Rapid analysis of forensic samples using an atmospheric solid analysis probe interfaced to a linear ion trap mass spectrometer.

RATIONALE: This paper highlights the simplicity of interfacing an Atmospheric Solid Analysis Probe (ASAP) to a Linear Ion Trap Mass Spectrometer and shows that this technique can be used for the rapid generation of high-quality data from a range of sample types with minimal or no sample preparation. METHODS: For a solid sample or surface deposit, the process entails rubbing a capillary melting tube a few times on the sample to transfer material to the capillary surface and then introducing it into the source of the mass spectrometer. Similarly, for a liquid sample, a capillary tube is dipped into the sample to just coat the surface or a few microliters may be applied to the tip of a capillary before being analyzed by Atmospheric Pressure Chemical Ionization in both positive and negative mode. RESULTS: A rodenticide containing brodifacoum, black tar heroin and its impurities (morphine, codeine, noscapine, papaverine, and monoacetylmorphine), crack cocaine and 1-methylaminoanthraquinone dyestuff were successfully analyzed directly without any sample preparation. All compounds were detected using full scan mass spectrometry (MS), followed by confirmation by MS/MS. Preliminary results suggest that this technique could be used for quantitation. CONCLUSIONS: Interfacing the ASAP to an ion trap mass spectrometer allows the ability to perform full scan, MS(n) experiments, and rapid positive/negative switching from a single sample introduction. Because of these features, this instrument is very useful for rapid, routine analysis and for confirmation with the use of in-house MS/MS libraries.

Analysis of trace amount of bank dye and lachrymators from exploding bank devices by solid-phase microextraction and gas chromatography-mass spectrometry.

Solid-phase microextraction (SPME) is a fast, solvent-free alternative to conventional sample preparation techniques. This technique involves exposing a fused silica fiber that has been coated with a stationary phase to an aqueous solution or its headspace to selectively extract compounds from their matrix. The fiber is then removed, and the analytes are thermally desorbed in the injector of a gas chromatograph. By sampling from the headspace above sample matrices, SPME can be used to extract target analytes from very complex matrices. In this study, SPME in the headspace is used in developing a method for the dye 1-methylaminoanthraquinone (MAAQ) and two lachrymators: orthochlorobenzalmalononitrile (CS) (tear gas) and 2-chloroacetophenone (CN) (tear gas). The focus is to develop a robust method to minimize sample preparation and to reduce matrix interferences encountered by other extraction techniques. In developing the method, several fibers are studied for their affinity for the compounds of interest. Although this method is developed for qualitative analysis, the extraction time and temperature profile are thoroughly investigated to provide the optimal conditions. The use of a salt solution is evaluated to increase the partitioning of MAAQ into the headspace. Using this method, qualitative extraction is achieved for the analysis of CN, CS, and MAAQ from its matrices. CN and CS are extracted in less than 5 min, though MAAQ needed more than 15 min to achieve a reasonable response. If more sensitivity is required, the use of a salt solution increases the response of MAAQ by 90-fold.