Group Picture 2008 - Back row from left: Howard, Steve, Erica, Jenny, Gela, Ben, Cleon, Dr. Almirall

Front row from left: Tatiana, Hanh, Yisenny, Patty, Monica, Maria. Missing from picture: Waleska and Yaribey

Group Picture 2007 - Ladies from left to right: Erica, Tatiana, Monica, Hassel, Hanh, Yisenny, Maria, Waleska, Gela, Dr. Jeannette Perr, and Patty

Guys in the back row: Steve, Ben, Dr. Almirall, Dr. Cleon Barnett, Anthony

Group Picture 2006 - Group members: Ben, Erica, Tatiana, Gela, Patty, Dr. Almirall, Hanh, Monica, Waleska, Steve, and Dr. Cleon Barnett

Group Picture 2005 - Group members: Jeannette, Patricia, Joe, Waleska, Ben, Sayuri, Gela, Tatiana (Research Programs Coordinator), Frank and Dr. Almirall (Agnes, Heather and Marilyn not present)

Group Picture 2004 - Click on the picture for a larger image of group members: Dr. Almirall, Marilyn, Sayuri, Jeannette, Nicole, Waleska, Patricia and Joe (Agnes and Heather not present)

Group Picture 2003 - Click on the picture for a larger image of group members: Tatiana, Jeannette, Carlos, Dr. Almirall, Andria, Jodi and Linda

Group Picture 2002 - From left to right: Shirly Montero, Carlos Diaz, Tatiana Trejos, Andria Hobbs, Sabrina Frank, Jodi Meyers, Jeannette Perr and Dr. Almirall (Oliver Spicer, Hussain AlGhanim, Agnes Garcia and Louis Morris and are not present)

Group Picture 2001 - From left to right: Dr. Almirall, Jeannette Perr, Shirly Montero, Sabrina Frank, Gigi Galiana, Oliver Spicer, Andria Hobbs, and Hussain AlGhanim (Agnes Garcia, Louis Morris and Jodi Meyers are not present)

Graduate Student Research Projects, Scientific Publications and Scientific Presentations

Current Graduate Students

Ion-Molecule Interactions in an Ion-Trap Mass Spectrometer for the Characterization of Explosives and Ignitable Liquid Residues

by: Jeannette Perr - Ph.D. in Chemistry Student

The objective of my research will involve studying ion-molecule interactions within the ion trap detector in order to identify and characterize explosive residues and pyrolysis products found in scene debris from other possible ignitable liquid residues while optimizing the conditions for this set of forensically interesting analytes. Prior to trapping the fragments and molecular ions that result from the sample, I will study the effects of three different ionization sources: electron impact ionization (EI), chemical ionization (CI), and glow discharge (GD). There are two main sample sources I will be concentrating on: high explosives that might be found in post-blast debris or environmental contamination of storage facilities and ignitable liquid residue that might be found in fire debris.

High explosives can be thermally labile and not amenable to EI requiring the exploration of softer, gentler ionization methods, such as CI and GD. At some point in the future I will begin work on constructing a RF GD ionization source to be placed on the front end of the ion trap. RF GD ionization sources are currently not in a stage of commercial production.

Ion mobility spectrometry (IMS) is the most common instrument used in the field today to presumptively identify drugs of abuse and explosives. These instruments are typically found in airports where they are used to detect these substances on luggage after swabbing the item. IMS is an analytical technique that distinguishes ionic species based on their reduced mobilities. It is a highly sensitive technique for the detection of trace organics, such as drugs of abuse, under atmospheric pressure conditions. Ion mobility spectroscopy affords a low cost, rapid, and portable method for analysis of organic materials. It is often used for analysis of drugs of abuse by many government agencies. Unfortunately, IMS is not a very selective technique and many substances can interfere with the presumptive identification of a sample. Another aspect of my project will be developing a system that can be used in the field to sniff for explosives that is better then IMS.

The third aspect of my project will be to examine the extraction of explosive residues and pyrolysis products found in scene debris from other possible ignitable liquid residues. Some of the techniques of interest are charcoal strip headspace extraction and solid phase micro extraction (SPME).

Papers:

J. M. Perr, K. G. Furton, and J. R. Almirall,Chemical Ionization Tandem Mass Spectrometry (CI/MS/MS) of Organic Explosives, Talanta, submitted 2004

J. M. Perr, K. G. Furton, and J. R. Almirall,  Solid Phase MicroExtraction Ion Mobility Spectrometer Interface for Explosives and Taggant Detection, Separation Sciences, 2004, in press.

J.R. Almirall and J. Perr, The use of compound specific MS/MS for the identification of ignitable liquid residues in fire debris analysis”, in Advances in Forensic Applications of Mass Spectrometry, J. Yinon, Ed., CRC Press, 2003, 181-230.

J.R. Almirall, T. Trejos, A. Hobbs, J. Perr and K.G. Furton, Mass Spectrometry in Forensic Science,in Advances in Mass Spectrometry, Vol 16, A.E. Ashcroft, G. Breton and J.J. Monaghan, Eds., Elsevier, 2004, 167-187.

Presentations:

"Rapid Screening of Hair Samples Using Solid Phase Extraction and Ion Mobility Spectroscopy"
2001 Pittsburgh Conference and Exposition on Analytical Chemistry and Applied Spectroscopy, presenting author

"Characterization of Drugs of Abuse by Ion Mobility Spectrometry and GC/MS"

2000 American Chemical Society, co-author

"One Interference Filter, One Silicone Oil, and a Lot of Glass: Glass Refractive Index Database"
2000 American Academy of Forensic Sciences, co-author, 1999 Mid Western Association of Forensic Scientists, presenting author

A Comprehensive Approach to Determine the Absolute Detection Limit for Organic Compounds in a Standard Accelerant Mixture Between GC/MS and GC/MS/MSä, 2002 American Academy of Forensic Scientists

Awards:

American Institute of Chemists Award

3^rd place in Graduate Student Association Scholarly Forum

Quantitation of Gamma-hydroxybutyric Acid and Gamma-butyrolactone using Capillary Electrophoresis and High Performance Liquid Chromatography

 by Agnes D. Garcia, Master of Science in Forensic Science Student

The objective of this project is to develop a rapid analytical method for the screening and quantitation of gamma-hydroxybutyrate (GHB) and gamma-butyrolactone (GBL) and to overcome inherent difficulties with other instrumental techniques. 

In recent years there has been an increase in the illicit manufacture of GHB, for the purpose of being sold in the clandestine market.  Possession of GHB has been recently scheduled as a federal offense and is commonly abused as a recreational drug in rave clubs.  It is a depressant with euphoric and hallucinatory effects, and is often abused in conjunction with other illicit controlled substances.

Instrumental analysis of aqueous solutions containing gamma-hydroxybutyrate (GHB), a Schedule I drug, presents difficulties due to its equilibrium with its precursor, gamma-butyrolactone (GBL).  Further, GHB easily undergoes esterification, converting to the butyrolactone in the presence of small amounts of acid.  Gas chromatography, a commonly employed instrument used for quantitation, can convert GHB to the lactone due to thermal reactions in a heated injection port.  The use of a high performance liquid chromatography  (HPLC) or capillary electrophoresis (CE) method and associated instrumentation overcomes thermal degradations  which are prevalent with gas chromatographic methods.  In this study, analysis of  GHB and its lactone was achieved via  HPLC and CE.  

A capillary electrophoresis was utilized, equipped  with a fused silica capillary column using an electrokinetic system.  Reversed phase HPLC was also investigated using a complete aqueous HPLC system. Linearity, accuracy, and reproducibility studies are presented.  The effects of organic modifier type, organic modifier concentration, temperature, and voltage on the separation GHB and GBL are also presented. 

I officially began the Master of Science in Forensic Science program at FIU in the Fall of 2000 but I have been collaborating with Dr. Almirallâs group since Sept. 1999 and I have taken courses at FIU since Sept. 1999.

Papers:

Presentations: 

1999:

Garcia, A.D., Shannon, M., Almirall, J.R. ãFast Analysis of Gamma-Hydroxybutyric Acid (GHB) by In-Situ Derivatization on an SPME Fiberä  oral presentation at the American Academy of Forensic Sciences Meeting, February 1999.

Gross, S., Garcia, A.D., Almirall, J. R. ãThe Analysis of the Psilocybe Cyanescens (Wakefield) Mushroomä  oral presentation at the American Academy of Forensic Sciences Meeting, February 1999.

Almirall, J. R., Gross, S., Garcia, A.D., ãA Comparison of GC-MS, LC-ECD, LC-MS, and CE Methods for the Analysis of the Psilocybe Cyanescens (Wakefield) Mushroomä oral presentation at the Pittcon Meeting, March 1999.

Garcia, A.D. and Lurie I. ãSimultaneous Chiral Determination and Quantitation of Methamphetamine and Related Compounds Using Capillary Electrophoresisä oral presentation at the International Association of Forensic Sciences Meeting, August 1999.

Garcia, A.D. and Almirall, J.R. ãQuantitative Analysis of Psilocybin and Psilocin from the Psilocybe Cyanescens (Wakefield) Mushroom by CEä poster presentation at the International Association of Forensic Sciences Meeting, August 1999.

2000: 

Garcia, A.D., Lurie I. ãQuantitation of 3,4-Methylenedioxymethamphetamine and Related Compounds using Capillary Electrophoresisä  oral presentation at the American Academy of Forensic Sciences Meeting, February 2000.

Garcia, A.D., Almirall, J.R., Lurie, I. ãA Comprehensive Review of the Analysis of Controlled Substances by Capillary Electrophoresis, Using Free Zone, MECC, and Cyclodextrin Systemsä poster presentation at the American Academy of Forensic Sciences Meeting, February 2000. 

Almirall, J.R. and Garcia, A.D. ãQuantitative Analysis of Common Benzodiazepines by Free Zone Electrophoresisä poster presentation at the American Academy of Forensic Sciences Meeting, February 2000. 

Lurie, I., et al. ãUse of Dynamically Coated Capillaries for the Routine Analysis of Methamphetamine, Amphetamine, MDA, MDMA, MDEA, and Cocaine using Capillary Electrophoresisä oral presentation at the American Academy of Forensic Sciences Meeting, February 2000.

Garcia, A. ãAnalytical profile of GHBä oral presentation at the Southern Association of Forensic Sciences Meeting, April 2000.

Garcia, A. ãRise of GHBä oral presentation at Club Drugs Conference, August 2000.

           “Ion-molecule reactions and High resolution in ICP-MS Analysis”.

Waleska Castro, Ph.D. in Chemistry Student

           “Elemental Charaterization of Paint Samples”

Joseph Gagnon, M.S. in Forensic Science Student

QUANTITATIVE ANALYSIS OF TRACE METALS IN MATERIALS BY LASER ABLATION INDUCTIVELY COUPLED PLASMA MASS-SPECTROMETRY (LA-ICP-MS) WITHOUT THE NEED FOR MATRIX-MATCHED STANDARDS

Sayuri Umpierrez, M.S. in Chemistry Student

The principal aim of this research is the development, optimization and validation of a LA-ICP-MS method that does not require matrix-matched standards so it can be applied to the quantitative analysis of any solid material. This consists of an addition experiment that uses a calibration solution of known concentration of each element to produce a constant background signal, so the spike generated by the ablation signal of the sample can be measured in certain amount of time.

The usefulness of this LA-ICP-MS without matrix-matched standards method for glass and paint analysis will be evaluated in terms of precision, reproducibility, accuracy, limits of detection, and discrimination power. This evaluation will be based on a direct comparison of the new method results from some sets of samples with the previously validated LA-ICP-MS that utilizes internal and external standards for calibration.

Besides, the comparison of two laser systems: LSX-200 plus and New Wave UP213 has been carried out in order to determine the best one for the experiments. Since the New Wave Laser ablates at a shorter wavelength (213 nm), its higher energy allows a better interaction with the sample. Therefore, the New Wave Laser gives better limits of detection and precision (RSD < 5%) due to its increased power compared to the Cetac LSX-200 plus. The crater that results from the New Wave Laser looks like a perfect cylinder while the crater resulting from using the Cetac LSX-200 plus is conical. This difference in the shape of the crater is translated into a different amount of material being removed from the sample. In the case of the Cetac LSX-200 plus, the conical crater produced probably due to less uniform energy distribution along the focus of the sample during the ablation  causes lower signal reproducibility.

Presentations:

“Forensic Elemental Analysis of Glass by Laser Induced Breakdown Spectroscopy (LIBS), Laser Ablation Inductively Coupled Plasma Mass Spectrometry, and X-Ray Fluorescence”. Sayuri Umpierrez, B.S., Stephannie Thacker, B.S., Scott Ryland B.S.,  and José R. Almirall, Ph.D. Joint Meeting of the SAFS, MAFS, MAAFS and the CSFS in Orlando, Sept. 2004 (poster)

“Análisis Forense de vidrio por SEM-EDS, XRF, LIBS y LA-ICP-MS”. Sayuri Umpierrez, B.S. y Dr. Almirall. I Congreso de Ciencias Forenses en Costa Rica, Nov. 2004 (oral presentation)

         “The use of Ion Mobility Spectrometry (IMS) for the detection of drugs and explosives”

Nicole Manley,  M.S. in Forensic Science Student

Narcotics use and abuse is a major issue and contributes to many societal problems.  The detection and identification of illicit drugs is of major interest in current research.  The objective of this project is to comprehensively evaluate and validate GE Ion Track’s EntryScan3 portal.  The EntryScan3 (ES3) from General Electric (GE) is a new walk-through particle detection portal that rapidly examines individuals for concealed narcotics in a non-intrusive manner with the use of an Ion Mobility Spectrometer (IMS).  Through this research scientific data will be collected from an objective source with the availability of multiple resources. 

Controlled experiments with known quantities of cocaine and heroin will be designed to test the capabilities of the instrument.  The limits of detection given by GE, 5ng for both forms of cocaine and 25ng for heroin, will be examined under controlled laboratory conditions.  Five different fabric surfaces located at five different regions of the body will be tested for detection.    

In addition to the controlled experiments with known quantities of drugs, experiments also will include the detection of concealed drugs as they are packaged in real cases.  A law enforcement agency will participate in an experiment involving real drugs and with packaging typically used in the illicit market of controlled substances. 

Experiments will also be designed to test the instruments selectivity by assessing false positives and false negatives.  Fifteen commonly encountered substances ranging from water and coffee to commonly carried legal drugs will be tested. 

A comparative sensitivity study will also be conducted with Ion Track’s next generation Itemiser 2.

Research will also be conducted to determine if the ES3 is capable of alerting for THC.  The instrument is calibrated to detect the active ingredient in cannabis sativa L. and this compound has a low vapor pressure, unlikely to be detected by IMS in the portal.  The detection of the odor signatures of cannabis will be carried out with the use of Solid Phase Micro Extraction (SPME) and gas chromatography/mass spectrometry (GC/MS). 

Presentations:

Southern Association of Forensic Scientists Fall 2004 Joint Meeting, Orlando, Florida, September 20-23, 2004.  “Narcotic Detection By The EntryScan3 Using Ion Mobility Spectrometry (IMS)” N. Manley and J. Almirall.

The 80th Florida Annual Meeting and Exposition (FAME), Orlando, Florida, May 6-8, 2004. “Narcotic Detection By The EntryScan3 Using Ion Mobility Spectrometry (IMS)” N. Manley and J. Almirall.

USE OF MULTIPLEXED MICROSATELLITE MARKERS IN CANNABIS SATIVA FOR GENETIC FINGERPRINTING

Heather Erek, M.S. in Forensic Science Student

Cannabis sativa (marijuana) is the most commonly abused drug in the United States.  There is an increasing need for the development of a method to track the sale and distribution of cannabis plants in the United States.  It is routinely identified in laboratories by using microscopic examination and chemical tests.  However these methods only identify the plant as C. sativa.  A genetic test could demonstrate individuals and clones and associate these clones to a source.  The most common method of human genetic identification is through the use of short Tandem Repeats (STRs).  This method can also be applied to the Cannabis sativa plant.  There are many single reaction STR primers to use for the identification of C. sativa.  The aim of this project is to combine primers into a multiplex for quick and thorough identification of recovered plants. To multiplex the primers many parameters will need to be optimized, including PCR reaction mix, thermal cycling parameters and electrophoresis protocols.  This task will be achieved by combining primers that provide high sensitivity, good reproducibility and a high power of discrimination.

POSTER:

Almirall, J., Erek, H., Al-Ghanim, H., Development and Use of Microsatellite Markers in Cannabis sativa for Fingerprinting and Genetic Relatedness Analyses, 17th International Symposium on the Forensic Sciences, March 2004.

Current Undergraduate Students

DEVELOPING OF A STANDARDIZED FIELD PORTABLE EXTRACTION GAS CHROMATOGRAPHY TANDEM MASS SPECTROMETRY FOR THE ANALYSIS OF IGNITABLE LIQUID RESIDUES

By:  Marilyn Prieto – B.S. Candidate in Chemistry

The discovery and assimilation of small amounts of Ignitable Liquid Residues (ILR) in fire debris evidence can be difficult because of the considerable loss of these compounds during the fire, extraction techniques that are not the most sensitive, co-extraction of interfering products (IP), and analysis techniques that provide low discrimination. The main purpose of my project was to optimize a general method that can be used by examiners to improve current analysis of fire debris without significantly altering the workload or time required for analysis.  Hopefully, the method that is created will increase the sensitivity and selectivity that is necessary to detect minute amounts of ILR remaining after a fire and to differentiate ILR from IP. It is anticipated that the results using GC/IT/MS/MS will not require sophisticated training, longer analysis times, or data analysis programs.

USING LASER INDUCED BREAKDOWN SPECTROSCOPY (LIBS) FOR ELEMENTAL ANALYSIS OF MATRICES OF FORENSIC INTEREST

Elemental analyses within matrices of forensic interest such as glass, paint, fibers, gunshot residues, etc. are of extreme importance in the forensic field.  LIBS is a technique which already has a wide variety of practical applications in several realms of science and industry, but is new to the forensic science arena.   The advantages of LIBS is that it is virtually non-destructive, requires little or no sample preparation, user friendly, affordable, provides good detection limits (~50 ppm), offers qualitative analysis, and has the potential for portability.  LIBS uses a laser beam to induce breakdown in the target material.  This breakdown consequently results in an emission that can be spectroscopically analyzed.  I am attempting to observe whether this technique may be utilized as a quantitative tool for the target materials named above.  It is imperative that a fast and efficient method for those materials exist due to the increasing number of traffic accidents occurring in the United States today. 

Former Graduate Student Section

Elemental Analysis of Glass by Laser Ablation Inductively Coupled Mass Spectrometry (LA-ICP-MS)

by  Tatiana Trejos - Master of Science in Forensic Science (Awarded 2003)

The elemental analysis of glass evidence left at the scene of burglaries, kidnappings and hit and run accident cases, has demonstrated to provide useful information to associate a  suspect or victim to an event.

The solution  introduction techniques (external calibration and isotope dilution) provide for excellent sensitivity and precision but have the disadvantages of destroying the sample and also involve a complex sample preparation. The laser ablation method significantly reduces the sample preparation and can be considered as a non-destructive technique.

The aim of my research is to optimize and apply the LA-ICP-MS in a variety of glass samples  in order to  compare the results with the previously solution method developed by Shirly Montero. The evaluation of these results will determine the overall impact on both ease of use, cost of analysis and relative informing power of each method.

I began in the Masterâs Program in spring 2002. I have worked for the  Organism of Judicial Investigation (OIJ) in Costa Rica for five years in the areas of Drug Analysis, Toxicology and Trace Evidence and at this moment I have a permission to obtain my Masterâs degree here at FIU. I expect to learn as much as I can at the program in order to improve my professional skills and background in the forensic area and try to share this knowledge with my colleagues in Costa Rica.

In addition to my thesis research Iâm currently a research assistant at IFRI.

Posters:

2002 16^th meeting of the International Association of Forensic Sciences, Montpellier (coming event) 

2002 ACS 221th National Meeting Orlando, FL

Conferences:

2002 VII ENFSI Paint and Glass WG Meeting, Madrid (coming event)

Elemental Analysis of Automotive Paint Samples by Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS) and Paint and Glass by Laser Induced Breakdown Spectroscopy (LIBS)

by Andria Hobbs -Master of Science in Forensic Science (Awarded 2003)

Glass and paints are frequently encountered forms of evidence submitted to forensic laboratories.  This study has developed methods to complement commonly used techniques in a crime laboratory to better characterize these evidence materials for forensic purposes.  Automotive paint samples have been analyzed by LA-ICP-MS to determine the discrimination power of the technique.  Optimization and validation studies were first conducted, including a homogeneity study.  Automotive paints indistinguishable by common methods have been analyzed in order to determine the forensic utility of LA-ICP-MS and have shown that LA-ICP-MS can distinguish between those samples.  Additionally, household paint samples known to contain high levels of lead were analyzed by the developed LIBS technique.  For glass samples, LIBS was able to classify the glass by type and to further distinguish 51% of the containers.  These techniques are now available for forensic scientists for the analysis of automotive paint samples and glass samples. 

Presentations:

*AAFS 56th Annual Meeting, Dallas, TX., February 2004,  “Improved Discrimination of Automotive Paints through LA-ICP-MS” A. Hobbs, T. Trejos, and J. Almirall.

SPIE's 17th Annual International Symposium on Aerospace/Defense Sensing, Simulation, and Controls, Orlando, FL.  “Trace Elemental Analysis of Glass and Paint Samples of Forensic Interest by ICP-MS Using Laser Ablation Solid Sample Introduction” J.R. Almirall, T. Trejos, A. Hobbs, and K. Furton.

*AAFS 55th Annual Meeting, Chicago, IL., February 2003,  “Comparison of the Elemental Profiling Techniques of LA-ICP-MS and LIBS for Forensic Automotive Paint Samples” A. Hobbs and J. Almirall.

*FACSS 29th Annual Meeting, Providence, Rhode Island.  “Optimization of Ablation Parameters for the Elemental Profiling of Automotive Glass and Paints by LA-ICP-MS and LIBS” A. Hobbs, S. Montero, T. Trejos, and J. Almirall.

ENSFI 8th Working Group Meeting, Madrid, Spain.  “Elemental Analysis of Glass and Paint by ICP-MS, ID-ICP-MS, and LA-ICP-MS”. J. Almirall, T. Trejos, S. Montero, and A. Hobbs.

*IAFS 16th Triennial Meeting, Montpellier, France.  “Trace Elemental Profiling of Automotive Paints by Laser Ablation- Inductively Coupled Plasma- Mass Spectrometry” A. Hobbs and J. Almirall.

ACS 223rd National Meeting, Orlando, Florida. “Sample introduction of materials of forensic interest using laser ablation for inductively coupled plasma mass spectrometry analysis of metals” S. Montero, J. Almirall, A. Hobbs, T. Trejos, L. Morris, S. Gross.

*AAFS 54th Annual Meeting, Atlanta, Georgia, February 11-16, 2002. “Elemental Profiling of glass fragments by ICP-MS as evidence of association: analysis of a case” S. Montero, A. Hobbs, T. French, J. Almirall.

* Presenting author

Publications:

J.R. Almirall, T. Trejos, A. Hobbs and S. Montero, Significance of elemental analysis comparisons for a wide variety of glass samples using ICP-MS; Description and use of a database, Journal of Forensic Science, in preparation.

A. Hobbs and J.R. Almirall, Laser Induced Breakdown Spectroscopy (LIBS) in forensic analysis of glass and paint samples, Forensic Science International, in preparation.

J. Almirall, T. Trejos, A. Hobbs, Jeannette Perr and K. Furton.  Mass spectrometry in forensic science, Advances in Mass Spectrometry, 2004, 16: 167-187.

 E. Livengood, A. Hobbs, and J.R. Almirall, A comparative analysis of GRIM2 and GRIM3 for refractive index measurements, Science and Justice; Journal of the Forensic Science Society, submitted 2003.

J.R. Almirall, T. Trejos, A. Hobbs and K.G. Furton, Trace elemental analysis of glass and paint samples of forensic interest by ICP-MS using laser ablation solid sample introduction, in Sensors, and Command, Control, Communications, and Intelligence Technologies for Homeland Defense and Law Enforcement (5071), E.M. Carapezza, Ed., Proceedings of the SPIE - The International Society for Optical Engineering, 2003, 193-204.

A. Hobbs and J.R. Almirall, Trace elemental analysis of automotive paints by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), Journal of Analytical and Bioanalytical Chemistry, 2003, 376: 1265-1271.

S. Montero,  A. Hobbs,  T. French and J.R. Almirall, Elemental profiling of glass fragments by ICP-MS as evidence of association: analysis of a case”, Journal of Forensic Sciences, 2003, 48(5) 1101-1107.

Identification of Gamma-HydroxyButyrate (GHB) and Gamma-Hydroxybutyrolactone (GBL) in aqueous samples

by Jodi Meyers- Master of Science in Forensic Science (Awarded 2003)

Gamma-HydroxyButyrate (GHB) is an inhibitory neurotransmitter with euphoric, hallucinatory and sedative effects.  In recent years there has been an increase in the abuse of this drug which has led to a demand for analytical methods of GHB.  GHB, also known as the ãdate rapeä drug, has received much media attention for its abuse as a strong sedative which is being placed in the drinks of unknowing victims at bars. 

In aqueous solutions GHB exists in equilibrium with its lactone, GBL (Gamma-Hydroxybutyrolactone).  This research will include a study of the equilibrium reached between GHB and its corresponding lactone under acidic and basic conditions.  Equilibrium ratios for solutions of GHB and GBL buffered at various pHs and maintained in different temperature environments will be determined over time using    ¹H NMR.  Further study of current methods of GHB detection will be investigated to optimize parameters and determine detection limits.  Specifically, a SPME on-fiber derivatization method followed by GC-MS analysis will be developed and optimized for detection of GHB and its analogues. 

Papers

Meyers JE, Almirall JR. A study of the effectiveness of commercially available drink coasters for the detection of ‘date rape’ drugs in beverages. J. Analyt. Tox.,Volume 28, Issue 8, November/December 2004, pp.685-689.

Meyers JE, Almirall JR.  Analysis of gamma-hydroxybutyric acid (GHB) in spiked water and beverage samples using solid phase microextraction (SPME) on-fiber derivatization/ gas chromatography-mass spectrometry (GC/MS).  Accepted to the Journal of Forensic Science 2003.

Conferences

2003 American Chemical Society Florida Annual Meeting and Exhibit, Orlando, Florida, presenting author.  “A Study of the Effectiveness of Coasters in Detecting the Presence of Illicit Date Rape Drugs in Beverages.”  Jodi E. Meyers*, and José Almirall.

2003 American Academy of Forensic Sciences, Chicago, Illinois, presenting author.  “The Analysis of gamma-Hydroxybutyric Acid (GHB) and gamma-Butyrolactone (GBL) in Forensic Samples Using GC/MS and 1H NMR.”  Jodi E. Meyers*, and José Almirall.

ACS 223rd National Meeting, Orlando, Florida, April 7-11.  “SPME on-fiber derivatization of Gamma-Hydroxybutyric Acid (GHB) in Forensic Analysis.”  Jodi E. Meyers*, Gigi Galiani, Agnes Garcia, José Almirall.

Awards

ACS Analytical Chemistry award (2000)

MBRS Rise Scholarship (2002)

Development of Microsatellite Loci in Cannabis Sativa L.

by Hussain AlGhanim - Master of Science in Forensic Science (Awarded 2003)

Microsatellite DNA or simple sequence repeat (SSR) provide an ideal tool for assessing the genetic diversity of plants due to their high information content, ease of genotyping, codominant and multiallelic nature, high discriminatory power, and reproducibility.  Microsatellites have been used successfully in agricultural and breeding studies as well as in the analysis of natural population.

Microsatellites are DNA sequences of four or fewer bases that are repeated in tandem arrays (i.e. ATATATATATATATATATAT).  Such microsatellite sequences have been found randomly distributed throughout the genomes of all eukaryotes assayed except yeast.  The highly polymorphic microsatellites have proved very useful in population genetics studies. 

This proposed work specifically aims to identify a number of microsatellite loci capable of capturing polymorphism among different Cannabis individuals. The microsatellite loci will be searched for in a systematic effort by marker enrichment technique, which consists of: 1) screening the extracted DNA of Cannabis sativa L. with specific repeat unit probes, 2) sequencing the positive clones, and 3) designing oligonucleotide primers on either side of the repeat region. 

It is felt that this information can be used to track marijuana growers and distribution networks as well as confirm (through comparisons akin to human DNA comparisons) the source of origin of individual plants. Therefore, this technique could be used by operational laboratories that have an interest in tracking marijuana sources through genetic data. 

Elemental Analysis of Forensic Glass by ICP-MS

 Shirly Montero, Ph.D.(Awarded 2002)

The value of glass evidence in forensic investigations has been well established in a number of studies and publications. Measurements of physical and optical characteristics are widely used to compare recovered pieces to a known source. However, improvements in glass quality control limit their discriminating power and have led to a need for the development of instrumental techniques for the elemental analysis of glass fragments that provide better discrimination between specimens.

This project addresses the optimization, standardization and validation of a method for the analysis of small glass samples (~ 2 mg) by ICP-MS using external calibration and isotope dilution experiments. Later on, we will also introduce laser ablation LA-ICP-MS for the analysis of glass using isotope ratios. The limitations of the instrumental techniques and the sample preparation protocols, including challenges in the dissolution of the glass or uniformity of the sample, are to be evaluated. A representative set of glasses (~1000) from a variety of sources will be analyzed by these methods to determine the informing power of elemental analysis determinations from glass specimens.

I began in the Ph.D in Chemistry program in the Spring of 1999. In the summer of 1999 I was a graduate student guest at Oak Ridge National Laboratory, Chemical and Analytical Science Division, Analytical Spectroscopy Section. Inorganic Mass Spectrometry Group.  I began my research in the Fall of 1999.

Papers

S. Montero,  A. L. Hobbs,  T. A. French,  J. R. Almirall. “Elemental Profiling of Glass Fragments by ICP-MS as Evidence of Association: Analysis of a Case” J Forens Sci , 2003, 48 (5), 1101-7.

T. Trejos,S. Montero, J.R. Almirall. “Analysis and Comparison of Glass Fragments by Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) and ICP-MS” Anal Bioanal Chem, 2003, 376, 1255-64.

D.C. Duckworth, S.J. Morton, C.K. Bayne, S. Montero, R.D. Koons and J.R. Almirall, "Forensic Glass Analysis by ICP-MS: A Multi-Element Assessment of Discriminating Power Via Analysis of Variance and Pair-Wise Comparisons", J. Anal. At. Spectrom., 2002, 17, 662-8.

D.C. Duckworth, S.J. Morton, C.K. Bayne, S. Montero, and J.R. Almirall, "ICP-MS and ID-ICP-MS Methods for the Analysis of Forensic Glass", in Proceedings of the 49th ASMS Conference on Mass Spectrometry and Allied Topics, Chicago, Illinois, May 27-31, 2001.

Conferences, Workshops and Presentations

2002 IAFS 16th Meeting, Montpellier, France, September 2-7. “Elemental analysis of glass fragments by inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS (LA-ICP-MS)” S. Montero, A. Hobbs, T. Trejos, J.R. Almirall

2002 6th European Laser Ablation ICP-MS Workshop. Utrecht, Netherlands, 24-25 June. “ICP-MS, ID-ICP-MS and LA-ICP-MS methods for the analysis of forensic glass” S. Montero, J.R. Almirall

2002 ACS 223rd National Meeting, Orlando, Florida, April 7-11. “Sample introduction of materials of forensic interest using laser ablation for inductively coupled plasma mass spectrometry analysis of metals” S. Montero, J. Almirall, A. Hobbs, L. Morris, S.Gross

2002 SPIE 16th Annual International Symposium, Orlando, Florida, April 1-5. “Associations of glass fragments by their trace elemental content using ICP-MS and LA-ICP-MS in the analysis scheme” J.Almirall, S. Montero, K. Furton

2002 AAFS 54th Annual Meeting, Atlanta, Georgia, February 11-16. “Elemental Profiling of glass fragments by ICP-MS as evidence of association: analysis of a case” S. Montero, A. Hobbs, T. French, J. Almirall

2001ASMS 49th  Annual Conference, Chicago, Illinois, May 27-31. “ICP-MS and ID-ICP-MS Methods for the analysis of forensic glass”  S. Montero, J. Almirall, D. Duckworth, C. Bayne

200 AAFS 53rd Annual Meeting, Seattle, Washington, February 19-24. “Method validation studies for glass comparisons using elemental data from ICP-MS and ID-ICP-MS” S. Montero, D. Duckworth, C. Bayne, R. Koons, J. Almirall

2000 FACSS 2000, Nashville, Tennessee, September 24-28. “Relative discriminating power of refractive index, ICP/AES, and ICP/MS for forensic glass comparisons” D. Duckworth, C. Bayne, S. Montero, J. Almirall, R. Koons

2000 FAME 2000, Orlando, Florida. “Trace elemental analysis of forensic glass by ICP-MS” S. Montero, K. Furton, J. Almirall , D. Duckworth, S. Morton, C. Bayne, R. Koons

2000 AAFS 52nd Annual Meeting, Reno, Nevada, February 21-26. “Advances in Elemental Analysis of Glass by ICP-MS” S. Montero, K. Furton, D. Duckworth, S. Morton, C. Bayne, R. Koons, J. Almirall

2000 AAFS 52nd Annual Meeting, Reno, Nevada, February 21-26. “Improved Sensitivity and Selectivity for the Detection and Identification of Ignitable Liquid Residues from Fire Debris by Ion Trap Mass Spectrometry” M. Plasencia, S.Montero, J. Krivis, A. Amstrong, J. Almirall

Constructing a database for Cannabis sativa L. Using Amplified Fragment Length Polymorphisms

by Sabrina Frank - Master of Science in Forensic Science (Awarded 2002)

In a collaborative research project between the Institute of Forensic Science at the University of New Haven, Connecticut Forensic Science Laboratory and Florida International University we have decide to focus on a single plant species, Cannabis sativa L., for the development of a molecular strategy for plant DNA typing.  We have selected Cannabis (marijuana) because it is an illegal substance grown across the United States and in other countries.  In addition cannabis is generally accepted as being a single species so botanical identification is not difficult. 

 Goals and Objectives:

The research includes the generation of DNA profiles from different Cannabis sativa L. to populate a database and to determine the genetic diversity present in the sample population. The survey of genetic diversity will result in an Amplified Fragment Length Polymorphism (AFLP) database for marijuana. The database can be used to provide linkage between marijuana growers, distributors and users.  The current technology of AFLP is a DNA typing technique used to generate large numbers of molecular markers for genetic mapping.   The use of AFLP will allow the Forensic Community and Law enforcement to improve there current methods that are being used for DNA typing.   Currently there is not a Cannabis AFLP population databases that exist for comparison with evidentiary profiles.   

Characterization of Inks and their Aging Properties

 by Louis Morris - Master of Science in Forensic Science (Awarded 2002)

The purpose of this research was to study the potential of two analytical techniques in distinguishing individual ink samples.  Lines from forty-one (22 black, 19 blue) different pens were written on three types of paper and chemically analyzed.  Thin Layer Chromatography/Laser Induced Fluorescence (TLC/LIF) was used to characterize the organic properties of dyes, while Laser Ablation Inductively Coupled Mass Spectrometry (LA/ICP/MS) examined their trace metal composition.  TLC/LIF could not discriminate twelve out of the forty-one inks using Rf values and band fluorescence.  LA/ICP/MS could not discriminate sixteen out of the forty-one inks using count ratios and relative percentages of selected metals.  Copper was the most abundant element in all forty-one inks, while lead and zinc were the best discriminators.  Seven out of the twenty-two black, and six out of nineteen blue pens could not be discriminated using either method.

I began the Master of Science in Forensic Science in the Spring of 2000 and attended a summer internship at the U.S. Secret Service Laboratory in Washington D.C.  I began my research on inks in the Fall of 2000.

FORENSIC EVALUATION OF AUTOMOTIVE LENSES

 By Susan T. Gross, Master of Science in Forensic Science (Awarded 2001)

Hit and run type accidents and other vehicle accidents often leave trace evidence behind.  This trace evidence can include small pieces of paint, body fillers, plastic bumper bars, tire rubber and/or plastic lenses.  Due to the lack of background information as to the diversity and physical and chemical properties of plastic lenses, the evidentiary value of this type of evidence is unknown. To generate the discrimination power of automotive lenses, this study proposes to analyze the lenses by five different instrumental techniques.  These techniques will examine both the organic and inorganic composition of these plastic lenses.  The five techniques that will be utilized are:  Pyrolysis Gas Chromatography (PGC), Fourier Transform Infrared Spectroscopy (FTIR), Raman Spectroscopy, Scanning Electron Microscopy - Energy Dispersive X-ray (SEM-EDX), and Laser Ablation Inductively Coupled Plasma - Mass Spectrometry (LA-ICP-MS).   Three of these techniques (PGC, FTIR and SEM-EDX) were chosen for this project since they are commonly found in forensic science laboratories and they characterize materials based on both organic and inorganic content.  Two additional instruments that will be utilized in this project, that may provide additional information, are Raman and LA-ICP-MS.  The informing power of using each of the techniques by itself and the informing power of using the techniques in combination are being researched. Automotive lenses of known origin are being analyzed in triplicate by PGC, FTIR, SEM-EDX, Raman, and LA-ICP-MS.  Various autobody shops and junk yards were contacted to obtain a representative cross-section of automotive lenses that would be expected to be found at a crime scene.  Automotive lenses were obtained from a variety of vehicles of model years 1985 through 2000.  Both American and Foreign cars were included in this diverse sample set.  Quantitative data from all five instrumental techniques will be summarized and evaluated by the method of Smalldon and Brown for the determination and assessment of discrimination power.

I began in the Master's of Forensic Science program in the Fall of 1999.  I began my research in the Spring of 2000.  My research will be presented at the American Academy of Forensic Sciences at the 2001 Meeting in Seattle, Washington , February 19 - 24.

Papers:

S. Gross, J. Wilson, R. Duevel and J.R. Almirall, ãEvaluation of Automotive Lenses for Forensic Applications by FTIR, PGC, Raman, and Laser Ablation ICP-MSä, Journal of Forensic Sciences, 2002, submitted.

Gross, S. "Detecting Psychoactive Drugs in the Developmental Stages of Mushrooms". J Forensic Sci 2000; 45(3): 527-537.

Conferences:  

Gross, S. "Detecting Psychoactive Drugs in Mushrooms" oral presentation at the Midwestern Association of Forensic Scientists Meeting, October 1998.

Gross, S., Garcia, A.D., Almirall, J. R. "The Analysis of the Psilocybe Cyanescens (Wakefield) Mushroom"  oral presentation at the American Academy of Forensic Sciences Meeting, February 1999.

Almirall, J. R., Gross, S., Garcia, A.D., ãA Comparison of GC-MS, LC-ECD, LC-MS, and CE Methods for the Analysis of the Psilocybe Cyanescens (Wakefield) Mushroomä oral presentation at the Pittcon Meeting, March 1999.  

Gross, S., Garcia, A.D., Almirall, J. R. "The Analysis of the Psilocybe Cyanescens (Wakefield) Mushroom"  poster presentation at the International American Academy of Forensic Sciences Meeting, August 1999.

Awards:

New Scientist Award Recipient.  Award presented by Midwestern Association of Forensic Scientists, October 1999.

 Identification and Characterization of Pyrolysis Products in Fire Debris Analysis

 By Eric Stauffer, Master of Science in Forensic Science - 2001

The objective of my research is to identify and characterize pyrolysis products found in fire debris in order to distinguish these compounds from possible ignitable liquid residues (ILR).

Pyrolysis products are released by burning substrate during a fire. These products produce a response in a gas chromatograph that can mask the pattern of petroleum distillates, during the analysis of fire debris in a suspected arson case. Different objects and materials commonly encountered in fire debris analysis have been burned under different conditions and their pyrolysis products have been studied.

Common materials considered to be possible sources of pyrolysis products once burned, and found in residential buildings have been classified into four main levels of types of substrates. Level 1 includes materials fixed on the floor, walls and ceiling of a building. Level 2 includes all the furniture and other large items that can be found in a room. Smaller objects found inside or nearby the furniture constitute level 3 type substrates. Finally, level 4 items are categorized as components within larger objects but are present in small quantities and not part of the bulk material of the object for example, the dyes found in carpet fibers. The dyes themselves would classify as level 4 while the polymer material of the carpet would classify as level 1.

Each level is then separated into sublevels according to the class of compounds of the materials and objects found in each level such as polymers from a carpet fiber, wood products from a furniture item, natural fibers from cloth materials, etc.  This classification has been constructed in order to be able to group some target pyrolyzates by both object types and by material (chemical) composition, after burning.

A first study of pyrolysis products has been conducted under controlled heating conditions with a Pyrolyzer-Gas Chromatograph-Mass Spectrometer (CDS AS-2500, HP 6890-HP 5973). By using a pyrolyzer it has been possible to obtain the set of pyrolysis products released by the substrates under specific temperature conditions. Generally, there are only three degradation mechanisms by which the pyrolysis process occurs. The first one is random scission, which is the production of free radicals along the backbone of the polymer. The second is the side group scission, where the backbone loses molecules or atoms attached to it. The final one is monomer reversion in which the polymer returns simply to its monomer. Hence, it has been possible to study these degradation mechanisms and to compare them to the pyrolyzates obtained during the analyses.

Samples have been burned under different conditions and extracted in the same way that ILR are usually extracted from fire debris. Passive headspace extraction using activated charcoal strip and elution with carbon disulfide has been used in this study. Analyses of the resulting extract were conducted with both GC-FID (HP 5890) and GC-MS (Varian 3400cx and Varian 2000).

Resulting chromatograms were compared to the ones obtained by Py-GC/MS in order to estimate the influence of the different burning conditions and the extraction procedure. Then, these have been compared to a collection of ILR standards in order to estimate their interference using peak pattern analysis.

It is possible to construct a classification of the pyrolysis products with respect to the different levels of objects and substrate materials. In addition, it has been possible to estimate some parameters in the burning procedure and in the extraction procedure that influence the presence of pyrolysis products. Finally, It has been possible to show the interference of pyrolysis products with the recovery of ILR.  Furthermore, a comparison of the relative detection limits of gasoline in the presence of pyrolysis products is presented. The effectiveness of using a GC-FID compared to a GC-MS or GC-MS-MS is also presented. These studies show the improved detection and identification of ILR in the presence of pyrolyzates when GC-MS or GC-MS-MS are used over just GC-FID alone. 

I began my Master of Science in Forensic Science degree program at FIU and joined the group in the Fall of 1999.

Participation at the Annual Meeting of the American Academy of Forensic Sciences in Reno, Nevada, 2000.

"Fire debris analysis by comprehensive two-dimensional gas chromatography", Presented at the Florida International University 2000 Scholarly Forum.

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