Solid-phase microextraction liquid chromatography/tandem mass spectrometry to determine postharvest fungicides in fruits.
A method to determine five postharvest fungicides (dichloran, flutriafol, o-phenylphenol, prochloraz, tolclofos methyl) in fruits (cherries, lemons, oranges, peaches) has been developed using solid-phase microextraction (SPME) coupled to liquid chromatography (LC) with photodiode array (DAD), mass spectrometry (MS), or tandem mass spectrometry (MS/MS) with ion trap detection. Extraction involved sample homogenization with an acetone/water solution (5:1), filtration, and acetone evaporation prior to fiber extraction. The pesticides were isolated with a fused-silica fiber coated with 50-microm Carbowax/template resin. The effects of pH, ion strength, sample volume, and extraction time were investigated, and their impact on the SPME-LC/MS was studied. Dynamic and static modes of desorption were compared and the variables affecting desorption processes in SPME-LC optimized. Static desorption provided the best recoveries and peak shapes. Recoveries at the limit of quantification (LOQ) levels were between 10% for prochloraz and 60% for o-phenylphenol, with relative standard deviations from 13.6% for prochloraz to 3.1% for o-phenylphenol. The versatility of the method was also exhibited by its excellent linearity in the concentration intervals between 0.0005 and 5 mg kg(-1) for dichloran and 0.01-10 mg kg(-1) for tolclofos methyl and prochloraz. LOQs ranged from 0.25 to 1 microg g(-1) using DAD, from 0.002 to 0.01 microg g(-1) using LC/MS, and from 0.0005 to 0.01 to microg g(-1) using LC/MS/MS. LOQs obtained in the present study using LC/MS and LC/MS/MS are lower than maximum residue limits established for all the fungicides in any matrix studied. The method enables to determine polar pesticides at low-microgram per gram levels in fruits.
Laboratorio de Bromatologia, Facultat de Farmàcia, Universitat de València, Av. Vicent Andres Estelles s/n, 46100 Burjassot, València, Spain.
Cristina
C
Blasco
Guillermina
G
Font
Jordi
J
Mañes
Yolanda
Y
Picó
D002138:Calibration; D002853:Chromatography, Liquid; D005638:Fruit / Q000737:chemistry*; D005659:Fungicides, Industrial / Q000032:analysis*; D007202:Indicators and Reagents; D013058:Mass Spectrometry; D010573:Pesticide Residues / Q000032:analysis*; D012015:Reference Standards; D013056:Spectrophotometry, Ultraviolet
D005659:Fungicides, Industrial; D007202:Indicators and Reagents; D010573:Pesticide Residues