Quantitative Analysis of Polycyclic Aromatic Hydrocarbons at Part Per Billion Levels in Fish Oil by Headspace Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry (HS-SPME-GC-MS).

Headspace solid-phase microextraction (HS-SPME) was used in combination with gas chromatography-mass spectrometry (GC-MS) for the analysis of polycyclic aromatic hydrocarbons (PAH) at part per billion levels in fish oil samples collected from menhaden fish. The method was initially developed using fish oil from capsules spiked with a standard PAH mixture. The final HS-SPME-GC-MS method presented a linear range from 3 to 1,500 ng/g, with precision for most analytes <10% relative standard deviation.

"Retention projection" enables reliable use of shared gas chromatographic retention data across laboratories, instruments, and methods.

Gas chromatography/mass spectrometry (GC/MS) is a primary tool used to identify compounds in complex samples. Both mass spectra and GC retention times are matched to those of standards; however, it is often impractical to have standards on hand for every compound of interest, so we must rely on shared databases of MS data and GC retention information. Unfortunately, retention databases (e.

Determination of steroids, caffeine and methylparaben in water using solid phase microextraction-comprehensive two dimensional gas chromatography-time of flight mass spectrometry.

Analysis of several emerging contaminants (steroids, caffeine and methylparaben) in water using automated solid-phase microextraction with comprehensive two dimensional gas chromatography coupled to time of flight mass spectrometry (SPME-GCxGC-ToF/MS) is presented. Experimental design was used to determine the best SPME extraction conditions and the steroids were not derivatized prior to injection. SPME-GCxGC-ToF/MS provided linear ranges from 0.

Analysis of Salvinorin A in plants, water, and urine using solid-phase microextraction-comprehensive two-dimensional gas chromatography-time of flight mass spectrometry.

Salvinorin A, a psychoactive hallucinogen, and related compounds, were analyzed in plants, water, and urine using liquid-liquid extraction (LLE), solid-phase microextraction (SPME) and comprehensive two-dimensional gas chromatography-time of flight mass spectrometry (GC×GC-ToFMS). A semi-qualitative study of the extraction of Salvinorin A and analogs from Salvia divinorum plants by LLE showed ppb levels of Salvinorin A and several analogs in the leaves and stems of S. divinorum plants, much lower than expected.

Sample preparation for gas chromatography using solid-phase microextraction with derivatization.

The development of SPME over the past 20 years, and the more recent wide availability of automated SPME systems, has generated renewed interest in derivatization with gas chromatography for the analysis of highly polar or labile analytes. By using an SPME fiber as the extracting phase, the derivatization process is straightforward and readily automated. From anecdotal examination of the literature, it appears that the fiber may offer benefits over traditional liquid phase reactions in that control over the selectivity of the reaction for the desired product and fewer interfering byproducts may be more readily achieved.

Stir-bar sorptive extraction and thermal desorption-ion mobility spectrometry for the determination of trinitrotoluene and l,3,5-trinitro-l,3,5-triazine in water samples.

Stir-bar sorptive extraction (SBSE) is interfaced to ion mobility spectrometry (IMS) for the rapid detection of trace analytes, with the explosives, trinitrotoluene (TNT) and l,3,5-trinitro-l,3,5-triazine (RDX) shown as examples. SBSE retains its inherent advantages as a sensitive, straightforward, solventless, and inexpensive method. Additionally, the new SBSE-IMS technique exhibits excellent sensitivity, has onsite field analysis capabilities and provides the potential to detect and quantitate analytes that are difficult to accomplish using gas chromatography (GC) or high-performance liquid chromatography (HPLC).

Determination of parabens in pharmaceutical formulations by solid-phase microextraction-ion mobility spectrometry.

Solid-phase microextraction (SPME) coupled with ion mobility spectrometry (IMS) was used for the detection and quantitation of 4-hydroxybenzoate preservatives, methylparaben, ethylparaben, propylparaben, and butylparaben, in commercial pharmaceutical products. For the first time, SPME-IMS is described for the simultaneous detection, separation, and quantitation of multiple analytes in complex matrixes. The parabens are extracted from the samples using SPME, and the analytes on the fiber are heated by the IMS desorber unit and vaporized into the drift tube.

Solid phase micro-extraction coupled with ion mobility spectrometry for the analysis of ephedrine in urine.

Quantitative solid phase micro-extraction (SPME) coupled with ion mobility spectrometry is demonstrated using the analysis of ephedrine in urine. Since its inception in the 1970's ion mobility spectrometry (IMS) has evolved into a useful technique for laboratories to detect explosives, chemical warfare agents, environment pollutants and, increasingly, for detecting drugs of abuse. Ephedrine is extracted directly from urine samples using SPME and the analyte on the fiber is heated by the IMS desorber unit and vaporized into the drift tube.

Evaluation of the origins of the selectivity of polymers imprinted with a HIV protease inhibitor using infrared spectroscopy and high performance liquid chromatography.

This work investigates the origins of enantioselectivity of polymers imprinted with the HIV protease inhibitor, Indinavir. For the preparation of imprints of the drug, the critical interactions between the functional monomer, methacrylic acid, and Indinavir were characterized by infrared (IR) spectroscopy to explore the optimum functional monomer concentration for the polymerization. It was shown that a polymer with high selectivity and minimum non-selective binding for Indinavir was obtained when prepared with enough functional monomer to hydrogen bond with all of the functional groups of the drug without using an excess of monomer.