„PARTY DRUGS“ TESTING ON THE DANCE FLOOR ...€žPARTY DRUGS“ TESTING ON THE DANCE FLOOR:...
1
HPLC (measurement apparatus) For chemical analysis of party drugs separation and detection of different constituents of mix- tures (active ingredients and fillers) is necessary. With the mobile lab we are using High Per- formance Liquid Chromatography (HPLC) for the separation process. Our computer controlled HPLC-systems are equipped with DAD/UV-Vis Spectrometers (Diode Array Detector). Chemical analysis of “Party Drugs“ gives one of three possible results. The findings may be a single active agent, several active agents, or indeed no active agent. Reliable analysis of the substances in a sample cannot be achieved by means of a simple “quick test“ and is only possi- ble by the use of a complex measurement chain, as shown in the following basic diagram: Chemical analysis requirements HPLC-System Autosampler: HP-1100, Typ G1389A Pump: HP-1100, Binary Pump, Typ G1376A Detector: HP-1100, UV-Vis DAD-Detector, Typ G1315B Intrument control & integration ChemStation for LC 3D software HPLC- Conditions Stationary phase: Spherisorb 80-3 ODS-1 (Waters) Column dimension: 125 x 4.0 mm Hold-up volume: 1.002 ml Elutiontype: Gradient Eluent A 8,50 g ortho-phosphoric acid 85% + 280 µl hexylamine + purified water ad 1000 ml Eluent B 4,25 g ortho-phosphoric acid 85% + 140 µl hexylamine + 45,75 g purified water + 351 g acetonitrile Gradient program Time in min % A %B 0 – 2.5 95 5 2.5 – 9 95 - 60 5 - 40 9 – 13.5 60 40 13.5 – 14 60 - 95 40 - 5 14 – 16.5 90 5 Measuring parameters: Flowrate: 1 ml/min Pressure: 150 bar Injection volume: 2.5 μl Column temperature: 40 °C Detection: UV 198 nm Signal-Range: 190-400 nm Analytical method Health & Social Welfare Department State of Berne Office of the Cantonal Pharmacist Daniel Allemann, Hans Pauli, André Mürner, Lukas Mürner, Michael Staub, Fabienne Holzer, Hans-Jörg Helmlin, Samuel Steiner Dr. H.-J. Helmlin, MBA, Ph D Head Laboratory KAPA State of Berne Baltzerstrasse 5 CH-3012 Berne Switzerland e-mail: [email protected] Daniel Allemann Laboratory KAPA State of Berne Baltzerstrasse 5 CH-3012 Berne Switzerland e-mail: [email protected] Contacts: This arrangement applies to most modern chemical-analysis measurement systems. Update: 31.12.2016 Update: 31.12.2016 Flow diagram Collaboration between the prevention-teams and the laboratory Separation EDP- system Sample Input system Sample preparation Detector- system Measurement apparatus Analysis sequence Results „PARTY DRUGS“ TESTING ON THE DANCE FLOOR: EQUIPMENT, METHODS AND RESULTS Information stands at the party Sample- documentation HPLC- analysis Database Result quantification calibration known active substance unknown active substance HPLC-analysis (mobile) Questionnaire (anonymous) Identification Measurement data Extraction Measuring/weighing Photography Coding Information Prevention message Pharmaceutical Control Laboratory Bern (within 1-4 days) Laboratory measurements GC/MS, LC/MS, IR E-mail Telephone (Telephone) 10-15 mg Sample- material Sample Database Ravers Office Mülhauserstrasse 111 4056 Basel Office Wasserwerk- strasse 17 8006 Zürich Office Monbijoux- strasse 70 3007 Bern Introduction Since 1998 the mobile lab unit of the Office of the Cantonal Pharmacist (Health & Social Welfare Department, State of Berne, Switzerland) is testing so called „Party Drugs“ on the dance floor. At more than 160 events the team has tested over 3400 samples in cooperation with „Streetwork Zurich“, „Contact Bern“ and „Suchthilfe Region Basel“. The mobile lab consists of four custom made subunits mounted in steel framed racks on wheels, one for weighing and documentation, one for sample prepara- tion and two with the equipment for che- mical analysis (HPLC-DAD). The lab is operated by two experienced technicians. Before analysis the intere- sted customer is asked by the lab crew to fill out a questionnaire concerning in- formation about the sample; thereafter every sample is digitally documented and characterized by physical appearance (form, weight, dimensions etc.). Report Analytical results are available within about 20 minutes. The computer prints the results of the analysis as a report. The report consists of 3 parts: The header, the chromatogram, and the results (including identification and quantification) Header: The header contains details like: File- name, sample-number, date of analysis, name of method etc. Chromatogram: The chromatogram is a graphic visualisa- tion of the separation process. Detected substances appear as “Peaks”. Results (identification and quantification): The system compares the area-value of an integrated Peak with the correspondi- ng calibration of the active substance in the specified methods. This automatic process gives us a precise quantification. Additionally it is possible to get the UV- spectra of the “Peak” and compare it with our specific UV- Spectra-library. Sample preparation: Due to the very sensitive analytical methods, only a representative part of the sample is used for further analysis. Sample preparation is quick and effective. The material is pulverised in a mor- tar and dissolved in methanol with the aid of an ultrasonic extractor. Bottles with mobile phase (solvent mix) HPLC- Pump (Part of the separation-system). This high-pressure pump delivers the solvent (with the dissolved sample) through the separating column to the detector. Autosampler The autosampler transfers the prepared sample from the vial into the measurement apparatus. HPLC-column The “central unit“ of the HPLC-system serves to separate dis- solved mixtures of substances into their constituents. Detector The chemical detector is positioned at the end of the co- lumn. It is the highly sensitive “eye“ of the measurement chain and records sub- stances which absorb ultra-violet light when they pass trough the detector cell dissolved in the mobile phase. The detec- tor provides two kinds of information about the molecules measured: their identity and their quantity. The whole process is continuously monitored with a computer system. Measurement signals are converted into graphical displays appearing on the computer screen. The two most important displays are the chromatogram and the UV-spectrum. The chromatogram is a representation of the separation process. The UV- spectrum is a characteristic constant for a particular substance. An internal standard is added as control. In most cases this extract still contains insoluble com- ponents, which must be filtered off before analysis. The clear sample solution obtained is trans- ferred into a sample vial. 'Additives' in cocaine samples (n = 604) Cocaine content in % (n = 604) Frequency of occurrence of different pharmaceutical substances in cocaine samples Variation of MDMA-dose in tablets (mg/tablet) Quantitative comparison Variation of Amphetamine and Caffeine amount in powders (in weight-%) Chemical substances detected Chemical substance Count Frequency of occurrence [%] MDMA 1586 46.44 Caffeine 871 25.51 Amphetamine 790 23.13 Cocaine 607 17.77 Levamisole 277 8.11 Phenacetin 260 7.61 m-CPP 96 2.81 Lidocaine 66 1.93 no active ingredient 58 1.70 LSD 54 1.58 Ketamine 46 1.35 Amphetamine synthesis by-product 45 1.32 2C-B 43 1.26 Phenylacetone 43 1.26 Domperidone 41 1.20 unknown 40 1.17 MDA 35 1.02 MDEA 32 0.94 Paracetamol 32 0.94 Methamphetamine 28 0.82 Metoclopramide 22 0.64 Acetylsalicylic acid 21 0.61 Heroin 19 0.56 Noscapine 19 0.56 3,4-Methylendioxyphenyl-2-propanol 14 0.41 4-Methylamphetamin 13 0.38 iso-LSD 13 0.38 Hydroxyzine 12 0.35 Mescaline 12 0.35 Creatin 11 0.32 Ephedrine 11 0.32 p-Fluoroamphetamine 11 0.32 Benzocaine 10 0.29 Buflomedil 10 0.29 Tetracaine 10 0.29 Procaine 9 0.26 Salicylic acid 9 0.26 N-Formylamphetamine 7 0.20 Cimetropium bromide 5 0.15 Diltiazem 5 0.15 Mephedrone 5 0.15 related substance 5 0.15 TFMPP 5 0.15 Vanillin 5 0.15 Benzylpiperazine (A2) 4 0.12 Methylone (bk-MDMA) 4 0.12 Methylphenidate 4 0.12 2C-H 3 0.09 2C-H 3 0.09 DOC 3 0.09 MDMA synthesis by-product 3 0.09 MDPV 3 0.09 2C-E 2 0.06 3,4-Methylenedioxyphenylacetonitrile 2 0.06 3-Methylmethcathinone (3-MMC) 2 0.06 4-Methylethylcathinon (4-MEC) 2 0.06 6-Monoacetylmorphin 2 0.06 Butylone (bk-MBDB) 2 0.06 Ethcathinone 2 0.06 MDDM 2 0.06 MDHOET 2 0.06 PMMA 2 0.06 Pseudoephedrine 2 0.06 Sucrose octaacetate 2 0.06 TMA-2 2 0.06 Triprolidine 2 0.06 1-Benzyl-4-Methylpiperazin (MBZP) 1 0.03 2C-i 1 0.03 4-Chloroethcathinone 1 0.03 4-Chloromethcathinone 1 0.03 Amoxicillin 1 0.03 Atropine (Hyoscyamine) 1 0.03 Bisoprolol 1 0.03 Chloroquine 1 0.03 Clozapine 1 0.03 Desloratadine 1 0.03 Dextromethorphan (DXM) 1 0.03 Dimethyl terephthalate 1 0.03 DMT 1 0.03 DOI 1 0.03 Erdosteine 1 0.03 Ergotamine 1 0.03 Flephedrone 1 0.03 gamma-Butyrolactone 1 0.03 Isoniazid 1 0.03 Medicament 1 0.03 Metamizol 1 0.03 Metandienone 1 0.03 Methaqualone 1 0.03 Niacin (Vitamin) 1 0.03 N-Methylbenzylamin 1 0.03 N-Methylephedrine 1 0.03 Oxycodon 1 0.03 Pentedrone 1 0.03 Phenobarbital 1 0.03 Piperonal 1 0.03 Piracetam 1 0.03 Propranolol 1 0.03 Propyphenazone 1 0.03 Scopolamine 1 0.03 Scopolamine derivative 1 0.03 Tadalafil 1 0.03 Theophylline 1 0.03 Tryptophan 1 0.03 Xylazine 1 0.03 Capsules (n = 47) others 10% LSD 2% m-CPP 2% Cocaine 18% Amphetamine 22% MDMA 46% Active ingredients (all samples) (n = 3415) Active ingredients (evolution time based) Galenical forms (all samples) (n = 3415) Galenical forms (MDMA samples) (n = 1560) Tablets (n = 1355) Powders (n = 1950) Mean (n = 1094) = 99.6 mg/tablet Max = 268.0 mg (n = 759) Frequency of occurrence Qualitative results 0 10 20 30 40 50 60 70 80 90 100 2001- 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016 72 64 54 53 49 48 51 29 41 46 48 39 44 39 36 17 11 25 24 19 22 13 18 25 22 22 25 30 26 22 3 14 11 12 19 10 15 22 16 19 14 22 14 23 30 1.6 6.0 1.1 5.9 19.3 5.9 2.0 0.4 0.3 2.0 2.5 1.5 3.2 3.3 3.4 2.7 7 10 10 10 8 19 15 11 10 7 15 10 8 8 9 Frequency of occurrence [%] Year MDMA Amphetamine Cocaine m-CPP LSD others only tablets with dose > 5 mg/tablet (n = 1094) 0 10 20 30 40 50 60 70 80 90 100 2001- 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016 Frequency of occurrence [%] Year Phenacetin Levamisole Benzocaine / Lidocaine / Procaine / Tetracaine Diltiazem Caffeine MDMA 47% Amphetamine 2% Ephedrine 9% Methamphetamine 2% Methylphenidate 2% Benzylpiperazine (A2) 2% TFMPP 2% TFMPP + Benzylpiperazine 2% 2C-B 2% Mephedrone 4% Methylon (bk-MDMA) 4% Mescaline 2% TMA-2 2% Scopolamine derivative 2% Cathine 2% Caffeine 2% unknown 6% no active ingredient 4% 0 10 20 30 40 50 60 70 80 90 100 2001- 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016 Frequency of occurrence [%] Year Tablet Powder Capsule Blotter Drops other 0 10 20 30 40 50 60 70 80 90 100 2001- 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016 Frequency of occurrence [%] Year Tablet Powder Capsule Blotter Drops other 0 10 20 30 40 50 60 70 80 90 100 2001- 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016 Frequency of occurrence [%] Year MDMA m-CPP MDEA MDA 2C-B Methamphetamine p-Fluoroamphetamine 0 10 20 30 40 50 60 70 80 90 100 2001- 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016 Frequency of occurrence [%] Year Amphetamine Cocaine Ketamine MDMA 2C-B Methamphetamine Heroin Mescaline 0 50 100 150 200 250 300 350 400 2001- 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016 Samples Year 0 10 20 30 40 50 60 70 80 90 100 2001- 2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016 Frequency of occurrence [%] Year MDMA m-CPP MDEA MDA p-Fluoroamphetamine Amphetamine Cocaine Ketamine 2C-B Methamphetamine Heroin Mescaline LSD Samples per year All samples (n = 3415) 0 20 40 60 80 100 120 140 160 180 200 220 240 260 280 0 50 100 150 200 250 300 350 400 450 500 550 600 650 700 750 800 850 900 950 1000 1050 1100 MDMA dose [mg/Tbl.] Sample MDMA Year Moving average (period=50) 2001-2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016 0% 10% 20% 30% 40% 50% 60% 70% 80% 90% 100% 0 25 50 75 100 125 150 175 200 225 250 275 300 325 350 375 400 425 450 475 500 525 550 575 600 625 Cocaine Amount [weight-%] Sample Cocaine Year Moving average (period=20) 2001-2002 20032004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016 0% 20% 40% 60% 80% 100% 1 51 101 151 201 251 301 351 401 451 501 551 601 651 701 751 Amount [weight-%] Sample Amphetamine Caffeine Year Moving average Amphetamine (period=50) 2006 2007 2008 2009 2001- 2002 2003 2004 2005 2010 2011 2012 2013 2014 2015 2016
Transcript of „PARTY DRUGS“ TESTING ON THE DANCE FLOOR ...€žPARTY DRUGS“ TESTING ON THE DANCE FLOOR:...
HPLC (measurement apparatus)For chemical analysis of party drugs separation and detection of different constituents of mix-tures (active ingredients and fillers) is necessary. With the mobile lab we are using High Per-formance Liquid Chromatography (HPLC) for the separation process. Our computer controlled HPLC-systems are equipped with DAD/UV-Vis Spectrometers (Diode Array Detector).
Chemical analysis of “Party Drugs“ gives one of three possible results. The findings may be a single active agent, several active agents, or indeed no active agent. Reliable analysis of the substances in a sample cannot be achieved by means of a simple “quick test“ and is only possi-ble by the use of a complex measurement chain, as shown in the following basic diagram:
Chemical analysis requirements
HPLC-SystemAutosampler: HP-1100, Typ G1389APump: HP-1100, Binary Pump, Typ G1376ADetector: HP-1100, UV-Vis DAD-Detector, Typ G1315BIntrument control & integration ChemStation for LC 3D softwareHPLC- ConditionsStationary phase: Spherisorb 80-3 ODS-1 (Waters)Column dimension: 125 x 4.0 mmHold-up volume: 1.002 mlElutiontype: GradientEluent A 8,50 g ortho-phosphoric acid 85% + 280 µl hexylamine + purified water ad 1000 ml Eluent B 4,25 g ortho-phosphoric acid 85% + 140 µl hexylamine + 45,75 g purified water + 351 g acetonitrile
Gradient programTime in min % A %B
0 – 2.5 95 52.5 – 9 95 - 60 5 - 409 – 13.5 60 40
13.5 – 14 60 - 95 40 - 514 – 16.5 90 5
Measuring parameters: Flowrate: 1 ml/minPressure: 150 barInjection volume: 2.5 μlColumn temperature: 40 °CDetection: UV 198 nmSignal-Range: 190-400 nm
Analytical method
Health & Social Welfare Department State of Berne
Office of the Cantonal Pharmacist
Daniel Allemann, Hans Pauli, André Mürner, Lukas Mürner, Michael Staub, Fabienne Holzer, Hans-Jörg Helmlin, Samuel Steiner
Dr. H.-J. Helmlin, MBA, Ph DHead Laboratory KAPAState of Berne Baltzerstrasse 5CH-3012 Berne Switzerlande-mail: [email protected]
Daniel AllemannLaboratory KAPAState of Berne Baltzerstrasse 5CH-3012 Berne Switzerlande-mail: [email protected]
Contacts: This arrangement applies to most modern chemical-analysis measurement systems.
Update: 31.12.2016
Update: 31.12.2016
Flow diagramCollaboration between the prevention-teams and the laboratory
Separation EDP-system
SampleInputsystem
Samplepreparation
Detector-system
Measurement apparatus
Analysis sequence
Results
„PARTY DRUGS“ TESTING ON THE DANCE FLOOR: EQUIPMENT, METHODS AND RESULTS
Information standsat the party
Sample-documentation
HPLC-analysis
Database
Result
quantification
calibration
known activesubstance
unknownactive
substance
HPLC-analysis (mobile)
Questionnaire (anonymous)
Identification
Measurement data
Extraction
Measuring/weighing
Photography
Coding
Information Prevention message
Pharmaceutical Control Laboratory Bern
(within 1-4 days)
Laboratory measurements
GC/MS, LC/MS, IR
Office
Wasserwerkstrasse 17 8006 Zürich
E-mail Telephone
(Telephone)
10-15 mg
Sample-material
Sample
Information stand at the party
HPLC-analysis
Database
Ravers
OfficeMülhauserstrasse 1114056 Basel
OfficeWasserwerk-strasse 178006 Zürich
OfficeMonbijoux-strasse 703007 Bern
IntroductionSince 1998 the mobile lab unit of the Office of the Cantonal Pharmacist (Health & Social Welfare Department, State of Berne, Switzerland) is testing so called „Party Drugs“ on the dance floor. At more than 160 events the team has tested over 3400 samples in cooperation with „Streetwork Zurich“, „Contact Bern“ and „Suchthilfe Region Basel“.
The mobile lab consists of four custom made subunits mounted in steel framed racks on wheels, one for weighing and documentation, one for sample prepara-tion and two with the equipment for che-mical analysis (HPLC-DAD).The lab is operated by two experienced technicians. Before analysis the intere-sted customer is asked by the lab crew to fill out a questionnaire concerning in-formation about the sample; thereafter every sample is digitally documented and characterized by physical appearance (form, weight, dimensions etc.).
Report Analytical results are available within about 20 minutes. The computer prints the results of the analysis as a report. The report consists of 3 parts: The header, the chromatogram, and the results (including identification and quantification)
Header:The header contains details like: File-name, sample-number, date of analysis, name of method etc.
Chromatogram:The chromatogram is a graphic visualisa-tion of the separation process. Detected substances appear as “Peaks”.
Results (identification and quantification):The system compares the area-value of an integrated Peak with the correspondi-ng calibration of the active substance in the specified methods. This automatic process gives us a precise quantification.
Additionally it is possible to get the UV-spectra of the “Peak” and compare it with our specific UV- Spectra-library.
Sample preparation: Due to the very sensitive analytical methods, only a representative part of the sample is used for further analysis. Sample preparation is quick and effective. The material is pulverised in a mor-tar and dissolved in methanol with the aid of an ultrasonic extractor.
Bottles with mobile phase (solvent mix)
HPLC- Pump(Part of the separation-system). This high-pressure pump delivers the solvent (with the dissolved sample) through the separating column to the detector.
Autosampler The autosampler transfers the prepared sample from the vial into the measurement apparatus.
HPLC-columnThe “central unit“ of the HPLC-system serves to separate dis-solved mixtures of substances into their constituents.
DetectorThe chemical detector is positioned at the end of the co-lumn. It is the highly sensitive “eye“ of the measurement chain and records sub-stances which absorb ultra-violet light when they pass trough the detector cell dissolved in the mobile phase. The detec-tor provides two kinds of information about
the molecules measured: their identity and their quantity. The whole process is continuously monitored with a computer system. Measurement signals are converted into graphical displays appearing on the computer screen. The two most important displays are the chromatogram and the UV-spectrum. The chromatogram is a representation of the separation process. The UV-spectrum is a characteristic constant for a particular substance.
An internal standard is added as control. In most cases this extract still contains insoluble com-ponents, which must be filtered off before analysis. The clear sample solution obtained is trans-ferred into a sample vial.
'Additives' in cocaine samples (n = 604)Cocaine content in % (n = 604)
Frequency of occurrence of different pharmaceutical substances in cocaine samples
Variation of MDMA-dose in tablets (mg/tablet)
Quantitative comparison
Variation of Amphetamine and Caffeine amount in powders (in weight-%)
Chemical substances detectedChemical substance Count Frequency of occurrence [%]MDMA 1586 46.44Caffeine 871 25.51Amphetamine 790 23.13Cocaine 607 17.77Levamisole 277 8.11Phenacetin 260 7.61m-CPP 96 2.81Lidocaine 66 1.93no active ingredient 58 1.70LSD 54 1.58Ketamine 46 1.35Amphetamine synthesis by-product 45 1.322C-B 43 1.26Phenylacetone 43 1.26Domperidone 41 1.20unknown 40 1.17MDA 35 1.02MDEA 32 0.94Paracetamol 32 0.94Methamphetamine 28 0.82Metoclopramide 22 0.64Acetylsalicylic acid 21 0.61Heroin 19 0.56Noscapine 19 0.563,4-Methylendioxyphenyl-2-propanol 14 0.414-Methylamphetamin 13 0.38iso-LSD 13 0.38Hydroxyzine 12 0.35Mescaline 12 0.35Creatin 11 0.32Ephedrine 11 0.32p-Fluoroamphetamine 11 0.32Benzocaine 10 0.29Buflomedil 10 0.29Tetracaine 10 0.29Procaine 9 0.26Salicylic acid 9 0.26N-Formylamphetamine 7 0.20Cimetropium bromide 5 0.15Diltiazem 5 0.15Mephedrone 5 0.15related substance 5 0.15TFMPP 5 0.15Vanillin 5 0.15Benzylpiperazine (A2) 4 0.12Methylone (bk-MDMA) 4 0.12Methylphenidate 4 0.122C-H 3 0.092C-H 3 0.09DOC 3 0.09MDMA synthesis by-product 3 0.09MDPV 3 0.092C-E 2 0.063,4-Methylenedioxyphenylacetonitrile 2 0.063-Methylmethcathinone (3-MMC) 2 0.064-Methylethylcathinon (4-MEC) 2 0.066-Monoacetylmorphin 2 0.06Butylone (bk-MBDB) 2 0.06Ethcathinone 2 0.06MDDM 2 0.06MDHOET 2 0.06PMMA 2 0.06Pseudoephedrine 2 0.06Sucrose octaacetate 2 0.06TMA-2 2 0.06Triprolidine 2 0.061-Benzyl-4-Methylpiperazin (MBZP) 1 0.032C-i 1 0.034-Chloroethcathinone 1 0.034-Chloromethcathinone 1 0.03Amoxicillin 1 0.03Atropine (Hyoscyamine) 1 0.03Bisoprolol 1 0.03Chloroquine 1 0.03Clozapine 1 0.03Desloratadine 1 0.03Dextromethorphan (DXM) 1 0.03Dimethyl terephthalate 1 0.03DMT 1 0.03DOI 1 0.03Erdosteine 1 0.03Ergotamine 1 0.03Flephedrone 1 0.03gamma-Butyrolactone 1 0.03Isoniazid 1 0.03Medicament 1 0.03Metamizol 1 0.03Metandienone 1 0.03Methaqualone 1 0.03Niacin (Vitamin) 1 0.03N-Methylbenzylamin 1 0.03N-Methylephedrine 1 0.03Oxycodon 1 0.03Pentedrone 1 0.03Phenobarbital 1 0.03Piperonal 1 0.03Piracetam 1 0.03Propranolol 1 0.03Propyphenazone 1 0.03Scopolamine 1 0.03Scopolamine derivative 1 0.03Tadalafil 1 0.03Theophylline 1 0.03Tryptophan 1 0.03Xylazine 1 0.03
Capsules (n = 47)
others10%
LSD2%m-CPP
2%
Cocaine18%
Amphetamine22%
MDMA46%
Active ingredients (all samples) (n = 3415)
Active ingredients (evolution time based)
Galenical forms (all samples) (n = 3415) Galenical forms (MDMA samples) (n = 1560)
Tablets (n = 1355)Powders (n = 1950)
Mean (n = 1094)= 99.6 mg/tabletMax = 268.0 mg
(n = 759)
Frequency of occurrence Qualitative results
0
10
20
30
40
50
60
70
80
90
100
2001-2002
2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016
7264
54 53 49 48 51
2941 46 48
39 44 39 36
17
1125 24
19 22 13
18
2522 22
2530
2622
3
14 11 1219 10
15
22
1619 14 22
1423
30
1.6 6.0
1.1 5.919.3
5.92.0 0.4 0.32.0 2.5
1.53.2 3.3 3.4 2.7
7 10 10 10 8 19 15 11 10 7
15 10 8 8 9
Freq
uenc
y of
occ
urre
nce
[%]
Year
Main active ingredients (evolution time based)
MDMA Amphetamine Cocaine m-CPP LSD others
only tablets withdose > 5 mg/tablet
(n = 1094)
0
10
20
30
40
50
60
70
80
90
100
2001-2002
2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016
Freq
uenc
y of
occ
urre
nce
[%]
Year
Additives in Cocaine samples
PhenacetinLevamisoleBenzocaine / Lidocaine / Procaine / TetracaineDiltiazemCaffeine
MDMA47%
Amphetamine2%
Ephedrine9%
Methamphetamine2%
Methylphenidate2%
Benzylpiperazine (A2)2%
TFMPP2%
TFMPP + Benzylpiperazine2%
2C-B2%
Mephedrone4%
Methylon (bk-MDMA)4%
Mescaline2%
TMA-22%
Scopolamine derivative2%
Cathine2%
Caffeine2%
unknown6%
no active ingredient4%
0
10
20
30
40
50
60
70
80
90
100
2001-2002
2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016
Freq
uenc
y of
occ
urre
nce
[%]
Year
TabletPowderCapsuleBlotterDropsother
0
10
20
30
40
50
60
70
80
90
100
2001-2002
2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016
Freq
uenc
y of
occ
urre
nce
[%]
Year
TabletPowderCapsuleBlotterDropsother
0
10
20
30
40
50
60
70
80
90
100
2001-2002
2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016
Freq
uenc
y of
occ
urre
nce
[%]
Year
MDMAm-CPPMDEAMDA2C-BMethamphetaminep-Fluoroamphetamine
0
10
20
30
40
50
60
70
80
90
100
2001-2002
2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016
Freq
uenc
y of
occ
urre
nce
[%]
Year
AmphetamineCocaineKetamineMDMA2C-BMethamphetamineHeroinMescaline
0
50
100
150
200
250
300
350
400
2001-2002
2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016
Samples
Year
0
10
20
30
40
50
60
70
80
90
100
2001-2002
2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016
Freq
uenc
y of
occ
urre
nce
[%]
Year
MDMAm-CPPMDEAMDAp-FluoroamphetamineAmphetamineCocaineKetamine2C-BMethamphetamineHeroinMescalineLSD
Samples per year All samples (n = 3415)
020406080
100120140160180200220240260280
0 50 100 150 200 250 300 350 400 450 500 550 600 650 700 750 800 850 900 950 1000 1050 1100
MD
MA
dose
[mg/
Tbl.]
SampleMDMA Year Moving average (period=50)
2001-2002 2003 2004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016
0%
10%
20%
30%
40%
50%
60%
70%
80%
90%
100%
0 25 50 75 100 125 150 175 200 225 250 275 300 325 350 375 400 425 450 475 500 525 550 575 600 625
Coc
aine
Am
ount
[wei
ght-%
]
Sample
Cocaine Year Moving average (period=20)
2001-2002 20032004 2005 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016
0%
20%
40%
60%
80%
100%
1 51 101 151 201 251 301 351 401 451 501 551 601 651 701 751
Am
ount
[wei
ght-%
]
Sample
Amphetamine Caffeine Year Moving average Amphetamine (period=50)
2006 2007 2008 20092001-2002
2003 2004 2005 2010 2011 2012 2013 2014 2015 2016
