CN108535380A - A kind of detection method of new psychoactive drug substance MDBZP - Google Patents

A kind of detection method of new psychoactive drug substance MDBZP Download PDF

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Publication number
CN108535380A
CN108535380A CN201810325600.3A CN201810325600A CN108535380A CN 108535380 A CN108535380 A CN 108535380A CN 201810325600 A CN201810325600 A CN 201810325600A CN 108535380 A CN108535380 A CN 108535380A
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mdbzp
biological sample
concentration
gas
extracting solution
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常颖
赵阳
高利生
郑珲
张春水
翟晚枫
李彭
赵彦彪
郑晓雨
杨虹贤
刘克林
钱振华
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Institute of Forensic Science Ministry of Public Security PRC
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Institute of Forensic Science Ministry of Public Security PRC
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/72Mass spectrometers
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N2030/062Preparation extracting sample from raw material

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Abstract

The invention discloses a kind of detection methods of new psychoactive drug substance MDBZP.The qualitative and quantitative analysis methods such as method, including gas chromatography mass spectrometry, gas-chromatography, liquid chromatogram, LC-MS of MDBZP in accurate, efficient measurement biological sample provided by the present invention;Involved biological sample can be at least one of blood, urine, saliva and hair.Since the disturbing factor of biological sample is numerous, the pretreatment process of sample is extremely important.The present invention by solid phase extraction procedure, effectively fully extracts the MDBZP in biological sample, and realize efficient qualitative and quantitative analysis by a large amount of experiment;High sensitivity, the range of linearity of each analysis method are wide;Detector is at low cost, is conducive to the analysis operation of automation.

Description

A kind of detection method of new psychoactive drug substance MDBZP
Technical field
The present invention relates to a kind of detection methods of new psychoactive drug substance MDBZP, belong to criminal investigation illicit drugs inspection field.
Background technology
MDBZP (1- (3,4- methylenedioxy benzyl) piperazine) belongs to the new psychoactive drug substance of piperazines, and molecular formula is C12H18N2O2, molecular weight 190.29g/mol, shown in structural formula such as formula (1).It is peddled as designer drug, is that street corner is shaken the head A kind of ingredient of ball.But the stimulation of MDBZP is very weak, does not generate glad or hazy and illusionary effect.Side effect caused by it is Dizzy, nauseous and headache, high dose cause to twitch.
By consulting domestic and international lot of documents, report that MDBZP analysis methods include color reaction, crystallite experiment, thin layer Chromatography, gas chromatography, high performance liquid chromatography, Capillary Electrophoresis and Fourier are infrared etc..But it is more to have analysis method Lay particular emphasis on qualitative analysis.Simultaneously because during actually investigating, the detection object needed is mostly biological sample, such as blood, urine Liquid etc., biological sample have the characteristics that matrix is complicated, interference is more, difficult purification, very big puzzlement are brought for actually detected work.Therefore It is badly in need of a kind of accurate, efficient detection method for MDBZP in biological sample at present, to meet different demands.
Invention content
The object of the present invention is to provide a kind of accurate, efficient methods for measuring MDBZP in biological sample, including makings connection With, qualitative and quantitative analysis methods such as gas-chromatography, liquid chromatogram, LC-MS.
Biological sample according to the present invention can be at least one of blood, urine, saliva and hair.
Present invention firstly provides the gas chromatography mass spectrometry detection methods of MDBZP in biological sample, include the following steps:
(1) extraction biological sample obtains extracting solution;
(2) extracting solution is subjected to the gas chromatography mass spectrometry detection, if retention time is what 14.59~14.79min occurred The m/z of the corresponding fragment ion of absorption peak is 135.0 and 220.1, contains MDBZP in judging the biological sample.
The testing conditions of the gas chromatography mass spectrometry are as follows:
GC conditions:
Carrier gas is helium;
Chromatographic column is DB-5MS or HP-5MS;
Temperature program is:Initial temperature is 70 DEG C, rises to 300 DEG C with the rate of 10 DEG C/min, keeps 7min;
Mass Spectrometry Conditions:
Voltage scan range is 50~450M/z.
In above-mentioned gas chromatography mass spectrometry detection method, the biological sample is extracted using Solid Phase Extraction;
The condition of the Solid Phase Extraction is as follows:
Oasis HLB solid-phase extraction columns, specification can be 60mg, 3mL;
Use volume ratio for 1 first:1:1 methanol, deionized water and ammonium acetate (10mM, pH=9.5) pretreatment, such as For 2mL;Loading;It is cleaned with (1mL) deionized water, is then dried in vacuo;(1mL) methanol is used to elute again, nitrogen is blown to dry, uses methanol It redissolves.
The analysis time of the above-mentioned gas chromatography mass spectrometry detection method of the present invention controls within 30min, the separation between each substance For degree 2 or more, qualitative detection is limited to 2 μ g/mL.
The gas-chromatography detection method of MDBZP, includes the following steps in biological sample provided by the invention:
(1) extraction biological sample obtains extracting solution;
(2) standard solution is carried out gas chromatographic detection by the MDBZP standard solution for preparing at least five kinds of various concentrations, The peak area of the absorption peak corresponding to the MDBZP is obtained, is vertical with peak area with a concentration of abscissa of the standard solution Coordinate makes standard curve;
(3) extracting solution is subjected to gas chromatographic detection, obtains the peak area of the absorption peak corresponding to MDBZP, according to The standard curve is to get to the concentration of MDBZP in extracting solution;
The testing conditions of the gas-chromatography are as follows:
Carrier gas is nitrogen;
Chromatographic column is DB-5 or HP-5;
Column flow is 1.0mL/min;
Temperature program is:Initial temperature is 100 DEG C, rises to 140 DEG C with the rate of 18 DEG C/min, keeps 5min;Then with The rate of 50 DEG C/min rises to 280 DEG C, keeps 3min.
In above-mentioned gas-chromatography detection method, in the preparation method of the extracting solution and above-mentioned gas chromatography mass spectrometry detection method It is essentially identical;
Wherein, in above-mentioned gas-chromatography liquid detection method extracting solution preparation method Yu above-mentioned gas chromatography mass spectrometry detection method In it is essentially identical;
The concentration of the standard solution can be 0.001~1.0mg/mL.
The liquid chromatography detecting method of MDBZP, includes the following steps in biological sample provided by the invention:
(1) extraction biological sample obtains extracting solution;
(2) standard solution is carried out liquid chromatographic detection by the MDBZP standard solution for preparing at least five kinds of various concentrations, The peak area of the absorption peak corresponding to the MDBZP is obtained, is vertical with peak area with a concentration of abscissa of the standard solution Coordinate makes standard curve;
(3) extracting solution is subjected to the liquid chromatographic detection, obtains the peak face of the absorption peak corresponding to the MDBZP Product, according to the standard curve to get to the concentration of MDBZP described in the extracting solution;
The testing conditions of the liquid chromatogram are as follows:
Chromatographic column is C18 chromatographic columns, such as300SB-C18;
Column temperature is 35 DEG C;
Detection wavelength is 202nm;
Mobile phase A is the formic acid aqueous ammonium for a concentration of 10mM that pH value is 7, and Mobile phase B is acetonitrile, gradient elution, stream Speed is 1.0mL/min;
It is basic in the preparation method of extracting solution and above-mentioned gas chromatography mass spectrometry detection method in above-mentioned liquid chromatography detecting method It is identical;
The concentration of the standard solution can be 5~1000 μ g/mL;
The condition of the gradient elution is as follows:
The volume of 0~6min, the Mobile phase B are 20%;6.1min is raised to 60%;6.1~12min, the Mobile phase B Volume ratio be adjusted to 20% by 60%.
The liquid chromatograph mass spectrography detection method of MDBZP, includes the following steps in biological sample provided by the invention:
(1) extraction biological sample obtains extracting solution;
(2) standard solution is carried out liquid chromatography-mass spectrography by the MDBZP standard solution for preparing at least five kinds of various concentrations Combination detection obtains the peak area that ion pair is the absorption peak corresponding to 221.0-134.9, with a concentration of of the standard solution Abscissa makes standard curve using peak area as ordinate;
(3) extracting solution is subjected to the liquid chromatograph mass spectrography detection, it is 221.0-134.9 to obtain ion pair The peak area of corresponding absorption peak, according to the standard curve to get to the concentration of MDBZP described in the extracting solution;
The testing conditions of the liquid chromatograph mass spectrography are as follows:
Liquid phase chromatogram condition:
Chromatographic column is reverse phase C18 chromatographic columns;
Column temperature is 35 DEG C;
Mobile phase A is the aqueous formic acid that volumetric concentration is 0.1%, and Mobile phase B is acetonitrile, gradient elution, and flow velocity is 0.5mL/min;
Mass Spectrometry Conditions are:
Capillary outlet voltage is 100V;
The collision voltage of daughter ion 134.9 is 15V, and the collision voltage of daughter ion 77.1 is 45V;
Source parameters is:Dry temperature degree is 350 DEG C, dry gas stream amount 10L/min, and atomization gas pressure is 30psi.
In above-mentioned liquid chromatograph mass spectrography detection method, the preparation method of the extracting solution and above-mentioned gas chromatography mass spectrometry It is essentially identical in detection method;
A concentration of 1~10000ng/mL of the standard solution;
The condition of the gradient elution is as follows:
The volume ratio of 0~8min, the Mobile phase B are adjusted to 40% by 5%;8~8.01min, the body of the Mobile phase B Product by 40% than being adjusted to 5%.
Detection method has the following advantages:
(1) since the disturbing factor of biological sample is numerous, the pretreatment process of sample is extremely important.The present invention passes through A large amount of experiment, by solid phase extraction procedure, effectively fully extracts the MDBZP in biological sample, and realizes efficient Qualitative and quantitative analysis.
(2) high sensitivity of each analysis method, the range of linearity are wide.
(3) detector is at low cost, is conducive to the analysis operation of automation.
Description of the drawings
Fig. 1 is the gas chromatography mass spectrometry chromatogram of MDBZP in the embodiment of the present invention 1.
Fig. 2 is the gas chromatogram of MDBZP in the embodiment of the present invention 2.
Fig. 3 is the liquid chromatogram of MDBZP in the embodiment of the present invention 3.
Fig. 4 is the LC-MS collection of illustrative plates of MDBZP in the embodiment of the present invention 4.
Specific implementation mode
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.
MDBZP in embodiment 1, gas chromatography mass spectrometry detection urine sample
(1) preparation of sample solution
Using Oasis HLB solid-phase extraction columns (60mg, 3mL), 2mL methanol, 2mL deionized waters and 2mL acetic acid are used first Ammonium (10mM, pH=9.5) pre-processes.Loading, solid-phase extraction column are cleaned with 1mL deionized waters, are then dried in vacuo.With 1mL first Alcohol elutes, and nitrogen is blown to dry, is redissolved to 400 μ L, filter centrifugation with methanol, puts into sample bottle.
(2) setting of testing conditions
GC conditions set process as:
Carrier gas is helium;
Chromatographic column is DB-5MS or HP-5MS;
Temperature program is:Initial temperature is 70 DEG C, rises to 300 DEG C with the rate of 10 DEG C/min, keeps 7min;
Mass Spectrometry Conditions:Voltage scan range is set as 50~450M/z.
(3) gas chromatography mass spectrometry measurement and result
Using the condition Detection and Extraction liquid of above-mentioned setting, the retention time for obtaining 3 sample introductions of extracting solution is 14.69min left Fragment ion m/z corresponding to right absorption peak is 135.0 and 220.1, therefore, it is determined that containing MDBZP in urine sample.
The gas chromatography mass spectrometry chromatogram of MDBZP is as shown in Figure 1, wherein retention time is the suction at 14.69min in the present embodiment Attached peak is the absorption peak of MDBZP.
MDBZP in embodiment 2, gas chromatographic detection hair
(1) preparation of sample solution
With it is essentially identical in embodiment 1.
(2) preparation of standard working solution
Take MDBZP Standard Stock solutions, be diluted to successively mass concentration be respectively 1.0,0.5,0.25,0.125,0.1, 0.05, the series standard solution of 0.01,0.005,0.001mg/mL.
The 1 μ L sample introductions of titer of various concentration, the peak area of recording responses are taken respectively.
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 MDBZP:A=505.99c-49042, r2It is 0.9999, the range of linearity 5~1000 μ g/mL, 5 μ of detection limit g/mL(S/N≥3)。
(3) setting of testing conditions
Carrier gas is nitrogen;
Chromatographic column is DB-5 or HP-5;
Column flow is 1.0mL/min;
Temperature program is:Initial temperature is 100 DEG C, rises to 140 DEG C with the rate of 18 DEG C/min, keeps 5min;Then with The rate of 50 DEG C/min rises to 280 DEG C, keeps 3min.
(4) gas Chromatographic Determination and result
Using the condition Detection and Extraction liquid of above-mentioned setting, the average value of the peak area of 3 sample introductions of extracting solution is obtained (when reservation Between for the absorption peak corresponding to 10.79min), bring above-mentioned linear equation into, the concentration of MDBZP in extracting solution obtained, through converting To a concentration of 28.36 μ g/mL of MDBZP in hair.
The gas chromatogram of MDBZP is as shown in Figure 2 in the present embodiment.
The precision of the present embodiment detection method measures:The MDBZP samples for taking basic, normal, high 3 concentration, use the present embodiment The method established extracts analysis.Extraction and analysis 6 times in 1 day calculate the in a few days relative standard deviation (RSD) of sample;Even It is 5 days continuous, the relative standard deviation in the daytime of sample is calculated, the results are shown in Table 1.
The Precision test result of 1 various concentration MDBZP samples of table
The accuracy determination of the present embodiment detection method:Using sample-adding absorption method, 3 parts of the hair sample of known concentration is taken, Each 3 parts of the standard items of basic, normal, high three concentration are separately added into, are measured as stated above, it is 95.2% (n to acquire average recovery rate =3) 2, be the results are shown in Table.
2 rate of recovery of table (n=3)
MDBZP in embodiment 3, liquid chromatographic detection blood
(1) preparation of sample solution
With it is essentially identical in embodiment 1.
(2) preparation of standard working solution
Take MDBZP Standard Stock solutions, be diluted to successively mass concentration be respectively 1.0,0.75,0.5,0.1,0.05, 0.025, the series standard solution of 0.01,0.005,0.001,0.0005mg/mL.
The 10 μ L sample introductions of titer of various concentration, the peak area of recording responses are taken respectively.
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, The regression equation for obtaining MDBZP is A=7250.7c-75238, r2=0.9992,5~1000 μ g/mL of the range of linearity are quantitatively limited to 5 μg/mL(S/N≥3)。
(3) setting of testing conditions
Chromatographic column is300SB-C18 (4.6 × 150mm, 5 μm);
Column temperature is 35 DEG C;
Detection wavelength is 202nm;
Mobile phase A is the formic acid aqueous ammonium for a concentration of 10mM that pH value is 7, and Mobile phase B is acetonitrile, gradient elution, stream Speed is 1.0mL/min;
Mobile phase is put into 10~15min of ultrasound in ultrasonic cleaner using preceding after 0.45 μm of filtering with microporous membrane, fills Divide the gas in abjection mobile phase.
The condition of gradient elution is as follows:
The volume of 0~6min, Mobile phase B are 20%;6.1min is raised to 60%;6.1~12min, the volume ratio of Mobile phase B By 60% to 20%.
Using inner mark method ration, select caffeine as internal standard substance.
(4) liquid chromatogram measuring and result
Using the condition Detection and Extraction liquid of above-mentioned setting, the average value of the peak area of 3 sample introductions of extracting solution is obtained (when reservation Between for the absorption peak corresponding to 3.52min, as shown in Figure 3), bring above-mentioned linear equation into, obtain the dense of MDBZP in extracting solution Degree obtains a concentration of 28.12 μ g/mL of MDBZP in blood through conversion.
The precision of the present embodiment detection method measures:
The sample for taking basic, normal, high 3 concentration, analysis is extracted with the method that the present embodiment is established.It is extracted in 1 day Analysis 6 times, calculates the in a few days relative standard deviation (RSD) of sample;Continuous 5 days, the relative standard deviation in the daytime of sample is calculated, is tied Fruit is shown in Table 3.
The Precision test result of 3 various concentration sample of table
The accuracy determination of the present embodiment detection method:Using sample-adding absorption method, 3 parts of the blood sample of known concentration is taken, Each 3 parts of the standard items of basic, normal, high three concentration are separately added into, are measured as stated above, it is 96.7% (n to acquire average recovery rate =3) 4, are shown in Table.
4 rate of recovery of table (n=3)
MDBZP in embodiment 4, liquid chromatograph mass spectrography detection hair
(1) preparation of sample solution
With it is essentially identical in embodiment 1.
(2) preparation of standard working solution
Take MDBZP Standard Stock solutions, be diluted to successively mass concentration be respectively 1,5,10,50,100,500,1000, 5000, the series standard solution of 7500,10000ng/mL.
The 5 μ L sample introductions of titer of various concentration, the peak area of the 221.0-134.9 recording responses of selection are taken respectively.
Each concentration sample introduction 3 times, and linear regression is carried out to the average value A and mass concentration c (ng/ml) of 3 peak areas, The regression equation for obtaining MDBZP is A=222.69c+17275, r2=0.9994,1~10000ng/mL of the range of linearity, detection limit For 0.30ng/mL (S/N >=3), it is quantitatively limited to 1.00ng/mL (S/N >=10).
(3) setting of testing conditions
Mass Spectrometry Conditions set process as:
A. quasi-molecular ion is determined;
B. by selecting ion scan, optimize capillary outlet voltage;
C. it is scanned by daughter ion, selects daughter ion, while optimizing collision energy;
D. multiple-reaction monitoring MRM methods are established;
E. the optimization of source parameters.
Wherein, is optimized by Fragmentor voltages and CE values, is obtained optimal by selecting parent ion and daughter ion by MDBZP MRM parameters, to establish mass spectral database, as shown in table 5.
The mass spectral database of 5 MDBZP of table
Source parameters after optimization is:Dry 350 DEG C, dry gas stream amount 10L/min of temperature degree, atomization gas pressure are 30psi。
Liquid phase chromatogram condition:
Chromatographic column is reverse phase C18 chromatographic columns (2.1 × 150mm, 1.7 μm);
Column temperature is 35 DEG C;
Mobile phase A is the aqueous formic acid that volumetric concentration is 0.1%, and Mobile phase B is acetonitrile, condition of gradient elution such as table 6 Shown in, flow velocity 0.5mL/min.
6 condition of gradient elution of table
(4) liquid chromatogram measuring and result
Using the condition Detection and Extraction liquid of above-mentioned setting, the average value (221.0 of the peak area of 3 sample introductions of extracting solution is obtained → 134.9 ion pair), it brings above-mentioned linear equation into, obtains the concentration of MDBZP in extracting solution, obtained in hair through conversion A concentration of 252.08ng/mL of MDBZP.
In the present embodiment MDBZP LC-MS collection of illustrative plates as shown in figure 4, respectively 221.0 → 134.9 MRM collection of illustrative plates and 221.0 → 77.1 MRM collection of illustrative plates.
The precision of the present embodiment detection method measures:MDBZP samples are taken, are carried with the method that the present embodiment is established Take analysis.Extraction and analysis 6 times in 1 day are carried out continuously 5 days, and the results are shown in Table 7.
The Precision test result of 7 MDBZP of table

Claims (8)

1. the gas chromatography mass spectrometry detection method of MDBZP, includes the following steps in a kind of biological sample:
(1) extraction biological sample obtains extracting solution;
(2) extracting solution is subjected to the gas chromatography mass spectrometry detection, if retention time is the absorption that 14.59~14.79min occurs The m/z of the corresponding fragment ion at peak is 135.0 and 220.1, contains MDBZP in judging the biological sample;
The testing conditions of the gas chromatography mass spectrometry are as follows:
GC conditions:
Carrier gas is helium;
Chromatographic column is DB-5MS or HP-5MS;
Temperature program is:Initial temperature is 70 DEG C, rises to 300 DEG C with the rate of 10 DEG C/min, keeps 7min;
Mass Spectrometry Conditions:
Voltage scan range is 50~450M/z.
2. gas chromatography mass spectrometry detection method according to claim 1, it is characterised in that:The biological sample be blood plasma, serum, At least one of urine, saliva and hair;
The biological sample is extracted using Solid Phase Extraction.
3. the gas-chromatography detection method of MDBZP, includes the following steps in a kind of biological sample:
(1) extraction biological sample obtains extracting solution;
(2) standard solution is carried out gas chromatographic detection, obtained by the MDBZP standard solution for preparing at least five kinds of various concentrations The peak area of absorption peak corresponding to the MDBZP is vertical sit with peak area with a concentration of abscissa of the standard solution Mark makes standard curve;
(3) extracting solution is subjected to the gas chromatographic detection, obtains the peak area of the absorption peak corresponding to the MDBZP, According to the standard curve to get to the concentration of MDBZP described in the extracting solution;
The testing conditions of the gas-chromatography are as follows:
Carrier gas is nitrogen;
Chromatographic column is DB-5 or HP-5;
Column flow is 1.0mL/min;
Temperature program is:Initial temperature is 100 DEG C, rises to 140 DEG C with the rate of 18 DEG C/min, keeps 5min;Then with 50 DEG C/ The rate of min rises to 280 DEG C, keeps 3min.
4. gas-chromatography detection method according to claim 3, it is characterised in that:The biological sample be blood plasma, serum, At least one of urine, saliva and hair;
The biological sample is extracted using Solid Phase Extraction;
A concentration of 0.001~1.0mg/mL of the standard solution.
5. the liquid chromatography detecting method of MDBZP, includes the following steps in a kind of biological sample:
(1) extraction biological sample obtains extracting solution;
(2) standard solution is carried out liquid chromatographic detection, obtained by the MDBZP standard solution for preparing at least five kinds of various concentrations The peak area of absorption peak corresponding to the MDBZP is vertical sit with peak area with a concentration of abscissa of the standard solution Mark makes standard curve;
(3) extracting solution is subjected to the liquid chromatographic detection, obtains the peak area of the absorption peak corresponding to the MDBZP, According to the standard curve to get to the concentration of MDBZP described in the extracting solution;
The testing conditions of the liquid chromatogram are as follows:
Chromatographic column is C18 chromatographic columns;
Column temperature is 35 DEG C;
Detection wavelength is 202nm;
Mobile phase A is the formic acid aqueous ammonium for a concentration of 10mM that pH value is 7, and Mobile phase B is acetonitrile, gradient elution, and flow velocity is 1.0mL/min。
6. liquid chromatography detecting method according to claim 5, it is characterised in that:The biological sample be blood plasma, serum, At least one of urine, saliva and hair;
The biological sample is extracted using Solid Phase Extraction;
A concentration of 0.001~1.0mg/mL of the standard solution;
The condition of the gradient elution is as follows:
The volume of 0~6min, the Mobile phase B are 20%;6.1min is raised to 60%;6.1~12min, the body of the Mobile phase B Product by 60% than being adjusted to 20%.
7. the liquid chromatograph mass spectrography detection method of MDBZP, includes the following steps in a kind of biological sample:
(1) extraction biological sample obtains extracting solution;
(2) standard solution is carried out liquid chromatograph mass spectrography by the MDBZP standard solution for preparing at least five kinds of various concentrations Detection obtains the peak area that ion pair is the absorption peak corresponding to 221.0-134.9, with a concentration of horizontal seat of the standard solution Mark makes standard curve using peak area as ordinate;
(3) extracting solution is subjected to the liquid chromatograph mass spectrography detection, it is right for 221.0-134.9 obtains ion pair The peak area for the absorption peak answered, according to the standard curve to get to the concentration of MDBZP described in the extracting solution;
The testing conditions of the liquid chromatograph mass spectrography are as follows:
Liquid phase chromatogram condition:
Chromatographic column is reverse phase C18 chromatographic columns;
Column temperature is 35 DEG C;
Mobile phase A is the aqueous formic acid that volumetric concentration is 0.1%, and Mobile phase B is acetonitrile, gradient elution, flow velocity 0.5mL/ min;
Mass Spectrometry Conditions are:
Capillary outlet voltage is 90V;
The collision voltage of daughter ion 134.9 is 15V, and the collision voltage of daughter ion 77.1 is 45V;
Source parameters is:Dry temperature degree is 350 DEG C, dry gas stream amount 10L/min, and atomization gas pressure is 30psi.
8. liquid chromatograph mass spectrography detection method according to claim 7, it is characterised in that:The biological sample is At least one of blood plasma, serum, urine, saliva and hair;
The biological sample is extracted using Solid Phase Extraction;
A concentration of 1~10000ng/mL of the standard solution;
The condition of the gradient elution is as follows:
The volume ratio of 0~8min, the Mobile phase B are adjusted to 40% by 5%;8~8.01min, the volume ratio of the Mobile phase B It is adjusted to 5% by 40%.
CN201810325600.3A 2018-04-12 2018-04-12 A kind of detection method of new psychoactive drug substance MDBZP Pending CN108535380A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109655568A (en) * 2019-01-22 2019-04-19 杭州度安医学检验实验室有限公司 Efficient LC-MS measures the method and kit of 35 kinds of psychotropic agents simultaneously
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Application publication date: 20180914