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1.
Journal of Forensic Medicine ; (6): 176-185, 2023.
Article in English | WPRIM | ID: wpr-981852

ABSTRACT

Biological matrix reference material is a reference material that combines the target material with the biological matrix. The biological matrix reference material has higher consistency with the authentic specimens in forensic toxicology, and its application has a positive effect on improving the accuracy of test results. This paper reviews the research on the matrix reference materials corresponding to three common biological test materials (blood, urine and hair). In order to provide reference for the development and application of biological matrix reference materials in forensic toxicology, this paper mainly introduces the research progress of preparation technology of biological matrix reference materials and some existing products and their parameters evaluation.


Subject(s)
Forensic Toxicology/methods , Hair , Body Fluids
2.
Journal of Forensic Medicine ; (6): 168-175, 2023.
Article in English | WPRIM | ID: wpr-981851

ABSTRACT

Given the complexity of biological samples and the trace nature of target materials in forensic trace analysis, a simple and effective method is needed to obtain sufficient target materials from complex substrates. Magnetic nanoparticles (MNPs) have shown a wide range of application value in many research fields, such as biomedicine, drug delivery and separation, due to their unique superparamagnetic properties, stable physical and chemical properties, biocompatibility, small size, high specific surface area and other characteristics. To apply MNPs in the pretreatment of forensic materials, maximize the extraction rate of the target materials, and minimize interference factors to meet the requirements of trace analysis of the target materials, this paper reviews the application of MNPs in the fields of forensic toxicological analysis, environmental forensic science, trace evidence analysis and criminal investigation in recent years, and provides research ideas for the application of MNPs in forensic trace analysis.


Subject(s)
Magnetite Nanoparticles/chemistry , Forensic Medicine , Forensic Sciences , Forensic Toxicology
3.
Journal of Forensic Medicine ; (6): 151-160, 2023.
Article in English | WPRIM | ID: wpr-981849

ABSTRACT

OBJECTIVES@#To establish an LC-MS/MS method based on single hair micro-segmental technique, and verify the detection of 42 psychoactive substances in 0.4 mm hair segments.@*METHODS@#Each piece of single hair was cut into 0.4 mm segments and extracted by sonication and the segments were immersed in dithiothreitol-containing extraction medium. Mobile phase A was the aqueous solution containing 20 mmol/L ammonium acetate, 0.1% formic acid, and 5% acetonitrile. Mobile phase B was acetonitrile. An electrospray ionization source in positive ion mode was used for data acquisition in multiple reaction monitoring (MRM) mode.@*RESULTS@#The 42 psychoactive substances in hair had a good linear relationship within their respective linear ranges (r>0.99), the limits of detection were 0.2-10 pg/mm, the limits of quantification were 0.5-20 pg/mm, the intra-day and inter-day precisions were 1.5%-12.7%, the intra-day and inter-day accuracies were 86.5%-109.2%, the recovery rates were 68.1%-98.2%, and the matrix effects were 71.3%-111.7%. The method was applied to hair samples collected from one volunteer at 28 d after a single dose of zolpidem, with zolpidem detected in 5 hairs was 1.08-1.60 cm near the root tip, and the concentration range was 0.62-20.5 pg/mm.@*CONCLUSIONS@#The micro-segmental technique of single hair analysis can be applied to the investigation of drug-facilitated sexual assault cases.


Subject(s)
Humans , Chromatography, Liquid/methods , Zolpidem , Tandem Mass Spectrometry/methods , Hair , Acetonitriles , Chromatography, High Pressure Liquid
4.
Journal of Forensic Medicine ; (6): 144-150, 2023.
Article in English | WPRIM | ID: wpr-981848

ABSTRACT

OBJECTIVES@#To identify 1-(4-fluorophenyl)-2-(1-pyrrolidinyl) pentan-1-one (4-F-α-PVP) analog 1-(4-fluoro-3-methyl phenyl)-2-(1-pyrrolidinyl) pentan-1-one (4-F-3-Methyl-α-PVP) hydrochloride without reference substance.@*METHODS@#The direct-injection electron ionization-mass spectrometry (EI-MS), GC-MS, electrospray ionization-high resolution mass spectrometry (ESI-HRMS), ultra-high performance liquid chromatography-high resolution tandem mass spectrometry (UPLC-HRMS/MS), nuclear magnetic resonance (NMR), ion chromatography and Fourier transform infrared spectroscopy (FTIR) were integrated utilized to achieve the structural analysis and characterization of the unknown compound in the sample, and the cleavage mechanism of the fragment ions was deduced by EI-MS and UPLC-HRMS/MS.@*RESULTS@#By analyzing the direct-injection EI-MS, GC-MS, ESI-HRMS and UPLC-HRMS/MS of the compound in the samples, it was concluded that the unknown compound was a structural analog of 4-F-α-PVP, possibly with one more methyl group in the benzene ring. According to the analysis results of 1H-NMR and 13C-NMR, it was further proved that the methyl group is located at the 3-position of the benzene ring. Since the actual number of hydrogen in 1H-NMR analysis was one more than 4-F-3-Methyl-α-PVP neutral molecule, it was inferred that the compound existed in the form of salt. Ion chromatography analysis results showed that the compound contained chlorine anion (content 11.14%-11.16%), with the structural analysis of main functional group information by FTIR, the unknown compound was finally determined to be 4-F-3-Methyl-α-PVP hydrochloride.@*CONCLUSIONS@#A comprehensive method using EI-MS, GC-MS, ESI-HRMS, UPLC-HRMS/MS, NMR, ion chromatography and FTIR to identify 4-F-3-Methyl-α-PVP hydrochloride in samples is established, which will be helpful for the forensic science laboratory to identify this compound or other analog compounds.


Subject(s)
Benzene , Gas Chromatography-Mass Spectrometry/methods , Spectrometry, Mass, Electrospray Ionization , Chromatography, High Pressure Liquid/methods
5.
Journal of Forensic Medicine ; (6): 34-39, 2023.
Article in English | WPRIM | ID: wpr-984177

ABSTRACT

OBJECTIVES@#To establish a method for the detection of carbamazepine and its metabolites 10,11-dihydro-10,11-epoxycarbamazepine and 10,11-dihydro-10-hydroxycarbamazepine in blood samples by liquid chromatography-tandem mass spectrometry (LC-MS/MS).@*METHODS@#The blood samples were treated with 1-butyl-3-methylimidazolium hexafluorophosphate as an extraction solvent. The samples were extracted by ultrasound-assisted extraction and separated by ZORBAX Eclipse Plus C18, 95Å column. The mobile phase A aqueous solution containing 0.1% formic acid and 10 mmol/L ammonium acetate, and mobile phase B mixed organic solvent containing acetonitrile/methanol (Vacetonitrile∶Vmethanol=2∶3) were used for gradient elution at the flow rate of 1.00 mL/min. An electrospray ion source in positive mode was used for detection in the multiple reaction monitoring.@*RESULTS@#The linearities of carbamazepine and its metabolites 10,11-dihydro-10,11-epoxycarbamazepine and 10,11-dihydro-10-hydroxycarbamazepine in blood samples were good within the corresponding range, with correlation coefficients (r) greater than 0.995 6. The limits of detection were 3.00, 0.40 and 1.30 ng/mL, respectively. The limit of quantitation were 8.00, 1.00 and 5.00 ng/mL, respectively. The extraction recoveries ranged from 76.00% to 106.44%. The relative standard deviations of the intra-day and inter-day precisions were less than 16%. Carbamazepine and its main metabolite 10,11-dihydro-10,11-epoxycarbamazepine were detected in blood samples of death cases with a mass concentration of 2.71 μg/mL and 252.14 ng/mL, respectively.@*CONCLUSIONS@#This method has high sensitivity and good selectivity, which is suitable for the detection of carbamazepine and its metabolites in blood samples, and can be used for carbamazepine-related forensic identifications.


Subject(s)
Chromatography, Liquid/methods , Tandem Mass Spectrometry , Methanol , Carbamazepine/analysis , Benzodiazepines/analysis , Solvents , Chromatography, High Pressure Liquid , Solid Phase Extraction
6.
Journal of Forensic Medicine ; (6): 564-570, 2023.
Article in English | WPRIM | ID: wpr-1009388

ABSTRACT

OBJECTIVES@#To establish a method for the simultaneous quantitative analysis of etomidate and its metabolite etomidate acid in blood, and to discuss its application value in actual cases.@*METHODS@#Acetonitrile precipitate protein method was used, and C18 column was selected. Gradient elution was performed with acetonitrile and 5 mmol/L ammonium acetate within 6 min. Electrospray ionization source in positive ion mode was used. The internal standard etomidate acid-d5 was obtained by etomidate-d5 alkaline hydrolysis reaction. Ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was used for quantitative analysis. The methodological verification was conducted.@*RESULTS@#Etomidate and etomidate acid in blood showed good linear relationship in the quantitative linear range (r>0.999), with the lower limit of quantification was 2.5 ng/mL and 7.5 ng/mL, respectively. The accuracy, precision, recovery rate, and matrix effect of the method met the professional verification standards. The practical application results showed that etomidate and etomidate acid could be detected in the blood of the abusers, and their mass concentrations ranged from 17.24 to 379.93 ng/mL.@*CONCLUSIONS@#The method established in this study can simultaneously quantify etomidate and etomidate acid in blood, which is simple and convenient to operate with accuracy. It can meet the detection needs of actual cases and provide technical support for law enforcement to crack down on etomidate abuse.


Subject(s)
Chromatography, High Pressure Liquid/methods , Chromatography, Liquid , Etomidate , Tandem Mass Spectrometry/methods , Liquid Chromatography-Mass Spectrometry , Acetonitriles
7.
Journal of Forensic Medicine ; (6): 406-416, 2023.
Article in English | WPRIM | ID: wpr-1009373

ABSTRACT

In recent years, the types and quantities of fentanyl analogs have increased rapidly. It has become a hotspot in the illicit drug control field of how to quickly identify novel fentanyl analogs and to shorten the blank regulatory period. At present, the identification methods of fentanyl analogs that have been developed mostly rely on reference materials to target fentanyl analogs or their metabolites with known chemical structures, but these methods face challenges when analyzing new compounds with unknown structures. In recent years, emerging machine learning technology can quickly and automatically extract valuable features from massive data, which provides inspiration for the non-targeted screening of fentanyl analogs. For example, the wide application of instruments like Raman spectroscopy, nuclear magnetic resonance spectroscopy, high resolution mass spectrometry, and other instruments can maximize the mining of the characteristic data related to fentanyl analogs in samples. Combining this data with an appropriate machine learning model, researchers may create a variety of high-performance non-targeted fentanyl identification methods. This paper reviews the recent research on the application of machine learning assisted non-targeted screening strategy for the identification of fentanyl analogs, and looks forward to the future development trend in this field.


Subject(s)
Fentanyl , Substance Abuse Detection/methods , Mass Spectrometry/methods , Illicit Drugs/analysis
8.
Journal of Forensic Medicine ; (6): 388-392, 2023.
Article in English | WPRIM | ID: wpr-1009370

ABSTRACT

OBJECTIVES@#To establish a rapid method for the analysis of bucinnazine in blood by UPLC-MS/MS and to apply the method to the practical case.@*METHODS@#After the internal standard was added to blood, the protein was precipitated with 900 μL mixed solution (Vacetonitrile∶Vwater=8∶2). After vortex and centrifugation, the protein was measured through 0.22 μm filter membrane. The separation was performed on C18 chromatography column, with acetonitrile and 5 mmol/L ammonium acetate containing 0.1% formic acid aqueous as mobile phase gradient elution at the flow rate of 0.4 mL/min. Multiple reaction monitoring scan was performed in electrospray positive ion mode, quantitative measurement was performed by internal standard method, and methodological verification was carried out.@*RESULTS@#The linear relationship of bucinnazine in blood was good in the range of 0.5-200 μg/L, the correlation coefficient (r) was 0.999 7, the limit of detection was 0.1 μg/L, the limit of quantitation was 0.5 μg/L, and the recovery was 78.3%-83.8% at 1, 10 and 100 μg/L mass concentration levels. The matrix effect was 69.4%-73.8%, the intra-day precision was 1.9%-2.8%, and the inter-day precision was 2.8%-3.2%, the accuracy was 3.1%-3.5%. The stability test results of 1 and 100 μg/L mass concentrations at -25 ℃ showed that the accuracy (bias) of 10 d was less than 4.5%.@*CONCLUSIONS@#This method has the advantages of simple pre-treatment process, fast sample processing speed, high sensitivity of instrument analysis, good stability of content determination and reliable identification results, and can meet the needs of case identification.


Subject(s)
Tandem Mass Spectrometry/methods , Chromatography, Liquid , Chromatography, High Pressure Liquid/methods , Acetonitriles
9.
Chinese Journal of Industrial Hygiene and Occupational Diseases ; (12): 139-142, 2022.
Article in Chinese | WPRIM | ID: wpr-935762

ABSTRACT

Objective: To investigate the clinical significance of blood purification on changes in serum toxicant concentration and prognosis of acute benzene-based thinner poisoning. Methods: A total of 44 patients with acute benzene-based thinner poisoning admitted to the emergency department of Characteristic Medical Center of Armed Police from August 2013 to August 2020 were collected and divided into a blood purification group (24 cases) and a conventional treatment group (20 cases) , the general data, toxicant concentrations and prognosis of the two groups of patients were analyzed, and logistic regression analysis was performed on the influencing factors of the prognosis to explore the clinical effect of blood purification. Results: The concentration of poisons in the blood purification group at 24 hours after treatment was significantly lower than that in the conventional treatment group (t=6.76, P<0.001) , and the reduction in the concentration of poisons was significantly higher than that in the conventional treatment group (t=3.33, P=0.002) . The overall improvement rate in the blood purification group was 91.7% (22/24) , which was higher than that in the conventional treatment group (60.0%, 12/20) . Logisitic regression analysis showed that blood purification treatment method was the main factor affecting the prognosis of patients (OR=7.605×10(-5), 95%CI: 6.604×10(-8)-0.087, P=0.008) , and the toxic dose was a synergistic effect on the prognosis of patients factor (OR=1.038, 95%CI: 1.008-1.068, P=0.011) . Conclusion: Early blood purification treatment in patients with acute benzene-based thinner poisoning can rapidly reduce blood toxin concentration, avoid disease progression, and ultimately improve patient prognosis.


Subject(s)
Humans , Benzene , Hazardous Substances , Poisoning/therapy , Prognosis , Retrospective Studies
10.
Journal of Forensic Medicine ; (6): 726-732, 2022.
Article in English | WPRIM | ID: wpr-984164

ABSTRACT

OBJECTIVES@#To analyze the chemical structure of the interfering substance that affects the result of methamphetamine analysis in wastewater.@*METHODS@#A combination of GC-MS and liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) was used to analyze the mass spectrum characteristics of the interfering substance that affects the result of methamphetamine analysis and to infer its possible structure. Liquid chromatography-triple quadrupole-mass spectrometry (LC-TQ-MS) was used to confirm the control material.@*RESULTS@#Using LC-QTOF-MS in positive electrospray ionization (ESI+) mode, the mass-to-charge ratio (m/z) of quasi-molecular ion in the MS1 mass spectrometry of interfering substance was identical to that of methamphetamine, indicating that the interfering substance was probably an isomer of methamphetamine. The MS2 mass spectra obtained at three collision energies of 15 V, 30 V and 45 V were highly similar to methamphetamine, suggesting that the interfering substance contained methylamino and benzyl groups. Further analysis using GC-MS in electron impact (EI) ionization mode showed that the base peak in the mass spectrum of the interfering substance was at m/z 44. The interfering substance was confirmed to be N-methyl-2-phenylpropan-1-amine by compared with the standard reference.@*CONCLUSIONS@#The chemical structure of N-methyl-2-phenylpropan-1-amine is highly similar to methamphetamine, which is easy to cause interference for the detection of trace amounts of methamphetamine in wastewater using LC-TQ-MS. Therefore, in the actual analysis, the chromatographic retention time can be used to distinguish between N-methyl-2-phenylpropan-1-amine and methamphetamine.


Subject(s)
Methamphetamine , Wastewater , Amines , Gas Chromatography-Mass Spectrometry/methods , Mass Spectrometry/methods , Spectrometry, Mass, Electrospray Ionization/methods
11.
Journal of Forensic Medicine ; (6): 473-477, 2022.
Article in English | WPRIM | ID: wpr-984138

ABSTRACT

OBJECTIVES@#To establish a method to identify unknown sample based on the combined use of Fourier transform infrared spectroscopy (FTIR), gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF-MS), ultra-high performance liquid chromatography-linear ion trap quadrupole-orbitrap mass spectrometry (UPLC-LTQ-Orbitrap MS) and 1H-nuclear magnetic resonance spectroscopy (1H-NMR) technique.@*METHODS@#The unknown sample was directly analyzed by FTIR. The unknown sample was dissolved in methanol solution containing internal standard SKF525A and the supernatant was detected by GC-QTOF-MS and UPLC-LTQ-Orbitrap MS. The unknown sample was dissolved in methanol-d4 solution for structural analysis of 1H-NMR.@*RESULTS@#The characteristic absorption peaks of FTIR spectra obtained from unknown sample were 1 682 (C=O bond), 1 503, 1 488, 1 436, 1 363, 1 256, 1 092, 1 035, 935, 840 and 800 cm-1, the characteristic fragment ions (m/z) of GC-QTOF-MS were 86.096 4 (base peak), 58.065 1, 149.023 5, 121.028 6 and 65.038 6, the accurate mass [M+H]+ detected by UPLC-LTQ-Orbitrap MS was 236.127 7. The sample was identified as synthetic cathinone new psychoactive substance Eutylone by 1H-NMR.@*CONCLUSIONS@#The method established in this study can be used for structural confirmation of Eutylone.


Subject(s)
Methanol , Chromatography, High Pressure Liquid/methods , Mass Spectrometry , Gas Chromatography-Mass Spectrometry/methods , Magnetic Resonance Spectroscopy
12.
Journal of Forensic Medicine ; (6): 516-523, 2021.
Article in Chinese | WPRIM | ID: wpr-985242

ABSTRACT

Objective To establish a method combining QuEChERS and ultra-high liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for rapid screening and testing of three types of new psychoactive tryptamines in human blood: 5-MeO-DALT, 5-MeO-MiPT and 5-MeO-DiPT. Methods The effects of the type of extractant, the type and dosage of salting-out agent, and the dosage of adsorbent on the test results of the three tryptamines were investigated. Blood samples were processed by QuEChERS method and then determined by UPLC-MS/MS. Results The linear relationships of 5-MeO-DALT, 5-MeO-MiPT and 5-MeO-DiPT in human blood were good in the range of 0.5-100, 0.5-100 and 0.2-100 ng/mL, respectively, with their coefficients higher than 0.99. The limits of detection (LODs) were 0.1-0.2 ng/mg. The recoveries ranged from 84.86% to 94.57%. Intra-day and inter-day precisions were good. Conclusion The method is simple, rapid, easy to operate and has a high recovery. It is suitable for the qualitative and quantitative study of tryptamines in blood and can provide the reference for public security organs to deal with related cases.


Subject(s)
Humans , Chromatography, High Pressure Liquid , Chromatography, Liquid , Limit of Detection , Tandem Mass Spectrometry , Tryptamines
13.
Journal of Forensic Medicine ; (6): 511-515, 2021.
Article in Chinese | WPRIM | ID: wpr-985241

ABSTRACT

Objective To detect the uncontrolled new psychoactive tryptamines involved in drug-related cases with high resolution mass spectrometry and nuclear magnetic resonance spectroscopy. Methods White and brown powder obtained in actual cases were extracted and analyzed by gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF-MS), ultra-high performance liquid chromatography-linear ion trap quadrupole-orbitrap mass spectrometry (UPLC-LTQ-Orbitrap MS) and 1H-nuclear magnetic resonance spectroscopy (1H-NMR). Results After detection by GC-QTOF-MS, the components of white powder showed main characteristic fragment ion peaks at m/z 218.141 0 (molecular ion peak), 72.080 6 (base peak), etc. After detection by UPLC-LTQ-Orbitrap MS, its protonated molecular ion was m/z 219.149 4. The main ions in the secondary mass spectrum under the collision-induced dissociation (CID) mode were m/z 160.076 3 and 72.080 8. After detection by GC-QTOF-MS, the components of brown powder showed main characteristic fragment ion peaks at m/z 246.135 7 (molecular ion peak), 58.065 1 (base peak), etc. After detection by UPLC-LTQ-Orbitrap MS, its protonated molecular ion was m/z 247.145 0. The main ions in the secondary mass spectrum under CID mode were m/z 202.087 1, 160.076 3 and 134.060 5. NIST 17 library retrieval and 1H-NMR confirmed that the white powder and brown powder contained new psychoactive tryptamines 4-OH-MET and 4-AcO-DMT, respectively. Conclusion GC-QTOF-MS, UPLC-LTQ-Orbitrap MS and 1H-NMR can be used together to identify unknown new psychoactive substances.


Subject(s)
Chromatography, High Pressure Liquid , Gas Chromatography-Mass Spectrometry , Magnetic Resonance Spectroscopy , Mass Spectrometry , Tryptamines
14.
Journal of Forensic Medicine ; (6): 505-510, 2021.
Article in Chinese | WPRIM | ID: wpr-985240

ABSTRACT

Objective To establish a method that combines a series of techniques including Fourier transform infrared spectrum (FTIR), gas chromatography-mass spectrometry (GC-MS), high resolution mass spectrometry and nuclear magnetic resonance spectroscopy (NMR) for identification of unknown substances. Methods The unknown samples (off-white powder and yellow crystal) seized in the actual cases were detected by FTIR, GC-MS (methanol as solvent), high resolution mass spectrometry (methanol as solvent) and NMR (deuterated methanol as solvent). Results The mass spectrum characteristic ions m/z of the main components in the samples measured by GC-MS were 219 (base peak), 363, 307, 304, 275, 145, 131 and 213 (base peak), 357, 301, 298, 269, 185, 171, 145 and 131, respectively. The accurate mass numbers [M+H]+ measured by high resolution mass spectrometry were 364.203 61 and 358.212 34, respectively. The unknown samples were identified as synthetic cannabinoid new psychoactive substances 4F-MDMB-BUTINACA and MDMB-4en-PINACA after data consultation and database retrieval and comparison, combined with infrared analysis and mass spectrometry data analysis, and their structures were confirmed by 1H-NMR. Conclusion The established multi-technology joint identification method can be used to identify 4F-MDMB-BUTINACA and MDMB-4en-PINACA in unknown samples. This method is fast, convenient, accurate, reliable and practical, and can provide reference for the identification of cases involving such substances in the future.


Subject(s)
Cannabinoids , Gas Chromatography-Mass Spectrometry , Illicit Drugs , Magnetic Resonance Spectroscopy , Mass Spectrometry
15.
Journal of Forensic Medicine ; (6): 500-504, 2021.
Article in Chinese | WPRIM | ID: wpr-985239

ABSTRACT

Objective To establish an ion chromatography method for the salt form determination of new psychoactive substances (NPS). Methods The method of conducting qualitative and quantitative analysis of six types of organic acid ions (acetate ion, tartrate ion, maleate ion, oxalate ion, fumarate ion, citrate ion) and five types of inorganic anions (fluoride ion, chloride ion, nitrate ion, sulfate ion, phosphate ion) in NPS sample by ion chromatography was developed. The salt forms of 222 seized NPS samples (103 samples with synthetic cannabinoids, 81 samples with cathinones, 44 samples with phenylethylamines, 12 samples with tryptamines, 7 samples with phencyclidines, 6 samples with piperazines, 2 samples with aminoindenes, 26 samples with fentanyls and 43 samples with other types of NPS) were analyzed by this method. Results Each anion had good linearity in the corresponding linear range, the correlation coefficients (r) were greater than 0.999, the limits of detection were 0.01-0.05 mg/L, and the limits of quantitative were 0.1-0.5 mg/L. Except that 5F-BEPIRAPIM was hydrochloride, the salt forms of the other 102 synthetic cannabinoids were all base. The salt form of 81 cathinone samples, 44 phenylethylamine samples, 7 phencyclidine samples and 2 aminoindene samples were all hydrochloride. The salt forms of tryptamine samples included base, hydrochloride, fumarate and oxalate. The salt forms of piperazine samples included base and hydrochloride. The salt forms of fentanyl samples and samples of other types included base, hydrochloride and citrate. Conclusion Ion chromatography is a simple, accurate and efficient method for determining the salt form of NPS samples, which makes the qualitative and quantitative conclusions of NPS more scientific and rigorous.


Subject(s)
Chromatography, Liquid , Gas Chromatography-Mass Spectrometry , Ions , Psychotropic Drugs/chemistry
16.
Journal of Forensic Medicine ; (6): 493-499, 2021.
Article in Chinese | WPRIM | ID: wpr-985238

ABSTRACT

Objective To study the metabolic transformation pathways of 4F-MDMB-BUTINACA in vivo by establishing zebrafish models. Methods Six adult zebrafish were randomly divided into blank control group and experimental group, with three fish in each group. After the zebrafish in the experimental group were exposed to 1 μg/mL 4F-MDMB-BUTINACA for 24 h, they were transferred to clean water and cleaned three times, then pretreated for instrumental analysis. The zebrafish in blank control group were not exposed to 4F-MDMB-BUTINACA. Mass spectrometry and structural analysis of 4F-MDMB-BUTINACA and its metabolites were conducted by liquid chromatography-high resolution mass spectrometry and Mass Frontier software. Results A total of twenty-six metabolites of 4F-MDMB-BUTINACA were identified in zebrafish, including eighteen phase Ⅰ metabolites and eight phase Ⅱ metabolites. The main metabolic pathways of phase Ⅰ metabolites of 4F-MDMB-BUTINACA in zebrafish were ester hydrolysis, N-dealkylation, oxidative defluorination and hydroxylation, while the main metabolic pathway of phase Ⅱ metabolites was glucuronidation. Conclusion Metabolite Md24 (ester hydrolysis) and Md25 (ester hydrolysis combined with dehydrogenation) would be recommended to be potentially good biomarkers for abuse of 4F-MDMB-BUTINACA.


Subject(s)
Animals , Cannabinoids , Chromatography, Liquid , Illicit Drugs , Microsomes, Liver/chemistry , Zebrafish
17.
Journal of Forensic Medicine ; (6): 486-492, 2021.
Article in Chinese | WPRIM | ID: wpr-985237

ABSTRACT

Objective To study the qualitative analysis strategy for unknown synthetic cannabinoid in the suspicious herbal product when no reference substance is available. Methods The synthetic cannabinoid in herbal blend was extracted with methanol. The extract was concentrated by rotary evaporator and separated and purified by preparative liquid chromatography, to obtain high purity synthetic cannabinoid sample. Gas chromatography-mass spectrometry (GC-MS), ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) and nuclear magnetic resonance (NMR) were used to determine the structure of the prepared compound. Results High purity unknown sample (10 mg) was obtained by preparative liquid chromatography. The sample was analyzed by GC-MS, UPLC-TOF-MS and NMR, and through spectrum analysis, the unknown synthetic cannabinoid was determined as 5F-EDMB-PICA. Conclusion The method to extract unknown synthetic cannabinoid from low content herbal products by preparative liquid chromatography was established, and the structure of the unknown sample was identified by comprehensive use of GC-MS, UPLC-QTOF-MS and NMR. The information will assist forensic laboratories in identifying this substance or other compounds with similar structures in their casework.


Subject(s)
Cannabinoids , Chromatography, High Pressure Liquid , Chromatography, Liquid , Gas Chromatography-Mass Spectrometry , Mass Spectrometry
18.
Journal of Forensic Medicine ; (6): 479-485, 2021.
Article in Chinese | WPRIM | ID: wpr-985236

ABSTRACT

Objective To establish a detection method for common new psychoactive substances of synthetic cannabinoids in hair with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods In the 1 mL of internal standard methanol solution, 20 mg hair was added. After cryogenic grinding and ultrasonic extraction, the extract was separated by ACQUITY UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm). The mobile phase A was aqueous solution that composed of 20 mmol/L ammonium acetate, 0.1% formic acid, and 5% acetonitrile. The mobile phase B was acetonitrile. Electrospray ionization source in positive ion mode was used for data acquisition in multi-reaction monitoring (MRM) mode. Results The seven common new psychoactive substances of synthetic cannabinoids in hair had a good linear relationship within their respective linear ranges (r>0.99), the limits of detection were 0.5-2 pg/mg, the limits of quantification were 1-5 pg/mg, the intra-day and inter-day precisions were 0.1%-12.6%, the intra-day and inter-day accuracies were 89.2%-110.7%, the recovery rates were 52.3%-93.3%, and the matrix effects were 19.1%-95.2%. Conclusion The established method has a simple sample preparation process and high sensitivity. It is suitable for qualitative and quantitative analysis of common new psychoactive substances of synthetic cannabinoids in hair.


Subject(s)
Cannabinoids , Chromatography, High Pressure Liquid , Chromatography, Liquid , Hair , Tandem Mass Spectrometry
19.
Journal of Forensic Medicine ; (6): 470-478, 2021.
Article in Chinese | WPRIM | ID: wpr-985235

ABSTRACT

In recent years, as the third-generation of drugs, new psychoactive substances (NPS) have expanded rapidly and become a serious concern for China's anti-drug prevention and control system. As a new drug monitoring technology in the current anti-drug field, wastewater analysis is an objective, real-time, accurate, convenient and effective drug monitoring method. In recent years, it has gradually been applied to the monitoring of NPS. This study summarizes wastewater sample collection, target stability research, wastewater sample pretreatment, wastewater sample analysis methods, target NPS consumption calculations and actual monitoring applications, with a view to the construction of a monitoring system for NPS in wastewater, real-time and accurate grasp of information on the use of NPS in cities, the reflection of the actual consumption of different types of NPS and consumption trends in a short period of time, and prediction of the development trend of abused use, which is of great significance for combating NPS crimes, serving and guaranteeing the personal safety of the people, and maintaining social stability.


Subject(s)
China , Cities , Illicit Drugs/analysis , Psychotropic Drugs/analysis , Wastewater/analysis , Water Pollutants, Chemical/analysis
20.
Journal of Forensic Medicine ; (6): 459-459, 2021.
Article in Chinese | WPRIM | ID: wpr-985234

ABSTRACT

Synthetic cannabinoids are currently a class of new psychoactive substances with the largest variety and most abused. Metabolite identification research can provide basic data for monitoring synthetic cannabinoids abuse, which is the current research hotspot. The main trend of structural modification of synthetic cannabinoid is to replace the fluorine atom on pentyl indole or indazole cyclopentyl with hydrogen atom, which greatly improves the biological activity of the compound. The main metabolic reactions include hydroxylation, fluoropentyl oxidative, ester hydrolyze, amide hydrolysis. Liquid chromatography-high resolution mass spectrometry has become the preferred choice for the structural identification of metabolites. This review mainly summarizes research on metabolism software prediction and human hepatocyte model, human liver microsomes model, rat in vivo model, zebrafish model and fungus C. elegans model in metabolite identification based on the structure and classification of synthetic cannabinoids.


Subject(s)
Animals , Rats , Caenorhabditis elegans , Cannabinoids , Chromatography, Liquid , Microsomes, Liver/chemistry , Zebrafish
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