CN110346470A - A kind of detection method of 3,4- methylene-dioxy methcathinone - Google Patents
A kind of detection method of 3,4- methylene-dioxy methcathinone Download PDFInfo
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Abstract
The invention discloses the detection methods of 3,4- methylene-dioxy methcathinone.A kind of method of the invention is to carry out organic solvent extraction to the Methylone in doubtful drugs sample, carries out qualitative analysis, gas-chromatography-flame ionization ditector (GC-FID) with gas chromatography-mass spectrography (GC-MS) and carries out quantitative analysis to Methylone.Another method of the invention is to carry out organic solvent extraction to the Methylone in doubtful drugs sample, carries out qualitative analysis, liquid chromatogram-diode array or UV detector (LC-DVD or LC-UV) under multiple-reaction monitoring (MRM) mode using liquid chromatogram-tandem mass spectrometry combination (LC-MS/MS) and carries out quantitative analysis to Methylone.
Description
Technical field
The invention belongs to drugs administration of justice detection fields, and in particular to the detection side of one kind 3,4- methylene-dioxy methcathinone
Method.
Background technique
New psychoactive drug substance, English name New psychoactive substances, abbreviation NPS are called in early days
Legal Highs or Designer Drug, Chinese claim " legal excitant " or " planning drug ", be the person of researching and producing in order to
Evade strike and the drugs analog that modifying for chemical structure obtains is carried out to part control drugs, has similar to control drugs
Effect, some excitements, cause is unreal, anaesthetic effect is stronger.The United Nations's drugs and crime office (UNODC) are by new psychotropic activity
Substance is divided into 9 major class, is respectively: synthesis Cannabinoids, cassie ketone, phenyl ethylamine class, tryptamines class, piperazines, ketamine and
Phencyclidines, amino indene, plant and other classes.
China is also very deficient for the research of new psychoactive drug substance at present, for 3, the 4- methylene-dioxy first of control
The detection method or blank of Cathinone qualitative, quantitative, therefore its method for qualitative and quantitative detection need be established, it is Related Cases
Technical support is carried out in investigation prosecution.
Summary of the invention
The 3,4- methylene-dioxy methcathinone that it is an object of the present invention to provide a kind of in doubtful drugs sample (with
Lower abbreviation Methylone) gas chromatography-mass spectrography (GC-MS) detection method.
3,4- methylene-dioxy methcathinone provided by the present invention in doubtful drugs sample is (hereinafter referred to as
Methylone the detection method of gas chromatography-mass spectrography (GC-MS)), includes the following steps:
1) organic solvent extraction is carried out to 3, the 4- methylene-dioxy methcathinone in doubtful drugs sample, collects and extracts
Liquid；
2) qualitative detection is carried out using gas chromatography-mass spectrography to the extracting solution；
By the total ion chromatogram and mass spectrogram of the extracting solution and 3,4- methylene-dioxy methcathinone standard substance
When being compared, while meeting two following conditions, it is judged to detecting 3,4- methylene-dioxy methcathinone；Otherwise it is determined as
It is not detected:
A) in the sample when reservation of the retention time of object and 3,4- methylene-dioxy methcathinone standard substance
Between relative error less than 2%；
B) mass spectrogram in the sample after object background correction and 3,4- methylene-dioxy methcathinone standard substance
Mass spectrogram matching degree after background correction is greater than 90%.
In above-mentioned method, when being judged to detecting 3,4- methylene-dioxy methcathinone in step 2), the method is also
Include the steps that carrying out quantitative analysis to the 3,4- methylene-dioxy methcathinone in the doubtful drugs sample；
The quantitative analysis includes the following steps: that (3) detect the extracting solution with gas-chromatography；
(4) content of the 3,4- methylene-dioxy methcathinone in the doubtful drugs sample is determined using external standard method
Amount analysis.
In above method step 1), concretely methanol, the extraction carry out the organic solvent under ultrasound condition.
In above method step 2), the testing conditions of the gas chromatography-mass spectrography (GC-MS) can refer to following
Part can also be adjusted certainly according to the actual conditions such as different brands instrument and different samples.
A) instrument: GC-MS.
B) ion source: electron bombardment ionization source (EI).
C) mass range: 35amu~500amu.
D) acquisition mode: full scan (Scan).
E) chromatographic column type: DB-5MS quartz glass capillary column (+95% dimethyl silicone polymer of 5% phenyl) or other
Equivalent column.
F) chromatography column parameter: 30m × 0.25mm × 0.25 μm.
G) chromatographic column temperature journey: 140 DEG C (3min) -20 DEG C/min-300 DEG C (16min).
H) injector temperature: 280 DEG C.
I) transmission line temperature: 250 DEG C.
J) ion source temperature: 230 DEG C.
K) split ratio: 40:1.
L) carrier gas: high-purity helium (He).
M) column flow (constant current): 1.0mL/min.
N) Multiplier voltage: tuning situation is referred to.
O) solvent is cut: 2min.
In above method step 3), the reference conditions of the gas-chromatography are as follows, specifically can according to different brands instrument and
The actual conditions such as different samples are adjusted.
A) instrument: gas chromatograph；
B) detector: flame ionization detector (FID)；
C) column model: DB-5 quartz glass capillary column (+95% dimethyl silicone polymer of 5% phenyl) or other etc.
Imitate column；
D) chromatography column parameter: 30m × 0.25mm × 0.25 μm.
E) column temperature: 140 DEG C (3min) -20 DEG C/min-300 DEG C (16min).
F) injector temperature: 280 DEG C.
G) detector temperature: 300 DEG C.
H) carrier gas: high pure nitrogen (N2)。
I) split ratio: 20:1.
J) column flow rate (constant current): 1mL/min.
K) combustion gas: H2。
L) combustion gas flow velocity: instrument default value is pressed.
M) combustion-supporting gas: air.
N) combustion air current speed: instrument default value is pressed.
In above method step 4), the quantitative analysis specifically comprises the following steps: to prepare at least five various concentration
3,4- methylene-dioxy methcathinone standard solution, gas-chromatography described in the standard solution step 3) is examined
It surveys, the peak area of absorption peak corresponding to 3, the 4- methylene-dioxy methcathinone of various concentration is obtained, with the standard solution
Concentration be abscissa, using peak area as ordinate, production standard working curve simultaneously obtain regression equation；Step 3) is measured
The peak area of absorption peak corresponding to the obtained 3,4- methylene-dioxy methcathinone in the doubtful drugs sample is brought into
It states in regression equation, that is, the content of 3, the 4- methylene-dioxy methcathinone in doubtful drugs sample is calculated.
The concentration range of the 3,4- methylene-dioxy methcathinone standard solution can be 0.05~2.5mg/mL.
It is also another object of the present invention to provide a kind of 3,4- methylene-dioxy methcathinones in doubtful drugs sample
(hereinafter referred to as Methylone) is with liquid chromatogram-tandem mass spectrometry combination (LC-MS/MS) under multiple-reaction monitoring (MRM) mode
The method detected.
3,4- methylene-dioxy methcathinone provided by the present invention in doubtful drugs sample is (hereinafter referred to as
Methylone it) is detected under multiple-reaction monitoring (MRM) mode with liquid chromatogram-tandem mass spectrometry combination (LC-MS/MS)
Method includes the following steps:
A organic solvent extraction) is carried out to 3, the 4- methylene-dioxy methcathinone in doubtful drugs sample, collects and extracts
Liquid；
B it) is mentioned under multiple-reaction monitoring (MRM) mode to described using liquid chromatogram-tandem mass spectrometry combination (LC-MS/MS)
Liquid is taken to carry out qualitative detection；
Under the same test conditions, two pairs of qualitative ion pair chromatographic peaks of appearance in sample to be tested, retention time and 3,
4- methylene-dioxy methcathinone standard substance retention time compares, and relative error is in ± 2%, and relative ion is to abundance
It is maximum more fair than being no more than with relative error of the relative ion in 3,4- methylene-dioxy methcathinone standard substance to abundance ratio
Perhaps range as defined in relative error, then there are 3,4- methylene-dioxy methcathinones in judgement sample；
Two pairs of qualitative ion pairs of 3, the 4- methylene-dioxy methcathinone are as follows: 1) m/z 208.1/160.1 goes cluster electric
Pressure is 30V, collision energy 16eV；2) m/z 208.1/132.1, removing cluster voltage is 30V, collision energy 25eV；
Relative ion is provided as follows to the maximum allowable relative error of abundance ratio:
In above-mentioned method, when being judged to detecting 3,4- methylene-dioxy methcathinone in step B), the method is also
Include the steps that carrying out quantitative analysis to the 3,4- methylene-dioxy methcathinone in the doubtful drugs sample；
The quantitative analysis includes the following steps: C) extracting solution is detected with liquid chromatogram；
D) content of 3,4- methylene-dioxy methcathinone in the doubtful drugs sample is quantified using external standard method
Analysis.
Above method step A) in, concretely methanol, the extraction carry out the organic solvent under ultrasound condition.
Above method step B) in, the chromatographic condition of the liquid chromatogram-tandem mass spectrometry is as follows, can be according to different brands
The actual conditions such as instrument and different samples are adjusted:
A) sampling volume: 1 μ L.
B) chromatographic column: C18 liquid-phase chromatographic column (1.7 μm, 100mm × 2.1mm) or other equivalent columns；
C) mobile phase: 0.1% aqueous formic acid of A volume fraction, B acetonitrile.
D) Gradient program: 0~1.5min, A phase volume fraction are 98%, B phase volume fraction is 2%；1.5~6.5min,
A phase volume fraction is down to 10%, B phase volume fraction from 98% and rises to 90% from 2%；6.5~8.0min, A phase volume fraction is
10%, B phase volume fraction is 90%；8.0~8.1min, A phase volume fraction from 10% rise to 98%, B phase volume fraction from
90% is down to 2%；8.1~10.0min, A phase volume fraction are 98%, B phase volume fraction is 2%；
E) flow velocity: 0.4mL/min.
F) ion source: electric spray ion source-positive ion mode (ESI+).
G) detection mode: multiple-reaction monitoring (MRM).
H) ion source temperature: 550 DEG C.
I) ion spray voltage: 5500V.
J) collision gas (CAD), gas curtain gas (CUR), atomization gas (GS1), auxiliary gas (GS2) are high pure nitrogen, before use
Each air flow rate is adjusted so that sensitivity of mass spectrometry reaches testing requirements.
K) go cluster voltage (DP), collision energy (CE) that optimum sensitivity should be optimized to.
In above method step 3), the chromatographic condition of the liquid chromatogram is as follows, can be according to different brands instrument and difference
The actual conditions such as sample are adjusted:
A) chromatographic column: C18 chromatographic column (5 μm, 150mm × 4.6mm) or other equivalent columns.
B) column temperature: 35 DEG C.
C) flow velocity: 1.0ml/min.
D) sampling volume: 5.0 μ l.
E) Detection wavelength: 280nm, bandwidth=4nm, reference wavelength=400nm, reference bandwidth=100nm.
F) mobile phase: A phase is acetonitrile, and B phase is phosphoric acid-triethylamine buffer solution (pH 2.6).
G) elution program: selection isocratic elution or gradient elution；
The sample is that purity is higher (concentration range is 70%~100%), then uses isocratic elution, mobile phase is by A phase
It is formed with B phase according to the ratio of volume ratio 14:86, analysis time 8min；
The sample is the sample of complicated component, then uses gradient elution, Gradient program are as follows: 0~7.5min, A phase volume
Score is 14%, B phase volume fraction is 86%；7.5~7.7min, A phase volume fraction rise to 80%, B phase volume point from 14%
Number is down to 20% from 86%；7.7~9.5min, A phase volume fraction are 80%, B phase volume fraction is 20%；9.5~
9.7min, A phase volume fraction are down to 14%, B phase volume fraction from 80% and rise to 86% from 20%；9.7~15min, A phase body
Fraction is 14%, B phase volume fraction is 86%；
H) detector: DVD or UV detector；
Above-mentioned method and step D) in, the quantitative analysis specifically comprises the following steps: to prepare at least five various concentration
3,4- methylene-dioxy methcathinone standard solution, liquid chromatogram described in the standard solution step 2) is carried out
Detection, obtains the peak area of absorption peak corresponding to 3, the 4- methylene-dioxy methcathinone of various concentration, molten with the standard
The concentration of liquid is abscissa, using peak area as ordinate, makes standard working curve and obtains regression equation；Step 2) is surveyed
Surely the peak area of absorption peak corresponding to the 3,4- methylene-dioxy methcathinone in the doubtful drugs sample obtained is brought into
In above-mentioned regression equation, the content of 3, the 4- methylene-dioxy methcathinone in doubtful drugs sample can be calculated.
The concentration range of the 3,4- methylene-dioxy methcathinone standard solution can be 0.005~0.5mg/mL.
It is by sample solution and-three second of phosphoric acid to the method that sample solution (extracting solution) is diluted in the above method
Amine buffer is diluted in 1:4 (V/V) ratio.
Compared with prior art, the present invention has the advantage that
Utilize common gas chromatography-mass spectrography, gas-chromatography, liquid chromatogram-tandem mass spectrometry, liquid chromatography technology
The qualitative and quantitative analysis method for establishing 3,4- methylene-dioxy methcathinone, the method established is quick, easy, easily operated,
It is easy to promote and utilize, it can satisfy the needs that judicial expertise department handles such case, mentioned for the smooth lawsuit of such case
For foundation.
Detailed description of the invention
Fig. 1 is the total ion chromatogram that gas chromatography-mass spectrometry analysis Methylone (RT=7.10min) is obtained.
Fig. 2 is that Methylone refers to EI mass spectrogram (electron impact ionization mass spectrometry).
Fig. 3 is the chromatogram that gas chromatographic analysis Methylone (RT=7.85min) is obtained.
Fig. 4 is MRM chromatogram (the m/z 208.1/160.1 that liquid chromatography-tandem mass spectrometry analyzes that Methylone is obtained；
m/z 208.1/132.1)。
Fig. 5 is the chromatogram that liquid-phase chromatographic analysis Methylone (RT=3.02min) is obtained.
Specific embodiment
Method of the invention is illustrated below by specific embodiment, but the present invention is not limited thereto, it is all at this
Any modifications, equivalent replacements, and improvements etc. done within the spirit and principle of invention, should be included in protection model of the invention
Within enclosing.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Quantitative test in following embodiments, is respectively provided with three repeated experiments, and results are averaged.
Embodiment 1, the Methylone in doubtful drugs sample is carried out with gas chromatography-mass spectrography (GC-MS) it is qualitative
Analysis
1, reagent and standard substance, instrument and measuring device tool
1.1 reagents and standard substance
This law agents useful for same is that analysis is pure.
Extract reagent: methanol.
Can trace to the source standard substance: Methylone.
1.2 instruments and measuring device tool
Gas chromatograph (GC) is furnished with flame ionization detector (FID).
Gas chromatograph-mass spectrometer (GC-MS) (GC-MS), the quadrupole mass spectrometer equipped with standard electronic bombardment source (EI).
Centrifuge.
Electronic balance, actual graduation value d=0.01mg.
Oscillator.
10mL and 1mL pipettor or pipette.
10mL bottleneck pipettor.
Note: involved all appts, measuring device tool need to be qualified by measurement verification.
2 qualitative analyses
2.1 sample preparation
Sample is fully ground mixing, weighs 5mg and is placed in centrifuge tube, and 10mL methanol is added, and ultrasonic dissolution is vortexed and mixes,
0.45 μm of membrane filtration, use to be analyzed.If target concentration is too low in sample, sample weighting amount can be increased to 100 mg.
2.2 gas chromatography-mass spectrographies (GC-MS) reference conditions
The following are reference conditions, can be adjusted according to the actual conditions such as different brands instrument and different samples.
A) instrument: GC-MS.
B) ion source: electron bombardment ionization source (EI).
C) mass range: 35amu~500amu.
D) acquisition mode: full scan (Scan).
E) chromatographic column type: DB-5MS quartz glass capillary column (+95% dimethyl silicone polymer of 5% phenyl) or other
Equivalent column.
F) chromatography column parameter: 30m × 0.25mm × 0.25 μm.
G) chromatographic column temperature journey: 140 DEG C (3min) -20 DEG C/min-300 DEG C (16min).
H) injector temperature: 280 DEG C.
I) transmission line temperature: 250 DEG C.
J) ion source temperature: 230 DEG C.
K) split ratio: 40:1.
L) carrier gas: high-purity helium (He).
M) column flow (constant current): 1.0mL/min.
N) Multiplier voltage: tuning situation is referred to.
O) solvent is cut: 2min.
The evaluation of 3 qualitative results
The total ion chromatogram (see Fig. 1) and mass spectrogram (see Fig. 2) of sample and Methylone standard substance are carried out
When comparing, while meeting two following conditions, it is judged to detecting corresponding substance；Otherwise it is judged to being not detected:
A) in sample the relative error of the retention time of the retention time and standard substance of object less than 2%；
B) mass spectrogram in sample after object background correction and the mass spectrogram matching degree after standard substance background correction are big
In 90%.
Embodiment 2, gas-chromatography-flame ionization ditector (GC-FID) are in doubtful drugs sample
Methylone carries out quantitative analysis
1, reagent and standard substance, instrument and measuring device tool
1.1 reagents and standard substance
This law agents useful for same is that analysis is pure.
Extract reagent: methanol.
Can trace to the source standard substance: Methylone.
1.2 instruments and measuring device tool
Gas chromatograph (GC) is furnished with flame ionization detector (FID).
Gas chromatograph-mass spectrometer (GC-MS) (GC-MS), the quadrupole mass spectrometer equipped with standard electronic bombardment source (EI).
Centrifuge.
Electronic balance, actual graduation value d=0.01mg.
Oscillator.
10mL and 1mL pipettor or pipette.
10mL bottleneck pipettor.
Note: involved all appts, measuring device tool need to be qualified by measurement verification.
2 quantitative analyses
2.1 external standard single-point methods
2.1.1 the preparation of standard solution
2.1.1.1 the preparation of 1.0mg/mL Methylone standard reserving solution
A certain amount of Methylone standard substance is accurately weighed, is dissolved with methanol, 1.0mg/mL Methylone is configured to
Standard reserving solution sets refrigerator cold-storage preservation, and the holding time is 6 months.
2.1.1.2 the preparation of 0.1mg/mL Methylone standard working solution
Appropriate 1.0mg/mL Methylone standard reserving solution is accurately pipetted, with methanol dilution to 0.1mg/mL, oscillation is mixed
It is even, set it is stored refrigerated in refrigerator, the holding time be 3 months.
2.1.2 gas-chromatography (GC-FID) reference conditions
The following are reference conditions, can be adjusted according to the actual conditions such as different brands instrument and different samples.
A) instrument: GC.
B) detector: flame ionization detector (FID).
C) column model: DB-5 quartz glass capillary column (+95% dimethyl silicone polymer of 5% phenyl) or other etc.
Imitate column.
D) chromatography column parameter: 30m × 0.25mm × 0.25 μm.
E) column temperature: 140 DEG C (3min) -20 DEG C/min-300 DEG C (16min).
F) injector temperature: 280 DEG C.
G) detector temperature: 300 DEG C.
H) carrier gas: high pure nitrogen (N2)。
I) split ratio: 20:1.
J) column flow rate (constant current): 1mL/min.
K) combustion gas: H2。
L) combustion gas flow velocity: instrument default value is pressed.
M) combustion-supporting gas: air.
N) combustion air current speed: instrument default value is pressed.
2.1.3 content range preanalysis
The purpose of preanalysis is to carry out preliminary survey to the Methylone content in sample, to calculate accurate quantitative analysis
When sample used weighing weight, thus guarantee the ultimate density of object in sample solution when accurate quantitative analysis as close possible to
The concentration of used standard working solution.
It weighs about 5mg sample to be placed in test tube with cover, 10mL methanol is added, sonic oscillation makes it dissolve, takes after centrifugation
Clear liquid is analyzed with GC-FID, using the Methylone standard working solution of 0.1mg/mL as quantitative reference.
If the excessive concentration of target compound in sample solution can suitably reduce sample weighing weight, or sample is mentioned
It is analyzed after taking liquid to be diluted with Extraction solvent.
If the concentration of target compound is too low in sample solution, it can suitably increase sample weighing weight, or sample is mentioned
Liquid is taken to volatilize, analyzed after constant volume.
According to the following formula 1 calculate sample in target components percentage composition.
In formula:
W (%) --- the percentage composition of Methylone in sample；
C0--- the concentration of Methylone, mg/mL in standard working solution；
A --- the chromatographic peak area value of Methylone in sample solution；
V1--- the first constant volume of sample solution, mL；
V3--- by V2The volume of Extraction solvent, mL are added when dilution；
A0--- the chromatographic peak area value of Methylone in standard working solution；
V2--- from V1In pipette the volume of sample solution, mL；
M --- the weighing weight of the sample for measurement, mg.
2.1.4 accurate quantitative analysis
2.1.4.1 the calculating of weight is weighed
According to Methylone assay in preanalysis as a result, selecting suitable constant volume, extension rate (referring to table
1), and according to the following formula 2 sample weighing weight (m) is calculated.
In formula:
M (mg) --- weigh weight；
C0--- the concentration of Methylone, mg/mL in standard working solution；
V --- first constant volume, mL；
D --- extension rate；
W (%) --- the preanalysis percentage composition of Methylone in sample.
1 outer marking quantitative method sample extraction operating parameter of table selects table
2.1.4.2 sample extraction
According to 2.1.4.1 calculated result, 2 parts of sample are weighed in parallel, and according to preanalysis content range, it is corresponding first fixed to be added
The methanol (referring to table 1) of volume product seals simultaneously sonic oscillation 10min；If sample solution needs to dilute, pipettes 1mL sample and mention
It takes liquid into another test tube, is diluted constant volume according to extension rate, takes supernatant to be analyzed with GC-FID after centrifugation.
2.1.4.3 content calculates
Methylone percentage composition in sample is calculated according to formula 1 in 2.1.3.
2.2 external standard working curve methods
2.2.1 standard working curve is drawn
Take respectively low (0.05mg/mL), in (1.0mg/mL), high (2.5mg/mL) 3 concentration Methylone standard
Solution, each 10 needle of concentration continuous sample introduction, calculates the in a few days relative standard deviation of sample；Continuous detection 6 days, calculates the day of sample
Between relative standard deviation.The in a few days relative standard deviation of Methylone is 0.57%, and relative standard deviation is 1.87% in the daytime.
Detection is limited to 10 μ g/mL.Using the method for blank sample-adding recycling, different amounts of Methylone is added respectively into blank solution
Standard solution obtains each 3 parts of Methylone solution that concentration is respectively 0.05mg/mL, 1.0mg/mL, 2.5mg/mL, measures
The accuracy range of Methylone is 96.67%-102.31%.
A certain amount of Methylone standard substance is accurately weighed, is dissolved with methanol, the mark that content is 2.5mg/mL is made into
Quasi- stock solution is sealed in 0~5 DEG C of refrigerator, validity period 6 months.Appropriate Methylone Standard Reserving Solution is accurately pipetted, according to
It is secondary to be diluted with methanol to 1,0.5,0.2,0.1,0.05mg/mL concentration, it mixes well.Using 2.5,1,0.5,0.2,
0.1,6 concentration such as 0.05mg/mL are depicted as the Methylone standard working curve that the range of linearity is 0.05~2.5mg/mL.
Each concentration sample introduction 3 times, and linear regression is carried out to the average value A and mass concentration C (mg/mL) of 3 peak areas,
Obtain the regression equation of Methylone: A=552.22c-12.357, r2It is 0.9997,0.05~2.5mg/mL of the range of linearity,
10 μ g/mL (S/N >=3) of detection limit
2.2.2 quantitative
2.2.2.1 extraction operation
2 parts of sample each about 25mg are weighed in parallel, 10mL methanol is added, and ultrasonic dissolution is analyzed with GC-FID after centrifugation, adopted
Quantitative calculating is carried out with the standard working curve in 2.2.1.
Gas-chromatography 2.2.2.2 (GC-FID) reference conditions
With 2.1.2 external standard single-point sizing technique GC-FID reference conditions.
2.2.2.3 content calculates
Sample size is calculated according to working curve.
The evaluation of 3 quantitative results
3.1 content results validity
To same a sample, 2 parallel determination data carry out relative differences (RD) according to formula 3 and calculate, and RD is no more than
10%, data are effective；Otherwise, it should examine again.
In formula:
RD- relative differences, unit %；
X1、X2What-two samples quantitative determined in parallel contains numerical quantity；
- two samples quantitative determine the average value of content in parallel.
3.2 content results calculate
Using the average value of 2 parts of sample measurement contents as content results.
The statement of 3.3 content results
After the completion of quantitative testing, inspection result should be stated are as follows: Methylone ingredient is detected from sample, wherein
Methylone(C11H13NO3) content be ×× × %.
The gas chromatogram of Methylone standard substance is as shown in figure 3, wherein retention time is in the present embodiment
Absorption peak at 7.85min is Methylone absorption peak.
Embodiment 3 is combined (LC-MS/MS) to the liquid chromatogram-tandem mass spectrometry of the Methylone in doubtful drugs sample
Qualitative analysis is carried out under multiple-reaction monitoring (MRM) mode
1, reagent and standard substance, instrument and measuring device tool
1.1 reagents and standard substance
Agents useful for same is chromatographically pure, and test water is level-one water (see GB/T 6682-2008), reagent and standard substance
Include:
A) reagent: methanol, acetonitrile, formic acid；
B) can trace to the source standard substance: Methylone；
C) 0.1% aqueous formic acid: measuring 1mL formic acid, and water is added and dissolves and be diluted to 1000mL, 0.22 μm after mixing
Membrane filtration, ultrasound after set aside for use；
D) standard reserving solution: weighing Methylone standard substance, dissolved respectively with methanol, is configured to the mark of 2.5mg/mL
Quasi- stock solution sets refrigerator cold-storage preservation, and the holding time is 6 months；
E) qualitative with 100ng/mL standard working solution: appropriate Methylone standard reserving solution accurately to be pipetted, with 0.1% first
Aqueous acid is diluted to 100ng/mL, use to be analyzed, i.e., with i.e. use step by step.
1.2 instruments and measuring device tool
Instrument and measuring device tool include:
A) liquid chromatogram-tandem mass spectrometry combined instrument (LC-MS/MS), the mass spectrograph equipped with electric spray ion source.
B) centrifuge.
C) electronic balance, actual graduation value d=0.01mg.
D) oscillator.
E) 10mL and 1mL pipettor or pipette.
F) 10mL bottleneck pipettor.
G) 0.22 μm of filter membrane.
2, qualitative analysis
2.1 sample preparation
Sample about 5mg is weighed, 10mL methanol is added, ultrasonic dissolution is vortexed and mixes.Appropriate amount of sample solution is taken, with 0.1%
Aqueous formic acid is diluted to 100ng/mL, 0.22 μm of membrane filtration, use to be analyzed, i.e., with i.e. use step by step.If target in sample
Object concentration is too low, can be diluted to 5000ng/mL.
2.2 liquid chromatograph-mass spectrometer reference conditions
The following are reference conditions, can be adjusted according to the actual conditions such as different brands instrument and different samples:
A) sampling volume: 1 μ L.
B) chromatographic column: C18 liquid-phase chromatographic column (1.7 μm, 100mm × 2.1mm) or other equivalent columns.
C) mobile phase: 0.1% aqueous formic acid of A, B acetonitrile.
D) 2 Gradient program: are shown in Table.
2 gradient elution program of table
| Time/min | A% | B% |
| 0 | 98 | 2 |
| 1.5 | 98 | 2 |
| 6.5 | 10 | 90 |
| 8.0 | 10 | 90 |
| 8.1 | 98 | 2 |
| 10 | 98 | 2 |
E) flow velocity: 0.4mL/min.
F) ion source: electric spray ion source-positive ion mode (ESI+).
G) detection mode: multiple-reaction monitoring (MRM).
H) ion source temperature: 550 DEG C.
I) ion spray voltage: 5500V.
J) collision gas (CAD), gas curtain gas (CUR), atomization gas (GS1), auxiliary gas (GS2) are high pure nitrogen, before use
Each air flow rate is adjusted so that sensitivity of mass spectrometry reaches testing requirements.
K) go cluster voltage (DP), collision energy (CE) that optimum sensitivity should be optimized to.
L) qualitative ion pair of Methylone, go cluster voltage and collision energy to being shown in Table 3.
The qualitative ion pair of 3 Methylone of table removes cluster voltage (DP) and collision energy (CE)
The evaluation of 3 qualitative results
Under the same test conditions, in sample to be tested occur two pairs of qualitative ion pair chromatographic peaks, retention time with add
Object retention time compares in sample-adding product, and relative error is in ± 2%, and relative ion is in abundance ratio and addition sample
Relative ion range as defined in table 4 is no more than to the relative error of abundance ratio, then can determine whether that there are objects in sample.
Maximum allowable relative error (%) of 4 relative ion of table to abundance ratio
Embodiment 4, liquid chromatogram-diode array or UV detector (LC-DVD or LC-UV) are to doubtful drugs sample
In Methylone carry out quantitative analysis
1, reagent and standard substance, instrument and measuring device tool
1.1 reagents and standard substance
Agents useful for same is chromatographically pure, and test water is level-one water (see GB/T 6682-2008), reagent and standard substance
Include:
A) reagent: methanol, acetonitrile, formic acid, phosphoric acid, triethylamine；
B) can trace to the source standard substance: Methylone；
C) phosphoric acid-triethylamine buffer solution: measuring concentrated phosphoric acid 4.12mL, and the dilution of 200mL water is added；Measure triethylamine 5.56
ML is instilled in above-mentioned phosphoric acid solution；It adds water and is diluted to 1000mL, 0.45 μm of water system membrane filtration after mixing is quiet after ultrasonic
It sets stand-by；
D) 10mL methanol and 40mL phosphoric acid-three methanol-phosphoric acid-triethylamine buffer solution mixed solution (V/V=1:4): are measured
Ethamine buffer mixes, set aside for use after ultrasound；
E) standard reserving solution: weighing Methylone standard substance, dissolved respectively with methanol, is configured to the mark of 2.5mg/mL
Quasi- stock solution sets refrigerator cold-storage preservation, and the holding time is 6 months；
F) it outer marking quantitative 0.1mg/mL standard working solution: pipettes 2.5mg/mL standard reserving solution 2mL and is added to 50 mL appearance
In measuring bottle, with methanol dilution to scale, it is configured to 0.1mg/mL object standard working solution, sets stored refrigerated in refrigerator, preservation
Time is 3 months.
1.2 instruments and measuring device tool
Instrument and measuring device tool include:
A) liquid chromatograph (LC), the liquid chromatograph equipped with two pole arrays or UV detector.
B) centrifuge.
C) electronic balance, actual graduation value d=0.01mg.
D) oscillator.
E) 10mL and 1mL pipettor or pipette.
F) 10mL bottleneck pipettor.
G) 0.45 μm of filter membrane.
2 quantitative analyses
2.1 liquid chromatograph reference conditions
The following are reference conditions, can be adjusted according to the actual conditions such as different brands instrument and different samples:
A) chromatographic column: C18 chromatographic column (5 μm, 150mm × 4.6mm) or other equivalent columns.
B) column temperature: 35 DEG C.
C) flow velocity: 1.0ml/min.
D) sampling volume: 5.0 μ l.
E) Detection wavelength: 280nm, bandwidth=4nm, reference wavelength=400nm, reference bandwidth=100nm.
F) mobile phase: A phase is acetonitrile, and B phase is phosphoric acid-triethylamine buffer solution (pH 2.6).
G) isocratic elution or gradient elution elution program: are selected according to sample situation.
Isocratic elution (is suitable for the higher sample of purity): 14%A+86%B (v/v), analysis time 8min.
Gradient elution (is suitable for the more complicated sample of ingredient): elution program reference table 5.
5 gradient elution program of table
| Time/min | A% | B% |
| 0 | 14 | 86 |
| 7.5 | 14 | 86 |
| 7.7 | 80 | 20 |
| 9.5 | 80 | 20 |
| 9.7 | 14 | 86 |
| 15 | 14 | 86 |
2.2 external standard single-point methods
2.2.1 content range preanalysis
The purpose of preanalysis is to carry out preliminary survey, institute when calculating accurate quantitative analysis to the object content in sample
With the weighing weight of sample, to guarantee the ultimate density of object in sample solution when accurate quantitative analysis as close possible to being made
With the concentration of standard working solution.
It weighs about 5mg sample to be placed in test tube with cover, the oscillation of 10mL methanol is added and makes it dissolve, is taken after centrifugation on appropriate
Clear liquid, in sample solution: phosphoric acid-triethylamine buffer solution=1:4 (V/V) ratio is diluted, 0.45 μm of organic system after mixing
Membrane filtration is analyzed with LC-DVD or LC-UV.Using the standard working solution of 0.1mg/mL as quantitative reference, standard solution is adopted
It is diluted with the same manner, it is appropriate to pipette 0.1mg/mL standard working solution, by standard working solution: phosphoric acid-triethylamine buffer solution=1:
The ratio of 4 (V/V) is diluted, and is mixed well, use to be analyzed, i.e., with i.e. use.
If the excessive concentration of target compound in sample solution can suitably reduce sample weighing weight, or sample is mentioned
It is analyzed after taking liquid to be diluted with Extraction solvent.
If the concentration of target compound is too low in sample solution, it can suitably increase sample weighing weight, or sample is mentioned
Liquid is taken to volatilize, analyzed after constant volume.
The percentage composition of target components in sample is calculated according to formula (1).
In formula:
W --- the percentage composition of Methylone in sample, unit %；
C0--- the concentration of Methylone in standard working solution, unit mg/mL；
A --- the chromatographic peak area value of Methylone in sample solution；
V1--- the first constant volume of sample solution, unit mL；
V3--- by V2The volume of Extraction solvent, unit mL are added when dilution；
A0--- the chromatographic peak area value of Methylone in standard working solution；
V2--- from V1In pipette the volume of sample solution, unit mL；
M --- the weighing weight of the sample for measurement, unit mg.
2.2.2 accurate quantitative analysis
2.2.2.1 the calculating of weight is weighed
According to object assay in preanalysis as a result, selecting suitable constant volume, extension rate (sample extraction
Operating parameter is selected referring to table 1), and sample weighing weight (m) is calculated according to formula (2).
In formula:
M --- weigh weight, unit mg；
C0--- the concentration of Methylone in standard working solution, unit mg/mL；
V --- first constant volume, unit mL；
D --- extension rate；
W --- the preanalysis percentage composition of Methylone, unit % in sample.
2.2.2.2 sample extraction
According to 2.2.2.1 calculated result, 2 parts of sample are weighed in parallel, and according to preanalysis content range, it is corresponding first fixed to be added
The methanol of volume product.It seals and vibrates 10min.If sample solution needs to dilute, 1mL sample extracting solution is pipetted to another examination
Guan Zhong is diluted constant volume according to extension rate, takes supernatant after centrifugation, by sample solution: phosphoric acid-triethylamine buffer solution=
The ratio of 1:4 (V/V) is diluted, and is analyzed with LC-DVD (or LC-UV).Sample extraction operating parameter is selected referring to table 1.
2.2.2.3 content calculates
Object percentage composition in sample is calculated according to according to formula in 2.2.1 (1).
2.3 external standard working curve methods
Take respectively low (0.005mg/mL), in (0.1mg/mL), high (0.5mg/mL) 3 concentration Methylone standard
Solution, each 10 needle of concentration continuous sample introduction, calculates the in a few days relative standard deviation of sample；Continuous detection 6 days, calculates the day of sample
Between relative standard deviation.The in a few days relative standard deviation of Methylone is 1.43%, and relative standard deviation is 2.84% in the daytime.
Detection is limited to 0.16 μ g/mL.Using the method for blank sample-adding recycling, added respectively into blank solution different amounts of
Methylone standard solution obtains the Methylone solution that concentration is respectively 0.005mg/mL, 0.1mg/mL, 0.5mg/mL
Each 3 parts, the accuracy range for measuring Methylone is 96.98%-101.92%.
2.3.1 standard working curve is drawn
Appropriate Methylone standard reserving solution is accurately pipetted, by standard reserving solution: phosphoric acid-triethylamine buffer solution=1:4
(V/V) ratio is diluted, and is mixed well, and the standard working solution of 0.5mg/mL is configured to；Reuse methanol-phosphoric acid-three
Ethamine buffer mixed solution is diluted the standard working solution of the above 0.5mg/mL, and being configured to concentration is 0.005mg/
The standard series working solution of mL, 0.025mg/mL, 0.05mg/mL, 0.1mg/mL, 0.25mg/mL, 0.5mg/mL.Standard system
Column working solution is stored refrigerated in refrigerator, and validity period 7 days.
Each concentration sample introduction 3 times, and linear regression is carried out to the average value A and mass concentration C (mg/mL) of 3 peak areas,
Obtain the regression equation of Methylone: A=6074.7c+12.012, r2It is 1,0.005~0.5mg/mL of the range of linearity, detection
Limit 0.16 μ g/mL (S/N >=3)
2.3.2 quantitative
2.3.2.1 extraction operation
2 parts of sample each about 25mg are weighed in parallel, 10mL methanol is added, and ultrasonic dissolution is vortexed and mixes.Take appropriate amount of sample molten
Liquid, in sample solution: phosphoric acid-triethylamine buffer solution=1:4 (V/V) ratio is diluted, 0.45 μm of organic system filter after mixing
Film filtering, is analyzed with LC-DVD (or LC-UV).
2.3.2.2 content calculates
It is quantified according to the standard working curve in 2.3.1, calculates sample size.
The evaluation of 3 quantitative results
3.1 content results validity
It carries out relative differences (RD) according to formula (4) to two parallel determination data to calculate, RD is no more than 10%, data
Effectively；Otherwise, it should examine again.
In formula:
RD- relative differences, unit %；
X1、X2What-two samples quantitative determined in parallel contains numerical quantity；
- two samples quantitative determine the average value of content in parallel.
3.2 content results calculate
Using the average value of two parts of sample measurement contents as content results.
The statement of 3.3 content results
After the completion of quantitative testing, inspection result should be stated are as follows: Methylone ingredient is detected from sample, wherein
Methylone(C11H13NO3) content be ×× × %.
Claims (10)
1. a kind of method that 3, the 4- methylene-dioxy methcathinone in doubtful drugs sample is detected, including following steps
It is rapid:
1) organic solvent extraction is carried out to 3, the 4- methylene-dioxy methcathinone in doubtful drugs sample, collects extracting solution；
2) qualitative detection is carried out using gas chromatography-mass spectrography to the extracting solution；
By sample and 3, the total ion chromatogram and mass spectrogram of 4- methylene-dioxy methcathinone standard substance are compared, together
When meeting two following conditions, be judged to detecting 3,4- methylene-dioxy methcathinone；Otherwise it is judged to being not detected:
A) retention time of object and the retention time of 3,4- methylene-dioxy methcathinone standard substance in the sample
Relative error is less than 2%；
B) after the mass spectrogram in the sample after object background correction and 4- methoxy methyl Cathinone standard substance background correction
Mass spectrogram matching degree be greater than 90%.
2. according to the method described in claim 1, it is characterized by: the organic solvent is methanol, described in the step 1)
Extraction carries out under ultrasound condition；
In the step 2), the testing conditions of the gas chromatography-mass spectrography are as follows:
A) instrument: GC-MS；
B) ion source: electron bombardment ionization source；
C) mass range: 35amu~500amu；
D) acquisition mode: full scan；
E) chromatographic column type: DB-5 MS quartz glass capillary column；
F) chromatography column parameter: 30m × 0.25mm × 0.25 μm.
G) chromatographic column temperature journey: 140 DEG C (3min) -20 DEG C/min-300 DEG C (16min)；
H) injector temperature: 280 DEG C；
I) transmission line temperature: 250 DEG C；
J) ion source temperature: 230 DEG C；
K) split ratio: 40:1；
L) carrier gas: high-purity helium；
M) column flow (constant current): 1.0mL/min；
N) solvent is cut: 2min.
3. method according to claim 1 or 2, it is characterised in that: the method also includes in doubtful drugs sample
The method that 3,4- methylene-dioxy methcathinones carry out quantitative analysis, includes the following steps:
3) extracting solution described in claim 1 is detected with gas-chromatography；
4) quantitative analysis is carried out using content of the external standard method to the 3,4- methylene-dioxy methcathinone in doubtful drugs sample.
4. according to the method described in claim 3, it is characterized by: the condition of the gas-chromatography is as follows in the step 3):
A) instrument: gas chromatograph；
B) detector: flame ionization detector；
C) column model: DB-5 quartz glass capillary column；
D) chromatography column parameter: 30m × 0.25mm × 0.25 μm；
E) column temperature: 140 DEG C (3min) -20 DEG C/min-300 DEG C (16min)；
F) injector temperature: 280 DEG C；
G) detector temperature: 300 DEG C；
H) carrier gas: high pure nitrogen；
I) split ratio: 20:1.
J) column flow rate (constant current): 1mL/min.
K) combustion gas: H2；
L) combustion gas flow velocity: instrument default value is pressed；
M) combustion-supporting gas: air；
N) combustion air current speed: instrument default value is pressed.
5. the method according to claim 3 or 4, it is characterised in that:
In the step 4), the quantitative analysis specifically comprises the following steps: 3, the 4- methylene two for preparing at least five various concentration
Gas-chromatography described in the standard solution step 3) is detected, obtains difference by oxygroup methcathinone standard solution
The peak area of absorption peak corresponding to 3, the 4- methylene-dioxy methcathinone of concentration, with the concentration of the standard solution for horizontal seat
Mark makes standard working curve and obtains regression equation using peak area as ordinate；Step 3) measurement is obtained described doubtful
The peak area of absorption peak corresponding to 3,4- methylene-dioxy methcathinone in drugs sample is brought into the regression equation, meter
It calculates and obtains the content of the 3,4- methylene-dioxy methcathinone in doubtful drugs sample；
The concentration range of the 3,4- methylene-dioxy methcathinone standard solution is 0.05~2.5mg/mL.
6. a kind of method that 3, the 4- methylene-dioxy methcathinone in doubtful drugs sample is detected, including following steps
It is rapid:
A organic solvent extraction) is carried out to 3, the 4- methylene-dioxy methcathinone in doubtful drugs sample, collects extracting solution；
B qualitative detection) is carried out to the extracting solution under multiple-reaction monitoring pattern using liquid chromatogram-tandem mass spectrometry combination；
Under the same test conditions, occur two pairs of qualitative ion pair chromatographic peaks, retention time and 3,4- in the extracting solution
Methylene-dioxy methcathinone standard substance retention time compares, relative error in ± 2%, and relative ion to abundance ratio with
Relative ion in 3,4- methylene-dioxy methcathinone standard substance is no more than maximum allowable phase to the relative error of abundance ratio
To range as defined in error, then there are 3,4- methylene-dioxy methcathinones in judgement sample；
Two pairs of qualitative ion pairs of 3, the 4- methylene-dioxy methcathinone are as follows: 1) m/z 208.1/160.1 goes the cluster voltage to be
30V, collision energy 16eV；2) m/z 208.1/132.1, removing cluster voltage is 30V, collision energy 25eV；
Relative ion is provided as follows to the maximum allowable relative error of abundance ratio:
7. according to the method described in claim 6, the it is characterized by: step A) in, the organic solvent is methanol, described
Extraction carries out under ultrasound condition；
The step B) in, the chromatographic condition of the liquid chromatogram-tandem mass spectrometry is as follows:
A) sampling volume: 1 μ L；
B) chromatographic column: C18 liquid-phase chromatographic column 100mm × 2.1mm × 1.7 μm；
C) mobile phase: 0.1% aqueous formic acid of A volume fraction, B acetonitrile；
D) Gradient program: 0~1.5min, A phase volume fraction are 98%, B phase volume fraction is 2%；1.5~6.5min, A phase body
Fraction is down to 10%, B phase volume fraction from 98% and rises to 90% from 2%；6.5~8.0min, A phase volume fraction are 10%, B
Phase volume fraction is 90%；8.0~8.1min, A phase volume fraction rise to 98%, B phase volume fraction from 10% and are down to from 90%
2%；8.1~10.0min, A phase volume fraction are 98%, B phase volume fraction is 2%；
E) flow velocity: 0.4mL/min；
F) ion source: electric spray ion source-positive ion mode；
G) detection mode: multiple-reaction monitoring；
H) ion source temperature: 550 DEG C；
I) ion spray voltage: 5500V；
J) collision gas, gas curtain gas, atomization gas, auxiliary gas are high pure nitrogen, adjust each air flow rate so that mass spectrum is clever using preceding
Sensitivity reaches testing requirements；
K) go cluster voltage, collision energy that should be optimized to optimum sensitivity.
8. method according to claim 7 or 8, it is characterised in that: the method also includes in doubtful drugs sample
The method that 3,4- methylene-dioxy methcathinones carry out quantitative analysis, includes the following steps:
C) extracting solution described in claim 6 is detected with liquid chromatogram；
D quantitative analysis) is carried out using content of the external standard method to the 3,4- methylene-dioxy methcathinone in doubtful drugs sample.
9. according to the method described in claim 8, the it is characterized by: step C) in, the chromatographic condition of the liquid chromatogram
It is as follows:
A) chromatographic column: C18 chromatographic column 150mm × 4.6mm × 5 μm；
B) column temperature: 35 DEG C；
C) flow velocity: 1.0ml/min；
D) sampling volume: 5.0 μ l；
E) Detection wavelength: 280nm, bandwidth=4nm, reference wavelength=400nm, reference bandwidth=100nm；
F) mobile phase: A phase is acetonitrile, and B phase is phosphoric acid-triethylamine buffer solution pH 2.6；
G) elution program: selection isocratic elution or gradient elution；
The purity of the sample is 70%~100%, then uses isocratic elution, mobile phase is by A phase and B phase according to volume ratio 14:
86 ratio composition, analysis time 8min；
The sample is the sample of complicated component, then uses gradient elution, Gradient program are as follows: 0~7.5min, A phase volume fraction
It is 86% for 14%, B phase volume fraction；7.5~7.7min, A phase volume fraction from 14% rise to 80%, B phase volume fraction from
86% depreciation 20%；7.7~9.5min, A phase volume fraction are 80%, B phase volume fraction is 20%；9.5~9.7min, A phase
Volume fraction is down to 14%, B phase volume fraction from 80% and rises to 86% from 20%；9.7~15min, A phase volume fraction is
14%, B phase volume fraction is 86%.
10. according to the method described in claim 9, the it is characterized by: step D) in, the quantitative analysis specifically include as
Lower step: preparing 3, the 4- methylene-dioxy methcathinone standard solution of at least five various concentration, and the standard solution is walked
Rapid C) described in liquid chromatogram detected, obtain absorption corresponding to 3, the 4- methylene-dioxy methcathinone of various concentration
The peak area at peak, using peak area as ordinate, makes standard working curve and obtains using the concentration of the standard solution as abscissa
To regression equation；
Absorption corresponding to the 3,4- methylene-dioxy methcathinone in the doubtful drugs sample that step C) measurement is obtained
The peak area at peak is stated in regression equation described in bringing into, and 3, the 4- methylene-dioxy methcathinone in doubtful drugs sample is calculated
Content；
The concentration range of the 3,4- methylene-dioxy methcathinone standard solution is 0.005~0.5mg/mL.
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| SALOMÉ BALLESTEROS 等: "The risk of consuming "Bath Salts". Exemplification through four forensic cases in Spain", 《FORENSIC CHEMISTRY》 * |
| ZHENHUA QIAN 等: "Identification and analytical characterization of four synthetic cathinone derivatives iso-4-BMC, β-TH-naphyrone, mexedrone, and 4-MDMC", 《DRUG TESTING AND ANALYSIS》 * |
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