Adventures at the Mississippi

Crime Laboratory
Mississippi Crime Laboratory
Locations:
Jackson Main Laboratory
Batesville
Meridian
Gulf Coast
Laboratory Divisions:
Impression Evidence Division
Latent Print
Firearm and Tool Mark
Questioned Documents

Analytical Division
Toxicology
Controlled Substances Identification
Trace Evidence
Implied Consent

Bioscience Division
Conventional Serology
DNA Testing
Offender DNA Database (CODIS)

Crime Scene Assistance

Our Trip to the Jackson Lab
Autopsy performed by
State Medical Examiner,
Dr. Davis
Examination of body
Collection of fingerprints
and fluids
Body excision
Collect and weigh organs
Hold until funeral service
Evidence Collection
Evidence vault
Chain of Custody
JusticeTrax
Filing room

Bioscience




Blood Testing
Kastle-Meyer
ABAcard HemaTrace
Takayama
Document physical description
Determine presence of biological fluid
Semen Testing
Poly-light
Acid-Phosphatase
Prostate Specific Antigen (P30)
ABAcard
Mock Case
Presumptive: Kastle-Meyer Test
Comfirmatory: ABAcard & HemaTrace
Controlled Substance Unit:
Drug Guys
GC-MS: workhorse for drug identification


Drug Analysis



Frequently Submitted
Marijuana
Cocaine
Medicinal tablets
Methamphetamine

Unique Submissions
LSD
Mushrooms
Drug Identification
Presumptive Testing
Library search for tablets
Color Tests
Microscopic Analysis
pH Testing

Confirmatory Testing
GC-MS
IR Spectroscopy
Mock Case:
Psilocybin Mushrooms
Latent Print
Collecting Fingerprints
Methods
Comparison Testing
Automated Fingerprint Identification System
&


Coming Soon. Footprint Section
Collecting Fingerprints
Methods
Ninhydrin
AccuTrans
Black Powder
Magnetic Powder
Superglue Chamber
Amido Black
Iodine Fuming
Crystal Violet


Fingerprint Patterns
Ridge Bifurcation
Footprint Section
Senior Research
Qualitative Approach for the Detection of Carryover
on a GC/MSD System
Gas chromatography (GC) is an effective method used to separate compounds
into various components. The effluent of the GC instrument is the fed to the
mass spectrometer (MS) instrument, which provides identification of the
compounds present. The ability to detect and correct systematic errors that occur
within the GC-MS is critical in maintaining the creditability and authenticity of
their results in a court of law. Forensic analysts depend on the precision and
accuracy of the instruments they use for identification of drugs. To ensure that
carryover and other errors remain minimal to none at all, there must only exist
analysts that are attentive and have the proper training and education to present
the most accurate and precise data available. To do so, a control standard made
of methamphetamine, diphenhydramine, lidocaine, amitriptyline, cocaine, and
codeine standards in methanol was analyzed with the GC-MS to determine how
many samples must be continuously injected for carryover appear. In addition,
samples containing various THC concentrations were analyzed to establish the
lowest concentration of THC at which carryover contamination could be
confirmed.



Qualitative Approach for the Detection of Carryover on a GC/MSD System
Cara Haven, Kallie Mosley
Department of Chemistry and Biochemistry, University of Mississippi, Oxford, MS. 38677.
Research Overview and Purpose
Methods
1."Marinol Capsules (Unimed), Drug Reference Encyclopedia." Marinol Capsules (Unimed), Drug
Reference Encyclopedia. Web. 7 May 2014.
http://www.theodora.com/drugs/marinol_capsules_unimed.html.
2.Chromatography Today Help Desk. "Why do I have Carryover?." Chromatography Today 3 Sept.
2013: 40-44. Chromatographytoday.com. Web. 16 Apr. 2014.
3.Goldberger, B. A., M. A. Huestis, and D. G. Wilkins. Commonly Practiced Quality Control and
Quality Assurance Procedures for Gas Chromatography/Mass Spectrometry Analysis in Forensic Urine
Drug-Testing Laboratories . Taoyuan County, Taiwan: Central Police University Press, 1997. Print.
References
Conclusions











It is important for forensic scientists to correctly and adequately obtain
analytical data that can be used in a court of law and can do so by following
the guidelines and Standard Operating Procedures set out by the crime
laboratory. Examination of the control standard sequence results showed no
signs of carryover in any of the methanol blanks, which is also true for the
THC sequence. However, carryover was present in the samples containing
higher concentrations of THC. Delta-9-tetrahydrocannabinol was confirmed
with mass spectra. This assessment further validates the necessity of
having attentive chemists with respectable training in order to detect and
correct for systematic and random errors that occur in the instruments of
use. It is vital for analysts to be cautious of the numerous factors that cause
these errors and be able to take the appropriate measures to solve the
problem. This research focuses on the systematic error of carryover that can
occur in the GC/MSD system and how analysts should prevent, if not detect
and resolve this error.

Control Standard
Two 1.5mL samples of test mix and two 1.5mL vials of MeOH prepared and
run on Agilent 5975C TAD Series GC/MSD system
Injection count in between the solvent blanks was steadily increased by one
until reaching a maximum of 15
Tetrahydrocannabinol
THC extracted from ten marijuana samples by saturation of MeOH followed
by 0.1mL of each sample transferred to separate vials and diluted to a final
volume of 1.5mL with MeOH
Injection count was gradually increased from one to 15 samples between the
MeOH blanks
Tetrahydrocannabinol & Carryover
THC extracted from 1.35 grams of marijuana by MeOH saturation
6 samples with various concentrations of THC 0.25mL, 0.5mL, 0.75mL,
1.0mL, 1.25mL, and 1.5mL - were transferred to individual vials and diluted
with MeOH to a final volume of 1.5mL
MeOH blank sample ran after each THC injection and examined for presence
of carryover
Results
Figure 4 Mass spectrum of Delta-9-Tetrahydrocannabinol peak detected in solvent
blank MeOH-G was confirmed with the spectral match from the library database.

After 15 injections of the control standard, the methanol blank was
examined and showed no presence of carryover. The last methanol blank
after the THC injections was also negative for presence of carryover.
However, four of the seven blank samples in the run with various THC
concentrations (Figure 3) were positive for carryover. Upon examination of
the blank injected after the 0.50 mL THC sample (Figure 2, MeOH-C), the
peaks of THC are visible but not enough is present to confirm. The
remaining blank samples (Figure 2, MeOH-D-MeOH-G) have defined
peaks. Mass spectra of these peaks were obtained and confirmed the
presence of delta-9-tetrahydrocannabinol due to carryover, shown in Figure
4.
Figure 1 Delta-9-
tetrahydrocannabinol
is confirmed with the
presence of peaks at
mass-to-charge ratios
of 299 and 314,
respectively.
Figure 3 Six samples
containing different
volumes of THC were
analyzed to test for the
presence of carryover.
Figure 2 A comparison of the total ion chromatogram (TIC) of the solvent
blanks after the THC injections, with the top TIC (MeOH-C) taken from the
blank after 0.5 mL THC sample and the bottom (MeOH-G) after the 1.50
mL THC sample.
A
B
U
N
D
A
N
C
E

LC/MS/MS