Time Intensity Q1Q2 CID ASAP Probe Corona ConeAbstract. Amphetamine-type stimulants (ATS) are among illicit stimulant drugs that are most often used worldwide. A major challenge is to develop a fast and efficient methodology involving minimal sample preparation to analyze ATS in biological fluids. In this study, a urine pool solution containing amphetamine, methamphetamine, ephedrine, sibutramine, and fenfluramine at concentrations ranging from 0.5 pg/mL to 100 ng/mL was prepared and analyzed by atmospheric solids analysis probe tandem mass spectrometry (ASAP-MS/MS) and multiple reaction monitoring (MRM). A urine sample and saliva collected from a volunteer contributor (V1) were also analyzed. The limit of detection of the tested compounds ranged between 0.002 and 0.4 ng/mL in urine samples; the signal-to-noise ratio was 5. These results demonstrated that the ASAP-MS/MS methodology is applicable for the fast detection of ATS in urine samples with great sensitivity and specificity, without the need for cleanup, preconcentration, or chromatographic separation. Thus ASAP-MS/MS could potentially be used in clinical and forensic toxicology applications.

The present work describes the development and analytical validation of a method involving microextraction packed sorbent and gas chromatography coupled to mass spectrometry (MEPS-GC-MS) for the multi-residue analysis of 22 pesticides (permethrin, fenpropathrin, aldrin, α-hexachlorocyclohexane, β-hexachlorocyclohexane, lindane, vinclozolin, endosulfan, heptaclor, dodecaclor, tetradifon, 1,1-dichloro-2,2-bis (p-chlorophenyl)ethane, 1,1-bis(p-chlorophenyl)-2,2-dichloroethylen, carbofuran, carbaryl, pirimiphos methyl, chlorpyriphos, dimethoate, disulfoton, fenamiphos, terbufos and profenofos) in honey samples. The MEPS variables of sample pH, draw-eject cycles, ionic strength and desorption procedure were optimized to improve the sensitivity of the proposed method. The method was shown to be linear at concentrations ranging from 2, 5 and 10 ng/g (limit of quantification) to 75-100 ng/g. These values are lower than those established as the maximum residue limits for honey samples. The accuracy values (82-114%) were adequate for all the analytes, as were the inter-day precision data, with coefficient of variation lower than 14%. On the basis of analytical validation, the MEPS-GC methodology has been shown to be a promising alternative for the analysis of pesticides in honey samples. The MEPS packed syringe can be reused 40 times for honey samples, whereas the conventional solid-phase extraction (SPE) column can only be used once. Compared with liquid-liquid extraction and SPE, MEPS is able to reduce sample preparation time and organic solvent consumption.

& Rapid and sensitive analytical method for the simultaneous determination of sulfonamides (sulfacetamide, sulfadiazine, sulfathiazole, sulfamethazine, sulfamethoxypyridazine, and sulfamethoxazole) in poultry litter wastewater samples by microextraction packed sorbent (C8) and liquid chromatography with spectrophotometric detection (MEPS=LC) analysis. We evaluated how MEPS variables, such as the pH extraction, draw-eject cycles, ionic strength, and desorption conditions (solvent and solvent volume) affected extraction performance, to obtain a more efficient extraction process in the proposed method. The proposed MEPS=LC method presented linear range at concentrations from 5.0 ng mL À1 (Limit of quantification -LOQ) to 200 ng mL À1 , inter-day precision with coefficient of variation lower than 8%, correlation coefficient greater than 0.998; the extraction phase C8 was used. On the basis of analytical validation, the MEPS=LC methodology can be used to analyze sulfonamides in poultry litter wastewater samples.