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A method has been developed to quantify the nitrofuran metabolites 3-amino-5-morphorinomethyl-1,3-oxazolidinone, 3-amino-oxazolidinone, 1-aminohydantoin, and semicarbazide, as well as chloramphenicol in shrimp with a single extraction procedure followed by LC-MS/MS analysis. Dynamic selected reaction monitoring with positive and negative ionization mode switching was used. The method LODs were 0.5 ng/g for the nitrofuran metabolites and 0.3 ng/g for chloramphenicol.

A collaborative study was conducted to evaluate stable isotope dilution assay (SIDA) and LC-MS/MS for the simultaneous determination of aflatoxins B1, B2, G1, and G2; deoxynivalenol; fumonisins B1, B2, and B3; ochratoxin A; HT-2 toxin; T-2 toxin; and zearalenone in foods. Samples were fortified with 12 13C uniformly labeled mycotoxins (13C-IS) corresponding to the native mycotoxins and extracted with acetonitrile/water (50:50 v/v), followed by centrifugation, filtration, and LC-MS/MS analysis. In addition to certified reference materials, the six participating laboratories analyzed corn, peanut butter, and wheat flour fortified with the 12 mycotoxins at concentrations ranging from 1.0 to 1000 ng/g. Using their available LC-MS/MS platform, each laboratory developed in-house instrumental conditions for analysis. The majority of recoveries ranged from 80 to 120% with relative standard derivations (RSDs)

Drug adulteration in dietary supplement materials is a world-wide problem and poses a regulatory challenge. Red yeast rice is a product used by consumers to lower blood levels of cholesterol. While most current methods to analyze red yeast rice are based on HPLC separation with a photo-diode array detector and/or a mass spectrometry detector, which takes 20-40min analysis time per sample, we developed a method to do fast screening of the active compound lovastatin by direct infusion into a mass spectrometer. This method takes under 1min per analysis on the instrument. By using multiple reaction monitoring with five product ions, all the ion ratios of the analyte in the samples are compared with those from the standards for qualitative analysis. The results from this method were compared to the result from the liquid chromatography tandem mass spectrometry, which uses retention time and one ion ratio as the confirmation criteria. No false positives or false negatives were found among the 12 samples tested. The method also seems to be effective in measuring the lovastatin in red yeast rice semi-quantitatively. This kind of method could be adapted to the screening of other dietary supplement products.

A new method has been developed using flow injection tandem mass spectrometry to semi-quantitatively screen for weight loss drugs, including sibutramine, N-desmethylsibutramine, N-didesmethylsibutramine, and phenolphthalein in dietary supplements. Positive identification of these drugs in samples was further confirmed and quantified by liquid chromatography tandem mass spectrometry. The degradation products of sibutramine were observed and identified by LC–MS/MS which include N-desmethylsibutramine, N-didesmethylsibutramine, N-formyldesmethylsibutramine, and N-formyldidesmethylsibutramine.

A flow injection tandem mass spectrometry method (FI-MS/MS) has been developed to detect enzyme phosphodiesterase type 5 inhibitors, including tadalafil, sildenafil, and vardenafil. Multiple reaction monitoring (MRM) was used to detect the drugs and product ion ratios were used for identification. FI-MS/MS was used for semi-quantification and liquid chromatography tandem mass spectrometry (LC-MS/MS) was used for further confirmation and quantification. One of 13 samples has been found to be adulterated with prescription levels of tadalafil and also low level of sildenafil. The method can be used for screening large numbers of herbal products for adulteration since it takes less than 1 min without chromatographic separation on a column.

Six different types of fabrics were compared for their ability to protect against human exposure to three different commercial household aerosol insecticides. Fabrics used in this investigation were, 100% cotton, cotton-polyester thermal underwear, cotton-polyester blend (twill), 100% acrylic, 100% wool and artificial silk (rayon). The household insecticides were, Black Flag (Ant and Roach Killer), Raid (Ant and Roach Killer) and Hot Shot (Wasp and Hornet Killer) containing propoxur, permethrin/pyrethrins and chlorpyrifos/allethrins as their active ingredients respectively. A fluorescent tracer, 4-methyl-7-diethyl amino coumarin was mixed with the aerosol (or equivalent aliquot) and sprayed onto cloth squares fitted on Whatman paper patches. The percentage of penetration through the cloth was quantified by the intensity of the fluorescence spectrum of each patch extract and the amount of the tracer recovered was calculated. The extract was concentrated to 1/10th of the volume to measure the content of each of the insecticides by supercritical fluid chromatography (SFC) using electron capture (ECD) and diode array detectors. Scanning electron microscope (SEM) images of the fabrics showed the geometry of the yarn. The results obtained from the fluorescence spectra, SFC and SEM showed that cotton-polyester (twill), cotton, wool and cotton thermal underwear were the least penetrable materials for the aerosols. On the other hand, acrylic and artificial silk (rayon) were the most penetrable cloth types.