Hollow fiber liquid-phase microextraction combined with supercritical fluid chromatography coupled to mass spectrometry for multiclass emerging contaminant quantification in water samples.

The hollow fiber liquid-phase microextraction allows highly selective concentration of organic compounds that are at trace levels. The determination of those analytes through the supercritical fluid chromatography usage is associated with many analytical benefits, which are significantly increased when it is coupled to a mass spectrometry detector, thus providing an extremely sensitive analytical technique with minimal consumption of organic solvents. On account of this, a hollow fiber liquid-phase microextraction technique in two-phase mode combined with supercritical fluid chromatography coupled to mass spectrometry was developed for quantifying 19 multiclass emerging contaminants in water samples in a total chromatographic time of 5.5 min. The analytical method used 40 µL of 1-octanol placed in the porous-walled polypropylene fiber as the acceptor phase, and 1 L of water sample was the donor phase. After extraction and quantification techniques were optimized in detail, a good determination coefficient (r2 > 0.9905) in the range of 0.1 to 100 µg L-1, for most of the analytes, and an enrichment factor in the range of 7 to 28,985 were obtained. The recovery percentage (%R) and intraday precision (%RSD) were in the range of 80.80-123.40%, and from 0.48 to 16.89%, respectively. Limit of detection and quantification ranged from 1.90 to 35.66 ng L-1, and from 3.41 to 62.11 ng L-1, respectively. Finally, the developed method was successfully used for the determination of the 19 multiclass emerging contaminants in superficial and wastewater samples.

Validation and assessment of matrix effect and uncertainty of a gas chromatography coupled to mass spectrometry method for pesticides in papaya and avocado samples.

In this paper a method of using the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) extraction and gas chromatography coupled to mass spectrometry detection (GC-MS) was developed for the analysis of five frequently applied pesticides in papaya and avocado. The selected pesticides, ametryn, atrazine, carbaryl, carbofuran, and methyl parathion, represent the most commonly used classes (carbamates, organophosphorous, and triazines). Optimum separation achieved the analysis of all pesticides in < 6.5 minutes. Validation using papaya and avocado samples established the proposed method as linear, accurate, and precise. In this sense, the correlation coefficients were > 0.99. The limits of detection (LOD) and quantification (LOQ) in papaya ranged from 0.03 mg/kg to 0.35 mg/kg and from 0.06 mg/kg to 0.75 mg/kg, respectively. Meanwhile for avocado, LOD values varied from 0.14 mg/kg to 0.28 mg/kg and LOQ values ranged from 0.22 mg/kg to 0.40 mg/kg. Recoveries obtained for each pesticide in both matrices ranged between 60.6% and 104.3%. The expanded uncertainty of the method was < 26% for all the pesticides in both fruits. Finally, the method was applied to other fruits.