The Direct Analysis in Real Time (DART) ion source is a relatively new mass spectrometry technique that is seeing widespread use in chemical analyses world-wide. DART studies include such diverse topics as analysis of flavors and fragrances, melamine in contaminated dog food, differentiation of writing inks, characterization of solid counterfeit drugs, and as a detector for planar chromatography. Validation of this new technique for the rapid screening of forensic evidence for drugs of abuse, utilizing the DART source coupled to an accurate mass time-of-flight mass spectrometer, was conducted. The study consisted of the determination of the lower limit of detection for the method, determination of selectivity and a comparison of this technique to established analytical protocols. Examples of DART spectra are included. The results of this study have allowed the Virginia Department of Forensic Science to incorporate this new technique into their analysis scheme for the screening of solid dosage forms of drugs of abuse.
A new screening method for detecting gamma-hydroxybutyric acid (GHB) in drink matrices, using the IonSense, Inc. (Saugus, MA) direct analysis in real time (DART) ion source coupled to a JEOL exact mass time-of-flight mass spectrometer (AccuTOF), was validated and compared with the current screening methodology. The DART ion source allows for analysis of samples under ambient conditions with little to no sample preparation. Fifty drink specimens were spiked at levels of 1, 2, 3, and 4 mg/mL GHB, and analyzed on the AccuTOF-DART. Positive detection of GHB occurred for each of the samples at each concentration level, giving 100% accuracy for the samples tested. Twenty-five of the 50 drink specimens were spiked at 1 mg/mL GHB and tested using a color test known as the GHB Color Test #3. Only two of these 25 specimens tested positive for the presence of GHB, giving only 8% accuracy. Implementation of this new methodology as a screening tool for GHB analysis will quickly eliminate negative specimens allowing the examiner to focus analysis time on those that screened positive.
Thin layer chromatography (TLC) is a technique that is commonly employed in the forensic drug analysis of pharmaceutical preparations. Detection is typically accomplished using various visualization spray reagents. Conventional gas chromatography-mass spectrometry (GC-MS) analysis is typically performed to confirm the TLC results. Depending on the drugs tested and the instrument conditions required, this confirmation can take up to an hour to complete. Direct analysis in real time (DART™) is an ionization source, coupled to an accurate-mass time-of-flight mass spectrometer that has the capability to ionize materials under ambient conditions. To streamline analysis, the combination of TLC with DART™ detection is proposed to screen and subsequently identify drug compounds, all from the same TLC plate. DART™ confirmations of TLC analyses take <10 min to complete and compare favorably to GC-MS in sensitivity and selectivity. This study validates the use of TLC-DART in the forensic identification of the components of several pharmaceutical preparations.
Nylons are chemically synthesized polymers that are used in a variety of ways. This study differentiates multiple nylon types using direct analysis in real time (DART) coupled with an orthogonal-acceleration time-of-flight (oaTOF) mass spectrometer (MS). Seven closely related nylon standards were studied. A DART helium gas temperature of 275 °C was chosen as an optimum for the analysis of nylons. Use of collision induced dissociation (CID) to induce fragmentation increased the power of discrimination. All seven nylon standards were successfully differentiated and identified using DART-MS.
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