the flask to about 0.3 ml, which corresponded to the reduction of the volume of the original sample is approximately 300 times.Obtained as a thick oil concentrate was diluted with 0.1 ml of a mixture of chloroform and ethanol, taken in the ratio 1:1 (solution B).100 μl of solution B was chromatographically on a column length of 2 m with an inner diameter of 2 mm using a stationary phase 15% rubber stamps SE-30 and SE-50 on the media Chromaton N-AWDMCS when programming the temperature of the column from the 50oC to 300oC with the speed of temperature rise of 5oC / minute at a temperature of evaporator 300oc, the speed of the carrier gas (helium) 25 ml/min, detector-flame ionization.The relative retention times were measured relative to the benchmark.On the chromatogram peaks were identified all of the characteristics of the substances selected as the criterion of authenticity, which allowed us to judge the authenticity of the investigated elixir.Example 2.Carried out analysis of the elixir, which is an aqueous-alcohol extract of a mixture of 17 species Lek is ing its authenticity on the composition of the volatile fraction.The study elixir contain the following herbal ingredients: pine nuts, blueberry, herb St. John's wort, licorice roots, yarrow herb, peppermint leaves, rhizome tormentil, kidney birch, hawthorn fruit, herb oregano, coriander fruit seed, rose hips, ginseng root, oak bark, rhizome bergenia, rhizome of calamus, chamomile flowers.A number of these herbal ingredients in the elixir ranged from 0.01 g up to 5.17 g per 1 l of the drug.In addition, the elixir contained ethyl alcohol 96% in an amount of about 400 ml, and water to make 1000 ml.For this elixir criterion of authenticity is the presence in the volatile fraction of the following characteristic substances: 1,1-Dimethyl-4-isopropylcyclohexane, 1,2-Dimethyl-4-isopropylcyclohexane, Menten, menthol, salicylic acid, benzoic acid, - terpinen, n-cineol, cinnamic alcohol, camphor, borneol, thymol, methyl ether of eugenol, eugenol, azaron, caryophyllene, Betulinol, betulin, stearic acid, tetradecylphosphonic, abietic acid, ethyllinoleate, tetrazacyclooctane, serpelloni, tetrachromat, heptadecenoic, octadecylammonium, nonacetylated, mirelly alcohol.Made of solvent for the operation of extraction of volatile compounds from the distillate used dichloromethane.On the chromatogram were identified by characteristic peaks of all the substances selected as the criterion of authenticity, which allowed to make a conclusion about the authenticity of the investigated elixir.It should be noted that the proposed method allows for the standardization of multicomponent liquid dosage forms such as elixirs, balms with an extremely wide variety of herbal ingredients at low contents, including the necessary supplements (Kohler, sugar, honey), which was impossible previously known methods.Sources of information taken into account
1. Jennigs Century RAPP A. sample Preparation for gas chromatographic analysis. M. Mir, 1986, S. 73-77.2. Auth.mon. USSR N 1704065, CL G 01 N 30/06, publ. 1992.3. Problems of standardization and quality control of drugs. Materials of all-Union conference under the General editorship of C. A. Severtsev, M. 1991, so 2, PM 1, S. 33. 1. The method of analysis of liquid medicinal preparations based on vegetable raw materials, including removing the volatiles by distillation of the original sample with water vapor and their subsequent determination by GLC, characterized in that the extracted after the boil no more than 60oC, followed by dehydration using a chemical agent resulting extract and its evaporation at a temperature not exceeding 70oTo stop the distillation, solvent vapor, and the operation of the concentration of volatile substances is carried out to reduce the amount of leaf concentrate in relation to the volume of the original sample at least 100 times.2. The method according to p. 1, characterized in that the extraction of the analyzed substances using diethyl ether.
FIELD: chemical technology.
SUBSTANCE: invention relates to a method for synthesis of ester perfluorinated derivative by using a chemical reaction. This reaction represents the fluorination reaction of the parent compound as a raw, the reaction of chemical conversion of fragment of ester perfluorinated derivative to yield another ester perfluorinated derivative or the interaction reaction of carboxylic acid with alcohol under condition that at least one or reagent, i. e. carboxylic acid or alcohol, represents a perfluorinated compound wherein indicated perfluorinated derivative of ester represents a compound comprising a fragment of the formula (1):
with a boiling point 400°C, not above. The reaction time for carrying out abovementioned chemical reaction is sufficient to provide the required yield of ester perfluorinated derivative and wherein this yield of ester perfluorinated compound is determined by the gas chromatography method by using a nonpolar column. Also, invention relates to a method for pyrolysis of ester perfluorinated derivative with a boiling point 400°C, not above, to yield the dissociation product wherein this product represents a derivative of acyl fluoride or ketone and wherein pyrolysis time is sufficient to provide the required degree of conversion of ester perfluorinated derivative and wherein the indicated conversion degree of ester perfluorinated derivative is determined by gas chromatography method by using a nonpolar column. Also, invention relates to a method for analysis of ester perfluorinated derivative with a boiling point 400°C, not above, that involves analysis of ester perfluorinated derivative in a sample containing ester perfluorinated derivative by gas chromatography method by using a nonpolar column wherein ester perfluorinated derivative represents compound comprising a fragment of above given formula (1).
EFFECT: improved method of synthesis.
8 cl, 1 dwg, 2 ex
FIELD: instrument engineering.
SUBSTANCE: device for generating flow of vapor-gas mixture with preset concentration of vapor has vessel partially filled with fluid, second vessel provided with branch pipes for supply and removal of gas, and vapors of fluid pipeline-leak. One of vessels is connected with gas discharge forcer; fluid vapors pipeline-leak connects both vessels. Vessel, partially filled with fluid, is mounted inside second vessel. Pipeline-line, connecting both vessels, is totally placed inside second vessel. Device is also provided with additional discharge forcer for adjusting concentration of fluid vapor in second vessel. Granulated filler is introduced into vessel partially filled with fluid. Device is also provided with gas analyzer for providing gas concentration in space of second vessel.
EFFECT: higher precision of keeping of preset concentration of vapor; improved efficiency of vapor concentration control and adjustment.
FIELD: instrument engineering.
SUBSTANCE: invention is designed for calibrating gas analyser detectors, according to which there prepared is calibration substance solution with concentration A=By/k (%) as per Henry constant value k (mg/m %) at calibration temperature and as per the specified value of calibration substance mass concentration in calibration steam/gas mixture By (mg/m). After the solution has been introduced into the vessel in quantity enough for fully saturated equilibrium calibration steam/gas mixture to appear above the solution surface, the sensor calibration is carried out by means of mixture; at that, mixture concentration is changed by means of direct proportional change of solution concentration by diluting concentrated reference solution of calibration substance with analytical accuracy up to the specified concentration value A (%). There also proposed is the device for realising this method, which includes a solution point for preparing calibration solution with analytical accuracy, vessel with thermostatic device for obtaining steam/gas mixture with constant concentration corresponding to Henry law; at that, solution point includes graduated dose metre, graduated diluter, mixer with a reducer, capacity with solvent, and reference container with reference solution, which is stabilised with a gate valve meant for multiple use of container, and vessel with thermostatic device consists of thermometre and heat-insulating cover plate with an inlet branch pipe containing a normally closed return valve and a pusher for valve opening.
EFFECT: decrease of calibration substance losses; accuracy and reproducibility of metrological performance, and meeting requirements of industrial and ecological safety.
6 cl, 2 dwg
SUBSTANCE: vapour-gas mixture source has a mixer which has connecting pieces for inlet and outlet of the vapour-gas mixture. The vapour-gas mixture source also has a diffusion pipe filled with working fluid and an auxiliary pipe designed for filling the diffusion pipe with working fluid. Part of the diffusion pipe is filled with substance which retains the working fluid. The level of working fluid in the auxiliary pipe is lower than the level of substance in the diffusion pipe. The substance which retains the working fluid used can be sand, granular material with particle size between 10 and 10000 mcm, porous substances, e.g. ceramic metal etc.
EFFECT: more accurate measurement and maintenance of concentration of the vapour-gas mixture coming out of the source, provision for constant diffusion flow of vapour of working fluid into the mixer.
11 cl, 2 dwg
SUBSTANCE: invention relates to laboratory methods of analysis and deals with method of quantitative determination of manganese, lead and nickel in bile by method of atomic-absorption analysis with atomisation in flame. Essence of method lies in the following: sampling of bile is carried out during duodenal probing, after that it is frozen, and unfrozen at room temperature, homogenisation of bile by mixing being performed already at partial soft unfreezing. After that, sampling of homogenised bile is carried out for preparation for analysis, concentrated nitric acid is introduced into it with volume ratio 1:1, mixture is kept at room temperature, then heated and further mixture is kept for not less than 2.5 hours at room temperature. In order to obtain analyte, to obtained mixture added is concentrated hydrogen peroxide in volume ratio 1:1 to volume of bile sample volume, analyte is heated, after that cooled to room temperature. After that by method of atomic-absorption spectrometry, using graduated diagram, quantitative content of particular type of metal: manganese, lead and nickel is determined in analyte.
EFFECT: invention allows increasing accuracy of quantitative determination of manganese, lead and nickel in bile.
FIELD: engines and pumps.
SUBSTANCE: proposed method is based on application of simplified model of intake of admixtures into cabin which allows for only oil decomposition products in gas turbine engine. Major portion of air samples, 95-97%, required for identification and quantitative determination of oil decomposition products, is sampled on surface from device simulating oil decomposition conditions including air temperature and pressure at point of sampling from engine compressor, and oil stay time in hot zone.
EFFECT: decreased time of in-flight experiments and that of surface analysis of samples.
1 cl, 1 ex, 1 tbl, 1 dwg
SUBSTANCE: invention relates to analytical chemistry, particularly to methods of determining benzoic acid, and describes a method for quantitative determination of benzoic acid from a methyl derivative thereof - methyl ether in aqueous matrices with determination sensitivity of 5.0·10-5 mg/cm3 with determination error of not more than 25%. The method is characterised by that quantitative determination of benzoic acid is carried out using a chromatographic method with flame-ionisation detection and includes the following steps: extraction concentration of an analyte with benzene in water samples acidified with 25% sulphuric acid solution to pH 1-3 while adding sodium chloride until a saturated solution is obtained, conducting a benzoic acid methylation reaction with diazomethane to obtain a derivative - methyl ether of benzoic acid and determining the formed methyl ether of benzoic acid by a chromatographic method with flame-ionisation detection.
EFFECT: method provides high sensitivity, selectivity and easy implementation during quantitative determination of benzoic acid in aqueous media and enables use thereof in practice in factory analytical laboratories, central laboratories of chemical companies and chemical-toxicology laboratories.
1 ex, 3 tbl
SUBSTANCE: device for preparing control gas mixtures comprises a gas mixer, at least one channel for supplying target gas to the gas mixer, at least two channels for supplying the diluent gas to the gas mixer, and the channel for output of the gas mixture from the gas mixer. And in each channel for supplying gas to the gas mixer the mass flow controller of gas and a solenoid valve are mounted successively, at least in one channel for supplying the diluent gas to the gas mixer the gas humidifier and the solenoid valve are mounted successively. In each of the channels equipped with the gas humidifier at least one bypass pipeline with the additional solenoid valve is mounted. and the output of the gas flow controller of this channel is connected to the input of the additional pipeline which output is connected to the output of the last solenoid valve, and at the input of the target gas and the input of the diluent gas at least one filter is mounted, which outputs are connected to the inputs of manually operated valves.
EFFECT: possibility of operational automated obtaining the dry or moist gas mixture, and reliable obtaining of the given values of concentrations of gas mixtures at the output of the device.
SUBSTANCE: each blood sample is analysed twice. A fresh blood sample is centrifuged at 2,000 rpm for 5 min. The samples are separated in plasma fractions and formed elements. A solid-phase plasma extraction is performed by sequential passing of 100% acetonitrile, plasma, distilled water, 50% acetonitrile solution under vacuum through a cartridge with Oasis HLB 3 cc sorbent. The cartridge with the sorbent is dried under vacuum, and 100% methylene chloride is passed through the sorbent. An aliquot portion of the produced extract is chromatographed. Producing the extract of formed elements is ensured by dispersed solid-phase extraction: by adding 100% acetonitrile thereto and agitating intensively. That is followed by adding a number of QuECHeRS salts for extraction, agitating, centrifuging for 10 minutes at 2,000 rpm; that is accompanying by forming 3 layers; an upper layer is transferred to another test tube, which contains a number of QuECHeRS salts for purification; the layers are centrifuged at 2,000 rpm; the upper layer is sampled. Plasma and formed elements extracts are analysed by Agilent 1200 liquid chromatograph with a fluorimetric detector on Zorbax column 50 mm long and having an inner diameter of 4.6 mm with Eclipse PAH C18 sorbent at column temperature 27°C; a movable phase is presented by mixed acetonitrile and water at flow rate 1.5 cm3/min and optimising elution in the gradient mode (supplying the movable phase of 60 vl % to 68 vl % of acetonitrile for 1 min, increasing 60 vl % to 68 vl % of acetonitrile for 3 min, increasing 68 vl % to 70 vl % for 0.5 min, increasing acetonitrile 70 vl % to 90 vl % for 1.5 min, increasing acetonitrile 90 vl % to 100 vl % for 4.5 min, supplying 100% acetonitrile for 1.5 min, reducing acetonitrile to 60 vl % and supplying 60% acetonitrile for 4 min to balance the column). An excitation wavelength of the fluorimetric detector makes 265 nm, and an emission wavelength makes 412 nm. A calibration chart is used to quantify benz(a)pyrene in plasma and formed elements separately, while the results are summed up.
EFFECT: invention provides high sensitivity of the method and ensures selectivity in a combination with its accessibility for routine analyses.
3 cl, 6 tbl, 1 ex
SUBSTANCE: invention relates to medicine, namely to experimental pharmacology, and can be used for quantitative determination of carnosine in tissues and physiological liquids. Determination of carnosine in biological materials is carried out by highly-selective mass spectrometry method using electrospray ionization. At that, deproteinization of blood plasma should be preliminary carried out using 10 % aqueous solution of trichloroacetic acid. Then aliquot of internal standard solution of L-alanyl-carnosine is added to deproteinizated sample. And separation of extraction products is performed at reversed-phase chromatographic column 4.6×150 mm with temperature separation of 35 °C and eluent feed rate 0.7 ml/min. Used eluent is 10 mM ammonium acetate, acidified with glacial acetic acid to pH 3.7, and mixture of acetonitrile with 10 mM ammonium acetate in ratio of 90:10, taken in ratio of 10:90, respectively. Detection of carnosine is carried out by four child ions with m/z 110.0, 156.1, 180.0, 210.1, formed as result of molecular ion carnosine disintegration with m/z 227.1. Concentration of carnosine is calculated by chromatographic peak carnosine area relation to L-alanyl-carnosine internal standard peak area.
EFFECT: invention provides highly selective and sensitive gas chromatography/mass-spectrometric method for quantitative determination of carnosine in biological substrates.
1 cl, 6 dwg, 2 tbl, 1 ex