Optimisation of pressurised liquid extraction by experimental design for quantification of pesticides and alkyl phenols in sludge, suspended materials and atmospheric fallout by liquid chromatography-tandem mass spectrometry.
The study proposes an analytical method to quantify 10 alkylphenols and 12 pesticides at ultra-trace levels by liquid chromatography in reverse mode coupled to positive electrospray ionisation-tandem mass spectrometry. The extraction procedure from environmental solids was optimised by pressurised liquid extraction using acetonitrile:isopropanol (1:1, v/v). The influence of several extraction experimental factors, temperature, pressure, duration and number of cycles, related to the PLE was investigated by an original and efficient chemometric approach. The optimised extraction method (80 degrees C, 40 bar, 10 min, 1 cycle) exhibited recoveries between 67 and 127% with RSD mostly under 13%. The whole method was applied to real samples: sludge, suspended materials, atmospheric fallouts and roof deposit. Pollutant levels were between 1 microg kg(-1) and 5.9 mg kg(-1).
Service Central d'Analyse du CNRS - USR59, Echangeur de Solaize Chemin du Canal, BP 22, Solaize, France.
Jean-Baptiste
JB
Baugros
Cécile
C
Cren-Olivé
Barbara
B
Giroud
Jean-Yves
JY
Gauvrit
Pierre
P
Lantéri
Marie-Florence
MF
Grenier-Loustalot
D005591:Chemical Fractionation / Q000379:methods*; D055598:Chemical Phenomena; D002853:Chromatography, Liquid; D004785:Environmental Pollutants / Q000737:chemistry; D010573:Pesticide Residues / Q000302:isolation & purification*; D010636:Phenols / Q000302:isolation & purification*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012722:Sewage / Q000737:chemistry*; D053719:Tandem Mass Spectrometry
D004785:Environmental Pollutants; D010573:Pesticide Residues; D010636:Phenols; D012722:Sewage