Methamphetamineand

BeyondRobert P. Di RienzoJohn M. ReynoldsJames B. Perkins

AIHCe, May 2006

Agenda

ProblemCompounds of InterestOther Drug Lab ContaminantsNew Methods

SamplingAnalysis

Methamphetamine Problem

• Increasing Use• Health and Safety• Precursors • Contamination and Exposure• Clandestine Laboratory Production

– 20,000 Meth Labs busted in 2004

Compound of InterestMethamphetamine

Other Possible Drugs of Interest

Amphetamine

Ephedrine and Pseudophedrine

MDMA (Ecstasy)

ManufactureHydrogenation of hydroxyl group

Red Phosphorus/Iodine Method (Most Common)

Phosphorus + Iodine = Hydroiodic Acid

Birch ReductionLithium and Ammonia

Hydrogenation of Hydroxyl Group

Commercial Products in the Manufacture of Methamphetamine

MSM (nutritional supplement)Pseudoephedrine (cold medications)Red phosphorus (matches or road flares)Salt (table or rock)Sodium hydroxide (lye)Sodium metalSulfuric acid (drain cleaner)Toluene (brake cleaner)Trichloroethane (gun cleaner)

AcetoneAlcohol (isopropyl or rubbing)Anhydrous ammonia (fertilizer)Ephedrine (cold medications)Ether (engine starter)Hydrochloric acid (pool supply)Iodine (flakes or crystal)Kitty litterLithium (batteries)Methanol (gasoline additive)

Metamphetamine Laboratory Hazards

Source: DEA Office of Diversion Control.

May explode as a result of contact or friction. Ignites if heated above 260° C. Vapor from ignited phosphorus severely irritates the nose, throat, lungs, and eyes.

Red phosphorus

A colorless gas with a pungent, suffocating odor. Inhalation causes edema of the respiratory tract and asphyxia. Contact with vapors damages eyes and mucous membranes.

Anhydrous ammonia

Inhalation can cause sudden cardiac arrest or severe lung damage. It is corrosive if ingested.

Freon

Extremely flammable, posing a fire risk in and around the laboratory. Inhalation or ingestion of these solvents causes severe gastric irritation, narcosis, or coma.

Acetone/ ethyl alcohol

Ingestion of doses greater than 240 mg causes hypertension, arrhythmia, anxiety, dizziness, and vomiting. Ingestion of doses greater than 600 mg can lead to renal failure and seizures.

PseudoephedrineHazardsChemical

Methamphetamine Laboratory Hazards

Source: DEA Office of Diversion Control.

Ingestion of doses greater than 75 mg causes hypertension, arrhythmia, anxiety, and dizziness. Quantities greater than 300 mg can lead to renal failure, seizures, stroke, and death.

Phenylpropanolamine

Give off vapor that is irritating to respiratory system and eyes. Solid form irritates the eyes and may burn skin. If ingested, cause severe internal damage.

Iodine crystals

A corrosive acid with vapors that are irritating to the respiratory system, eyes, and skin. If ingested, causes severe internal irritation and damage that may cause death.

Hydriodic acid

Extremely caustic to all body tissues. Reacts violently with water and poses a fire or explosion hazard.

Lithium metal

Extremely dangerous substitute for red phosphorus. If overheated, deadly phosphine gas is released. Poses a serious fire and explosion hazard.

Hypophosphorous acidHazardsChemical

Other Drug Lab Contaminants

Birch ReductionAmmonia

By product of Red Phosporus-Iodine Method

Phosphine

Iodine used to make Hydro Iodic AcidIodine

Red Phosporus used to make HydroicAcid/ Litium used in Birch Reduction

Phosphorus/Metals

Used to extract Pseudoephedrine and Ephedrine

Solvents

Hydroiodic Acid used in Red Phosphorous-Iodine method

Inorganics Acids

UseContaminant

Other Drug Lab Contaminants

NMAM 6015Ammonia

OSHA 1003Phosphine

NMAM 6005Iodine

NMAM 7300Phosphorus/Metals

TO-15 or TO-17Solvents

NMAM 7903Inorganics Acids

Analysis MethodsContaminant

Analysis Methods

LC/MS – Direct InjectionNMAM 9111 Draft

GC/MS with Solid-Phase Extraction

NMAM 9109 Draft

GC/MS with Liquid-Liquid Extraction

NMAM 9106 Draft

Analysis TypeNMAM Method

Analysis Methods

Accurate quantitation of all compounds of interestExtensive List of qualitative compoundsEasy Sampling ProceduresExtensive Validation

Qualitative IdentificationNorephedrineMethcathinoneNorspseudoephedrineAminorexAcetoaminophenMethyl phenidateMerperidineAtropine

NicotineFenfluraminePhenylethylaminePhentermineCathinoneBupropionN-Ethyl amphetamineEcgonine-methyl ester

Qualitative IdentificationPhencyclidine (PCP)MDEAMBDBTheophyllineMescalineChlorpheniramineMethyl phenidate4-Bromo-2,5-DMPEA

CaffeineN,N-DimethyltryptamineBDBKetamineLidocaineTrifluoromethylphenylpiperarazineBenzyl piperazine

Qualitative IdentificationMorphineCodieneOxycdoneHydromorphoneFlunitrazepamFentanylHydromorphone

4-MethylaminorexDextromethorphanMethaqualoneCocaineAtrpineDiazepamHydrocodone

Sampling• Media Tested

– Cotton Gauze, MIRASORB, NU GAUZE, SOF-WICK, TOPPER, AlphaWipe

• Solvents Tested– Methanol, Isopropanol, Water, 5% Vinegar

• Selected Media and Solvent– Cotton Gauze and Methanol

Wipe Sampling

• Media– Cotton Gauze

• Recoveries > 90%• Cost Effective• Availability

Wipe Sampling• Solvent

– Methanol (or Isopropanol)• Recoveries > 90%• Better recoveries than water• Available

Wipe Sampling• Procedure*

– Fold Gauze in quarters– Wet with 2 – 3 mL of Methanol– Remove excess Methanol– Wipe left to right in overlapping “N” Pattern– Refold gauze (fresh surface) – Wipe top to bottom in overlapping “Z” pattern– Insert gauze in 50mL poly centrifuge tube and cap– Transport to lab at < 6°C if possible

* Contact your state for required sampling procedures.

Method Summaries• NMAM 9106 Draft

– Add Solvent/Internal Standard and mix– Liquid-Liquid Extraction– Derivatize with perfluorinated acid anhydride– Solvent exchange to acetone-toluene– Analysis by GC/MS– Internal Standard Calibration– Wipes or Bulks

Method Summaries• NMAM 9109 Draft

– Add Solvent/Internal Standard and mix– Solid Phase Extraction– Elute with MeCl2/IPA/NH40H– Derivatize with Acetonitrile, MBHFBA and

MSTFA– Analysis by GC/MS– Internal Standard Calibration– Wipes or Bulks

Method Summaries• NMAM 9111 Draft

– Add Solvent/Internal Standard and mix– Analysis by LC/MS– Internal Standard Calibration– Wipes or Bulks

Method Selectivity

Internal Standard – Methamphetamine-d14

Retention Time

Mass Spectra

Derivatization (GC/MS Methods Only)

Method Sensitivity

0.50.50.5Cleanup Levels* (µg/100cm2)

0.050.050.05Reporting Limit (µg/wipe)

NMAM9111

NMAM9109

NMAM9106

* Colorado Department of Health - Contact your state for required cleanup levels.

Method Comparison

Derivatization/Extraction

CostAnalysis TimeAdditional AnalytesLC/MSGC/MSInternal Standard

DesorptionCotton Gauze and Methanol

NMAM9111

NMAM9109

NMAM9106

Thank YouRobert P. Di Rienzo

dirienzo@datachem.comJohn M. Reynolds

reynolds@datachem.comJames B. Perkins

perkins@datachem.com

(801) 266-7700