Method of authenticating medicinal plant raw material and apparatus for realising said method

FIELD: physics.

SUBSTANCE: sample of medicinal plant raw material is held for 40 minutes at 100°C. Components of the equilibrium vapour phase are analysed on a standard column. Interpolation characteristics of sorbates are then determined, and the input of equilibrium vapour phase samples and n-alkanes is synchronised based on a signal from the detector on part of the discharge line of the divider of the sample input unit. The apparatus has a sampling valve, a heated vessel for analysed samples and a sample input unit with a flow divider. The apparatus also has a capillary column, a detector connected through a constant fluidic resistor with the discharge line of the divider, an analysis programming unit and an additional amplifier for the detector signal, which generates a start command for the analysis programming unit.

EFFECT: high accuracy while standardising and improving precision of measurements under repeatability conditions.

2 cl, 1 dwg

 

The invention relates to gas chromatography and can be used to standardize and evaluate the authenticity of various pharmaceutical raw materials in medicine, pharmacology, health care, food, perfumery and other industries.

Known methods and devices for standardization of medicinal plants (herbal drugs and phytopharmaceuticals (AF) based on them, based on the determination of biologically active compounds (BASS) and standard samples comparison (WITH) using various types of chromatography and UV spectroscopy. These methods allow you to quickly and reliably assess the quality of raw materials on top of the BASS. In this case, as a rule, do not use the additional stage of treatment, which increases the analysis time and leading to an inevitable loss of part of the investigated substances (see: the Industry standard of Ministry of health of the Russian Federation OST. 91500.05.001-00. The quality standards of medicines. The main provisions. - An introd. 01.01.01. - 2000. - 12 S.).

Known as methods of standardization of herbal drugs, biologically active additives (BAA) and various OP (see: Kurkin V.A. Pharmacognosy. The tutorial. 2nd ed., added; and extra - Samara LLC "Etching". GOU VPO Samara state medical University, 2007 - 1239 S.).

To determine the authenticity of the LRS and the OP also use so-called "fingerprints", in which the chromatogram appreciate not separate classes and the individual is property of matter, and the totality of the BASS (see, for example, Tereshina NS, Abramov A.A., Margaryan A. Analysis of homeopathic medicines barberry chromatographic methods. // Vestnik MGU. Ser. 2. Chemistry, 2006. - 47 so. No. 5. - S-349.)

However, the known methods of determining the authenticity LRS do not provide a direct analysis of the BASS directly into the LRS, and require pre-cooked preparations, for example, essential oils, tinctures, extracts, teas, etc.

The closest to the invention by the combination of essential features is the way of standardization of polymers "fingerprint" in the form of a set of program products of their pyrolysis, in which a fixed number of crushed analyzed raw material is placed in a heated sealed vessel is maintained at a given temperature, the pyrolysis products are batched in a chromatographic column, measured value signal and the retention time for identification and standardization of polymers (see: Berezkin V.G., Eliseev V.R., Nemirovskaya IN Gas chromatography in chemistry of polymers. - M.: Nauka, 1972 - 283 S.)

The disadvantages of this method is the low reliability in the standardization of herbal drugs and the bad convergence of the analysis.

The closest to the invention by the combination of essential features is a gas chromatograph Color-100, provided the pyrolytic console tap-dispenser, the node of the input samples with the evaporator and the flow divider, the capillary column and a flame ionization detector (see: Eliseev V.R., V.G. Berezkin, pancakes A.S., Kolmanovskii placing V.N., Yashin YA and other Pyrolytic device for gas chromatography. Auth. mon. The USSR №284418 from 14.10.1970. // Bull. Fig. No. 32, 1970, see also: Technical description and operating instructions on the chromatograph series Color-100". Specifications TO).

A disadvantage of the known device for evaluating the authenticity of herbal drugs is the increased accuracy in the determination of the interpolation characteristics for qualitative and quantitative analysis of the components of the RPF, as the external standard homologues of n-alkanes is injected by syringe into the node of input samples with the evaporator, and the components RPF in line with the carrier gas tap-dispenser, resulting in the beginning of the two analyses, a fixed torque input samples differ from each other.

The objective of the invention is to increase the reliability in the standardization of herbal drugs and the improvement of the convergence analysis in terms of the frequency of occurrence.

This problem is solved due to the fact that the way to assess the authenticity of medicinal plants, in which a fixed number of investigated sample is placed in a sealed vessel, maintained at a given temperature, the components of the equilibrium vapor phase on serout in a chromatographic column, measured value signal and the retention time, wherein the sample is kept in a sealed vessel at 100°C for 40 minutes, the components of the equilibrium vapor phase will be analyzed by standard capillary column with a node of the input samples with a flow divider in a linear programming temperature, the output signals of the components of the equilibrium vapor phase compared with the signals of external standards homologues of n-alkanes to calculate the interpolation characteristics of the solutes, and the synchronization time of the input of the analyzed samples are carried out by the signal detector to a fixed part of the flow from the discharge line of the divider node of the input samples.

This problem can be solved also due to the fact that the device for evaluating the authenticity of medicinal plant raw materials containing preparation unit gas, tap-dispenser, heated sealed vessel for the studied samples, the node input samples with flow divider, capillary column, detector and software analysis, characterized in that the input of the detector is connected with the tee as with the exit of the capillary column and the vent line of the flow divider node of the input samples through a permanent pneumatic resistance and the measuring circuit of the detector is provided with an additional amplifier connected to the programmer analysis.

When the solution set is military tasks created technical result which are as follows:

1. Higher confidence in the standardization of herbal drugs by creating a reference data banks in the form of a "fingerprint" for different LRS. Reference banks contain a set of retention indices in linear programming temperature columnand quantitative information in the form of concentrations of components RPF (Cicalculated according to the relative output signals using the dual internal standard. Standardization and evaluation of the authenticity of the investigated LRS is to confirm together receivedand Ciaccording to published data Bank.

2. Improving the precision of analysis results in terms of repeatability (precision of measurement), which is achieved by use of the interpolation output signals for qualitative and quantitative analysis of herbal drugs.

This allows us to conclude that the claimed invention are connected by a single inventive concept.

The invention is illustrated in the drawing. Figure 1 schematically shows a device for evaluating the authenticity of medicinal plants, which includes the preparation unit gas 1, tap-dispenser 2, the pressurized heated vessel for samples 3, node of the input samples with flow divider 4, the capillary quartz is the third column 5 firm Varian type VF-1 (length 30 m, the internal diameter 0.32 mm, film thickness of 0.5 µl), the detector 6, an additional amplifier 7, programmer analysis of 8 and a constant pneumatic resistance 9.

The system for assessing the authenticity of medicinal plants is as follows: 5 g of crushed LRS put heated in a sealed vessel 3 and heated to 100°C. Crane dispenser 2 at this time is set to "analysis" (solid lines), and the carrier gas is nitrogen supplied to the input node of the sample 4, column 5 and the detector 6. LRS is kept in a vessel 340 minutes and crane dispenser switch to "set" (dotted line), the carrier gas sweeps the components of the RPF from the vessel 3 in column 5. The operation time is set to 30 seconds, after which faucet-spout again switch to position "analysis". The separation of components of the RPF carried out in the regime of linear temperature programming of the column. The initial column temperature of 40°C, heating rate 5°C/min Final temperature of 180°C. the Total analysis time of 40 minutes. The division of the flow at the inlet to column 1:40, the flow of carrier gas in the column of 1 cm3/min. the Beginning of each analysis is synchronized programmer analysis 8 by the signal detector 6 via the auxiliary amplifier from a fixed portion of the flow from the discharge line of the flow divider node of input sample 4.

To determine the interpolation output signals in the qualitative and the quantitative analysis of the components of the RPF as the external standards used homologues of n-alkanes (from hexane to hexadecane), the mixture which is metered by microprism 0.5 ál to the input node of the sample 4, the evaporator temperature 250°C.

According to the results of gas chromatographic analysis of the components of the RPF and mixtures of n-alkanes expect the following characteristics:

1. The retention times of the solutes RPF and homologues of n-alkanesandrespectively, where z is the number of carbon atoms in the molecule n-alkane.

2. The retention indices of the components of the RPF in linear programming the temperature of the column.

3. The normalized output signals to components RPFand for homologues of n-alkanes.

where yCR- chromatographic output signal from the discharge line of the flow divider is proportional to the sample volume; yiand yz- output signals of the components of the RPF and n-alkanes, respectively.

4. The concentration of the components RPF using the dual internal standard.

where Czand Cz+1the concentration of n-alkanes in the analyzed mixture.

5. Root mean square deviation (RMS) average of the measurements.

wherefor the proposed method;

x=yi- proceed. of the STN method;

n - number of measurements.

6. The relative standard deviation of the arithmetic mean of the measurements in %.

7. Limit of confidence interval in %.

8. The accuracy of measuring the concentration of a model mixture in %.

where Ciis measured by the equation (3) concentration using the output signal, yi(for a known way) and(the proposed method); (CEastthe true concentration in the mixture model, calculated by the procedure of preparation by weighing the components of the mixture on an analytical balance.

In the known method a portion of powdered herbal drugs are placed in a pyrolytic console, maintained at a temperature of 800°C, and the products of pyrolysis chromatographic and get a set of output signals (- retention time and Qi- the area of the chromatographic peak) in the form of a "fingerprint".

The experiments were conducted using the following LRS: peppermint leaves, grass, tarragon, St. John's wort herb and fruit, milk Thistle.

The correctness and precision of the measurements was assessed by the results of the analysis of model binary mixture of n-alkanes (decane - 35 wt.%, and undecane - 65 wt.%). The number of measurements n=5. The mixture is hotovely gravimetric method by weighing components on an analytical balance of POWER-200.

The results of the experiments are summarized in table Comparative data experimental verification of known and proposed methods.

Table 1
Comparative data experimental verification of known and proposed methods
№ p/pNameThe known methodThe proposed method
n-decanen-undecanen-decanen-undecane
1.The average value of the output signal, (2)
- absolute, yimV·7201275--
normalized,--0,3430,607
2.The relative standard deviation, Sr, %, (5)a 3.94,11,61,7
3.Limit of confidence interval, ±Δ, %, (6)10,811,44,4the 4.7
4.The accuracy of measuring the concentration of the mixture model, δ, %, (7)6,15,82,52,4
5.Analysis of the LRS for the standardization and evaluation of authenticityThe combination of the output signals "fingerprints"
Retention time, minIndex holding, (1)
5.1.Peppermint leaves20,251±3,1935, 968,1015,1026, 1059,1083, 1142, 1167 Δ=±2 units index
5.2. Herb tarragon593, 655, 665, 709, 804, 1145, 1504, 1512 Δ=±2 units index
5.3.St. John's wort herb11,972±1,8601,633,660, 686, 793,923
Δ=±2 units index
5.4.Fruits, milk Thistle9,055±1,4
14,755±2,2
540, 568, 580, 711, 869, 907, 998
Δ=±2 units index

As can be seen from the data in table 1, the proposed method provides a significant increase in the reliability in the standardization of herbal drugs in comparison with the known method. Thus, the set of output signals for all samples LRS (item 5, table 1) is not less than six signals with different indexes retention and limit of confidence interval does not exceed ±2 units of the index or 2%, while for known way herb tarragon generally not identified, and peppermint leaves and herbs St. John's wort is only one reference substance, and the bound of the confidence interval of the absolute retention time in the mode of pyrolysis is ±15%.

The precision or repeatability of measurement in the output signals in terms of repeatability and accuracy of measurement of the concentration of mixture model for the proposed method is more than two times higher than for known (see PP, 3, 4 of table 1).

The use of the proposed method of assessing the authenticity of medicinal plant materials and devices for its implementation allows you to:

1. To create a reference data Bank on the combination of the output signals of the components RPF (retention indices in linear programming the temperature of the column and the quantitative content of the individual components of the RPF normalized output signals using the dual internal standard).

2. Check the standardization and evaluation of the authenticity of the LRS using the reference of the Bank.

3. To conduct rapid analysis of the quality and facilities of various BAD and the OP of this LSR.

1. The way to assess the authenticity of medicinal plants, in which a fixed number of investigated sample is placed in a sealed vessel, maintained at a given temperature, the components of the equilibrium vapor phase is metered into the chromatographic column, measured value signal and the retention time, wherein the sample is kept in a sealed vessel at 100°C for 40 min, the components of the equilibrium vapor phase will be analyzed by standard capillary column with a node of the input samples with a flow divider in a linear programming temperature, the output signals of the components is tov equilibrium vapor phase compared with the signals of external standards homologues of n-alkanes to calculate interpolation characteristics of the solutes, and synchronizing the moment you enter the analyzed samples are carried out by the signal detector to a fixed part of the flow from the discharge line of the divider node of the input samples.

2. The system for assessing the authenticity of medicinal plant raw materials containing preparation unit gas, tap-dispenser, heated sealed vessel for the studied samples, the node input samples with flow divider, capillary column, detector and software analysis, characterized in that the input of the detector is connected with the tee as with the exit of the capillary column and the vent line of the flow divider node of the input samples through a permanent pneumatic resistance and the measuring circuit of the detector is provided with an additional amplifier connected to the programmer analysis.



 

Same patents:

Purification method // 2444511

FIELD: chemistry.

SUBSTANCE: present invention relates to versions of a method of purifying terbinafine from nonmetallic impurities, primarily a substance A of formula

, as well as to use of said methods to obtain purified terbinafine. One of the versions of the method involves molecular distillation of crude terbinafine in form of a free base and extraction the obtained purified terbinafine in form of a free base or acid-addition salt (method A). In another version (method B), crude terbinafine in form a free base undergoes molecular distillation combined with formation of a salt of the obtained product with simultaneous deposition of a purified trans-isomer, and the obtained highly pure terbinafine is extracted in form of a free base or acid addition salt.

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13 cl, 2 dwg, 6 ex

FIELD: analytic chemistry.

SUBSTANCE: invention relates to analytical chemistry and can be used to detect and identify chemical substances in the mixture by their characteristics. Method of detection and identification of components of chemical mixtures by their characteristics include a preliminary identification of indicators traits components to detect and identify these indicators and depending on the operating parameters in the whole range of changes in these parameters. Also method includes measuring of the operating parameters and preliminary identification of indicators of response variations in calibration of measuring devices in the whole range of possible changes in operating parameters. In addition the method includes defining critical limits values of the intensity variations in the subsets of values or ranges of characters in the absence of any of the parts. Then selects a subset of values or characteristic ranges of any of the intensity distribution in excess of the modulus of the critical border of intensity data subsets or ranges of values of attributes. Next, determine the center group parameters and the variation of the intensity distribution observed in selected subsets of values or ranges characteristics. Then the component identification is performed by comparing the values of clustering center of the intensity distributions and values of characteristics in the measured values of operating parameters and values variation of the intensity distributions and values of variations at an incorrect response that measured in operating parameters. In this first in the whole range of possible changes of operating parameters and intensities of the parameter definition of line segments approximating the contour or contour segments gauge responses measuring device. Then determine the relationship between the parameters of these segments and the type of gauge responses contour, and before identification determine sites selected subsets of values or ranges characteristics that can be approximated by line segments with a given deviation. From the values of the parameters of these segments separate the contours of the mixture components are successively subtracted from the subsets of values or ranges of characteristics.

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15 cl, 7 dwg

FIELD: medicine.

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3 ex, 4 tbl

FIELD: medicine.

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1 ex, 1 tbl, 2 dwg

FIELD: chemistry.

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2 dwg, 2 tbl, 1 ex

FIELD: chemistry.

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3 ex, 4 tbl

FIELD: medicine.

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1 ex

FIELD: physics.

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FIELD: medicine.

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5 cl, 1 ex, 4 tbl

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8 dwg

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FIELD: chemical industry.

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EFFECT: high reproduction; simplification; improved efficiency of operation.

3 ex

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2 tbl

FIELD: physics.

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4 dwg

Gas analyzer // 2267123

FIELD: investigating or analyzing materials.

SUBSTANCE: gas analyzer comprises chromatographic columns, detectors, unit for preparing air mounted inside the thermostat, unit for control and processing signals, member for sampling, switches of gas flows, pump for pumping gas mixture, and separating passages connected in parallel and provided with the check valve interposed between them. Each of the separating passages is made of absorbing and separating chromatographic columns connected in series, and the pump is connected to the input of the gas line through the electric valve. The gas analyzer can be made of two separating passages and low pressure chromatographic columns.

EFFECT: enhanced quality of analyzing.

2 cl, 1 dwg, 1 ex

FIELD: analytical methods.

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EFFECT: enabled determination of small concentrations of methyl alcohol in water with sufficient selectivity and reliability.

2 cl, 2 tbl, 6 ex

FIELD: analytical chemistry.

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EFFECT: simplified process of sample preparation.

3 ex, 3 tbl

FIELD: biotechnology, in particular content determination of polymer chitosan molecules, chitosan-chitine polymer molecules and molecules of chitosan-protein complex in finished form of chitosan.

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4 cl, 3 dwg

Express-chromatron // 2300764

FIELD: the invention refers to laboratory chromatographic devices for conducting high-speed chromatographic analysis.

SUBSTANCE: the express-chromatron has an injector, a chromatographic column located in a thermostat, a detector, an amplifier of the signal of the detector, an analog-digital converter, a control system, a pneumatic system. The column is fulfilled either in the shape of a short capillary column or either in the shape of a polycapillary column. The injector is fulfilled with possibility of introduction of the test for the time of 5-50 ms. The detector and the amplifier of its signal are fulfilled with possibility of ensuring constant time of no worse then 10-3 sec. The analog-digital converter is fulfilled with possibility of ensuring speed of no less then 200 measurements in a second.

EFFECT: ensures conducting high-speed chromatographic analysis.

11 cl, 2 dwg

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