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.

Benzodiazepines and metabolites from biological fluids by liquid chromatography electrospray tandem mass spectrometry.

Solid-phase extraction and liquid chromatography-tandem mass spectrometry are invaluable techniques for the determination of benzodiazepines and metabolites in biological matrices. The reason for using tandem mass spectrometry is to increase limits of detection without the need for chemical derivatization. Here we describe a technique for the detection of 26 benzodiazepines and metabolites at a detection limit of approximately 1-2 ng/mL in blood and 1-5 ng/mL in urine when screened using a data-dependent scan method.

Complete automation of solid-phase extraction with subsequent liquid chromatography-tandem mass spectrometry for the quantification of benzoylecgonine, m-hydroxybenzoylecgonine, p-hydroxybenzoylecgonine, and norbenzoylecgonine in urine--application to a high-throughput urine analysis laboratory.

A fully automated system utilizing a liquid handler and an online solid-phase extraction (SPE) device coupled with liquid chromatography-tandem mass spectrometry (LC-MS-MS) was designed to process, detect, and quantify benzoylecgonine (BZE), meta-hydroxybenzoylecgonine (m-OH BZE), para-hydroxybenzoylecgonine (p-OH BZE), and norbenzoylecgonine (nor-BZE) metabolites in human urine. The method was linear for BZE, m-OH BZE, and p-OH BZE from 1.2 to 10,000 ng/mL with limits of detection (LOD) and quantification (LOQ) of 1.2 ng/mL. Nor-BZE was linear from 5 to 10,000 ng/mL with an LOD and LOQ of 1.2 and 5 ng/mL, respectively. The intrarun precision measured as the coefficient of variation of 10 replicates of a 100 ng/mL control was less than 2.6%, and the interrun precision for 5 replicates of the same control across 8 batches was less than 4.8% for all analytes. No assay interference was noted from controls containing cocaine, cocaethylene, and ecgonine methyl ester. Excellent data concordance (R2 > 0.994) was found for direct comparison of the automated SPE-LC-MS-MS procedure and an existing gas chromatography-MS procedure using 94 human urine samples previously determined to be positive for BZE. The automated specimen handling and SPE procedure, when compared to the traditional extraction schema, eliminates the human factors of specimen handling, processing, extraction, and derivatization, thereby reducing labor costs and rework resulting from batch handling issues, and may reduce the number of fume hoods required in the laboratory.