Offline Solid-Phase Extraction and Separation of Mineral Oil Saturated Hydrocarbons and Mineral Oil Aromatic Hydrocarbons in Edible Oils, and Analysis via GC with a Flame Ionization Detector.

A method was developed for the determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in edible oils, achieving similar limits of quantification than those obtained by online extraction methodologies, i.e., 0.5 mg/kg. The isolation of MOSH and MOAH was performed in a silver nitrated silica gel stationary phase prior to their analysis by gas chromatography-flame ionization detector (GC-FID). To improve the sensitivity, the simulated on-column injection method, using a suitable liner, was optimized. The method was validated at 0.5, 10.0 and 17.9 mg/kg, and recoveries ranged from 80 to 110%. Intra and inter-day precision were evaluated at the same levels, and relative standard deviation (RSD) was lower than 20%. The method was applied to a total of 27 samples of different types of oil previously analyzed in an accredited laboratory, detecting MOSH up to 79.2 mg/kg and MOAH up to 22.4 mg/kg.

Development and validation of an ultra-high performance liquid chromatography-tandem mass-spectrometry (UHPLC-MS/MS) method for the simultaneous determination of neurotransmitters in rat brain samples.

A simple method for the simultaneous determination of glutamate, γ-aminobutyric acid (GABA), choline, acetylcholine, dopamine, 5-hydroxyindole-3-acetic (5-HIAA), serotonin, 3,4-dihydroxyphenylacetic acid (DOPAC) and homovanillic acid (HVA) was developed by using ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). These compounds are analysed in a single chromatographic run in less than 8 min, adding heptafluorobutyric acid (HFBA) in the mobile phase to improve the separation of the selected neurotransmitters. The analytes were detected using electrospray ionization (ESI)-MS/MS in positive mode with multiple reaction monitoring (MRM). Good linearity was obtained (R² > 0.98) and the intra and inter-day precision of the method (expressed as relative standard deviation) were lower than 26%. Limits of quantification were lower than 2.440 µg/g of brain in all the cases, allowing the sensitive determination of these compounds in rat brain extracts. Therefore, the method was successfully applied for the quantitative determination of neurotransmitters in several rat brain regions (prefrontal cortex, striatum, nucleus accumbens and amygdala), detecting glutamate, GABA and choline at concentrations higher than 1000 µg/g, 30 µg/g and 100 µg/g respectively, whereas the other compounds were found at lower concentrations.

Fast determination of herbicides in waters by ultra-performance liquid chromatography/tandem mass spectrometry.

A rapid multiresidue method for the analysis of more than 40 herbicides (such as simazine, terbuthylazine and diuron) in waters has been developed and validated by ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC/MS/MS). Prior to chromatographic determination, the samples were extracted using a solid-phase extraction procedure. The analysis was performed on an Acquity UPLC BEH C(18) column using a gradient elution profile and a mobile phase consisting of methanol and an aqueous solution of formic acid (0.01%). Other chromatographic and MS/MS parameters were optimised in order to improve selectivity and sensitivity of the analytes. The analytes were detected using electrospray ionisation (ESI)-MS/MS in positive ion mode with multiple reaction monitoring (MRM), optimising parameters such as voltage cone, capillary voltage, source and desolvation temperature, and desolvation and cone gas flow. The optimised method provides a rapid separation (less than 10 min) of the selected herbicides in the assayed matrices, and it was validated by the analysis of spiked blank matrix samples. Good linearity was obtained and the repeatability of the method was less than 20% for the lowest calibration point. The limits of detection ranged from 0.002 to 0.02 microg/L, and the limits of quantification from 0.005 to 0.05 microg/L, which were below the values specified by the European Union. Finally, the method was successfully applied to real environmental samples from Andalusia (southern Spain). Terbuthylazine, simazine, atrazine desisopropyl and desethyl terbuthylazine were the herbicides most frequently found in water samples.