Method of determining alcohols in biological tissues and excretas of human body

FIELD: biotechnology.

SUBSTANCE: sample under study is placed in a sealed container of inert material, thermostated to the temperature above 25°C but below the destruction temperature of the biological object under study. From the thermostated sample the sampling of gas-vapour phase is carried out, which is examined by chromatography-mass spectrometry method by separation on the chromatographic column. Then the components of mixture of the gas-vapour phase are recorded as a series of chromatographic peaks in the chromatogram and are identified on time of their exit on the chromatogram and mass spectrum. Calculation of the concentration of alcohols is carried out in accordance with the obtained chromatogram according to the relevant peak areas of components of mixture of the gas-vapour phase.

EFFECT: increased sensitivity, accuracy and reliability of the identification and quantitative research, preservation of the object under study for possible repeat or additional studies.

1 tbl, 8 dwg

 

The invention relates to an integrated analysis of biological tissues and secretions of the human body using the method of gas chromatography-mass spectrometry (GC/MS). The method can be used in medicine, biology, forensic science, forensic and investigative activities when establishing the existence of spirits in biological tissues and secretions of the person, presence and degree of alcoholic intoxication audited entities, the establishment of the actual data about the poisoning of counterfeit alcohol, etc.

As the samples of biological tissues and secretions of the human body can use the following objects: water extracts of exhaled air, blood, saliva, urine, aqueous extracts disintegrated tissues and organs.

A known method of identifying unknown substances in biological fluids of patients taking narcotic drugs or psychotropic substances, namely, that prepare three samples studied sample of biological fluid: first, by extraction with reconstitution, the second by acid hydrolysis and the third by enzymatic hydrolysis. Moreover, the first sample is subjected to GC/MS analysis mode temperature gradient 15°C/min, and the data is analyzed by comparing with the database, which reveal the characteristics of the unknown, washes the VA (HB), namely spectra with m/z coinciding with basic ions of narcotic or psychotropic substances or metabolites, and content (HB) in the sample. The second sample was subjected to GC/MS analysis mode temperature gradient 25°C/min and the third sample was subjected to GC/MS analysis mode temperature gradient 15°C/min With increasing content of HB in the last two samples in comparison with the first subjected to GC/MS analysis mode temperature gradient 15°C/min, the basic drug or psychotropic substance for the presence of NV and in its absence in the base substance verify the presence of HB in intact biological fluid, for which the sample it is prepared by acid hydrolysis and subjected to GC/MS the analysis of the modes of the temperature gradient 15°C/min and 25°C/min. In case of detection of HB in intact biological fluid it qualify as endogenous, and in the absence of signs of an aliquot of the first sample is mixed with a sample of intact biological fluid. Meanwhile, prepare the sample by acid hydrolysis of the mixture, subjecting the sample GC/MS analysis mode temperature gradient 15°C/min and 25°C/min, Then to define the content of HB on the results of both analysis modes and compare it with the content of HB in the first sample. When matching the values of the content of HB in these three samples qualify HB as new, previously unknown is the local product of the metabolism of the basic narcotic drugs or psychotropic substances - patent RU 2419788, G01N 30/02, 2009

The study, conducted by a known method is complicated and time-consuming. In addition, the method is destructive, that is, after the analysis object can not be used for any other additional studies, such as DNA, audiologically, scent and others

The prototype of the invention is a method for the determination of nitrite alcohols, consisting in the conversion of alcohols in more volatile than the original alcohols, alkyl nitrites by reacting them with sodium nitrite in the environment of trichloroacetic acid, and in the future - chromatographicaliy of alkyl nitrites. Separated through column chromatography components of the mixture sequentially arrive at the detector thermal conductivity - katharometer, the signals which are recorded in the form of a number of chromatographic peaks on the chromatogram. Identification of substances produced by the time of their confinement, which is calculated from the moment of introduction of the analyte into the column until the maximum peak. Sensitivity to ethanol is limited to 0.01%vol. The calculation of the concentration of ethyl alcohol is produced by the intensity of the peaks on the chromatogram after calibration by the method of internal standard. The internal standard is isopropyl alcohol (source: "Medical examination DL is determined that alcohol consumption and intoxication". The instruction of the Ministry of health of the USSR from 02 September 1988 No. 06-14/33-14. ), The Ministry of health of the USSR, 1988, p.57-59, p.65-71 (copy attached), available online).

The disadvantages of the prototype method:

- low sensitivity: for ethyl alcohol of 0.01% vol.;

- identification of alcohols is produced only by time out on the chromatogram, which can lead to possible errors in their identification (for example, when tobacco or oral consumption of alcohol-containing medicines audited entities, the presence of traces of acetone or hydrocarbons in ambient air and the like);

the method is destructive, that is, after the analysis object can not be used for any other research, such as DNA, audiologically or the scent of research, additional studies on the presence of narcotic, potent and psychotropic substances and other

The technical problem solved by the invention is to improve the sensitivity, accuracy and reliability of identification and quantitative research, as well as in the preservation of the object is used for possible follow up or additional studies, i.e. its nerazresene.

This problem is solved by the method of determination of alcohols in biological tissues and secretions of the human body, in which IP is ledway the sample is placed in a sealed tank of inert material, thermostatic to temperatures above 25°C, but below the temperature of destruction of the investigated biological object from a temperature-controlled sample perform sampling vapor phase, which are examined by gas chromatography-mass spectrometrically by separation on a chromatographic column, then the components of the mixture vapor phase register in the form of a number of chromatographic peaks on the chromatogram and identify the time of their release on the chromatogram and mass spectrum, and calculating the concentration of the alcohols produced in accordance with the obtained chromatogram on the corresponding peak areas of the components of the mixture vapor phase.

Consider the technology of the method.

As samples of biological tissues and secretions of the human body can use the following objects: water extracts of exhaled air, blood, saliva, urine, aqueous extracts disintegrated tissues and organs.

It should be noted that these objects can be removed as in the presence of the audited entity, for example when establishing the presence and extent of alcohol auditees, when sampling does not pose any technical difficulties, and in the absence of the audited entity - traces (trace) of biological objects in case of their detection at the scene, for example when running the TBE person from the place of a traffic accident, finding a person in a helpless (unconscious) state etc,and so on

As it is well known that all these above mentioned objects are homogeneous or heterogeneous systems, in large quantities containing water, as a model system in the experiment used a solution of ethyl alcohol in distilled water with different volume concentration.

Temperature temperature sample depends on the temperature of its destruction (his unfitness for possible follow up or additional studies) and in the study of samples of different types, such as urine and blood, will vary and depend on the properties of the object of study. For example, in the study of blood coagulation proteins may start at a temperature 43-46°C, and complete coagulation occurs as a result of prolonged heating of the blood to a temperature of 70-80°C.

Taking into account the above well-known fact that solutions of ethanol in water was heated (thermostatical) to two temperatures: 25°C and 40°C respectively.

It is this temperature range allows you to save the analyzed blood sample for use in any other research, such as DNA, audiologically or scent studies, additional studies on the presence of narcotics them, potent and psychotropic substances and other

Also, knowing the range of concentrations of endogenous alcohol produced in the body of some people and alcohol intoxication of the human body: from tenths-hundredths of a ppm up to 4-10 ppm, i.e. from 0.01% vol. up to 1% vol. ethanol in the blood, to test the efficiency of the proposed method the solutions of ethanol in distilled water was prepared in the same concentrations.

In practice, experimentally implemented it the following way.

In standard glass chromatographic vials of 5 ml poured ethanol solutions of three concentrations: 1% vol. 0,1% vol. and 0.1% vol., which corresponds to the concentration of ethanol in the blood: 10, 1 and 0.1 ppm, respectively. Only 6 samples (three for each temperature). In each case the volume of the liquid phase was 2 ml, and the volume of the vapor phase above it - 3 ml, respectively. Then each vial was immediately closed with a rubber gasket-cork, which wore special aluminum cap and hermetically sealed by compression.

After the first three vials thermostatically (heated) by immersing them in water with a temperature of 25°C for a period of approximately 15 minutes, and the second three vials - thermostatically in similar conditions to a temperature of 40°C.

Samples from each vial were selected by the standard chromatographic syringe, a volume of 10 μl, which before sampling, also thermostatically to temperatures of 25°C and 40°C, respectively, by heating a stream of warm air of the same temperature in an oven for 15 minutes. This was done in order to avoid loss of ethanol due to condensation of vapors of selected samples on the surfaces of the syringe (needle, piston, etc.) due to temperature differences. In all cases, the selection of the vapor phase was carried out from the free volume of the vial by piercing the rubber stopper. The volume of the selected sample vapor phase in all cases was 10 μl (10-6l).

After sampling them separately immediately investigated by gas chromatography-mass spectrometry.

The choice of method gas chromatography-mass spectrometry due to the following factors:

- identification of the substance in the sample vapor phase at the same time on two criteria: time out on the chromatogram and mass spectrum, which allows to ensure 100% reliability of identification of alcohols on the chromatogram, even in the presence of any contaminants or complicate identification of foreign substances in the gas-vapor and liquid phase of the investigated object;

- in addition, depending on the conditions and properties of the analyzed substances method gas chromatography-mass spectrometry has high sensitivity: tenths ng (not below 10-9-10-10

To obtain quantitative characteristics of the detected ethanol in the vapor phase samples pre-determined time on the chromatogram, the characteristic features of its mass spectrum and its concentration dependence of peak area on the chromatogram by direct analysis of samples as vapor, and the liquid phase of ethanol known concentration in the completely same conditions chromatography was carried out.

Study of gas chromatography-mass spectrometry was carried out under the following conditions:

Chromatograph: model "Trace GC Ultra," the company "Thermo Finnigan, USA.

Column - quartz capillary standard model "VRH-5":

- inner diameter: 0.25 mm;

- length: 30 PM

Stationary liquid phase:

- film thickness: 0.25 μm.

Temperature of the column - programming:

- initial temperature: 50°C,

- the speed of temperature rise: 10°C/min,

final temperature: 300°C, holding for 15 minutes

Evaporator: - "splitless" (1:1); temperature: 250°C.

Carrier gas: helium; flow rate through the column: 1 ml/min

The temperature of the interface: 250°C.

The volume of injected steam and gas samples: 10,0 ál.

Mass spectrometer: model "PolarisQ"the company "Thermo Finnigan, USA.

Type ionization: electron impact (70 eV).

Detection: - "total ion current" (SCAN-mode).

The temperature of the ionization who ameres: 200°C.

Mass range: 32-450 u

A data processing system: "Xcalibur", version 1.4 SR1.

Transcript of mass spectra was performed by comparison with a calibration mass spectrum of ethanol, and by comparison with a library of mass spectra.

In both cases, the mass spectra of ethanol by total ion current (SCAN-mode) identified the following major ions with characteristic relations mass-to-charge m/z (Amu): 347%, 372%, 412%, 427%, 4314%, 45100%, 465%, 472%respectively.

The method is illustrated figure 1-8 and table 1.

Figure 1 shows the typical appearance of the chromatogram and mass spectrum of ethanol in the sample; figure 2-6 - the results of the chromatography was carried out several samples at various concentrations of ethanol in the gas-vapor phase; 7, 8 shows the chromatogram obtained by the method prototype and the proposed method respectively.

In the result of the chromatography was carried out sampling vapor phase, and identify the peaks of ethanol at the time of output is about 1.5 minutes, and mass spectra were determined amount of ethanol in each sample (10 ál vapor phase) depending on the temperature of incubation and the concentration of ethanol in aqueous solution - 1.

For each of the peaks of ethanol on the chromatograms was calculated amount of ethanol in the sample (ng), thus to improve the accuracy and reliability of results the calculation was not on the intensities (heights) of the peaks, and their squares, as it is known, is directly proportional to the concentration of the substance in the sample.

The results of the chromatography was carried out on all samples and calculations of the concentration of ethanol in the vapor phase samples for them are given in table 1 and in figure 2-6.

Table 1
No.T, °CThe concentration of ethanol in solutionThe peak area on the chromatogram, Rel. unitsThe estimated amount of ethanol in the sample vapor phase, ng
% vol.ppm
1259494012205451008,772
2251106402952,919
3250,112102317,375
4 250,010,11518412,549
540110175573145,109
6400,112641321,830
7400,010,11573613,005

Directly from table 1 and figure 2-6 results by gas chromatography-mass spectrometry it is possible to draw the following conclusions:

the amount of ethanol in the vapor phase samples is directly proportional to its concentration in the liquid phase (figure 2-6 for convenience, the relevant equation Y=kX+b, and the values of the correlation coefficients R2(all correlation coefficients close to unity), obtained by direct processing of the data by the method of least squares - OLS);

- detectable amounts of ethanol in the vapor phase samples reliably quantify it in the sample is of biological tissues and secretions of the human body at concentrations significantly lower than 0,01% vol. (less than 0.1 ppm);

- when the temperature control of the sample from 25°C to 40°C, the amount of ethanol in the gas-vapor phase increases several times, which increases the sensitivity of this method, in the absence of any destruction of proteins in the liquid phase samples of biological tissues and secretions of the human body.

To illustrate the greater sensitivity of the proposed method in comparison with the prototype 7-8 shows the chromatogram obtained by gas chromatograph with thermal conductivity detector (RTA) by the method-prototype (Fig.7) and the proposed method (Fig) on the equipment and conditions described above for the solutions of ethanol of the same concentration of 0.01% vol.

When comparing the peak intensity of amylnitrite (derived ethanol)detected in the combined-sample (on the chromatogram Fig.7 peak with the time of approximately 1,546 min, the intensity 407 Rel. units), and the intensity and peak area of ethanol in the sample vapor phase (on the chromatogram Fig - intensity around 1060 Rel. units, area - 15736 Rel. units), selected at 40°C, which in both cases is directly proportional to the concentrations of substances in the gas-vapor phase above the solutions of ethanol of the same concentration, we can conclude that the proposed method of determining the presence of alcohol in samples of biological tissues and ejecta the human body is superior to the method-prototype sensitivity not less than 10-20 times.

It should also be noted that when using the analytical system GC-MS other equipment, such as a chromatograph type Agilent-6890 (produced by Agilent, USA), with a more selective than the one used) in relation to alcohol chromatographic column and gas chromatography-mass spectrometer with quadrupole analyzer type Agilent-5973N, allowing detection mode for the selected ions (SIMM-mode) to increase the sensitivity of detection of alcohols approximately 10 times (we used a mass detector type design "ion trap", not giving practical increase sensitivity in SIMM-mode compared to SCAN-mode), the sensitivity of the proposed method may be higher than protetion, 10-100 times or more.

Thus, the proposed method for the determination of alcohols in biological tissues and secretions of the human body than the known method-prototip sensitivity makes it possible to eliminate a possible error in the identification of alcohol and is non-destructive, i.e. after the analysis object can be used for any other repeated or additional research.

The method of determination of alcohols in biological tissues and secretions of the human body, in which the sample is placed in a sealed container of inert is the material, thermostatic to temperatures above 25°C, but below the temperature of destruction of the analyzed biological sample from a temperature-controlled sample perform sampling vapor phase, which are examined by gas chromatography-mass spectrometrically by separation on a chromatographic column, then the components of the mixture vapor phase register in the form of a number of chromatographic peaks on the chromatogram and identify the time of their release on the chromatogram and mass spectrum, and calculating the concentration of the alcohols produced in accordance with the obtained chromatogram on the corresponding peak areas of the components of the mixture vapor phase.



 

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