title: Fast determination of phenoxy acid herbicides in carrots and apples using liquid chromatography coupled triple quadrupole mass spectrometry.
abstract: A fast, simple and inexpensive method has been developed for the analysis of phenoxy acid herbicides: 2,4-dichlorophenoxyacetic acid (2,4-D), 4-chloro-2-methylphenoxyacetic acid (MCPA), 2-(4-chloro-o-tolyloxy)propionic acid (MCPP), 2-(4-aryloxyphenoxy)propionic acid (Fluazifop) and 2-(4-aryloxyphenoxy)propionic acid (Haloxyfop) in carrots and apples by liquid chromatography coupled to triple quadrupole mass spectrometry (LC/MS/MS). The compounds were analyzed by QuEChERS (quick, easy, cheap, effective, rugged, safe) methodology without cleanup. The recoveries were performed at two spiked levels (0.05 and 0.5 mg/kg) for both matrices with six replicates for each level. The mean recoveries ranged from 70-92% for both apples and carrots. The precision of the method expressed as relative standard deviation (RSD%) was found to be in the range 3-15%. For all compounds, good linearity (r(2) > 0.99) was obtained over the range of concentration from 0.05 micro g/mL to 0.5 micro g/mL, corresponding to the pesticide concentrations of 0.05 mg/kg and 0.5 mg/kg, respectively. The determination limits (LOQs) ranged from 0.01 ng/mL to 1.3 ng/mL in solvent, whereas, the LOQs calculated in matrix ranged from 0.05 ng/g to 21.0 ng/g for apples and from 0.06 ng/g to 10.2 ng/g for carrots. The developed methodology combines the advantages of both QuEChERS and LC/MS/MS producing a very rapid, sensitive and cheap method useful for the routine analytical laboratories.
authors.affiliation: Department of Environmental and Primary Prevention, Pesticide Unit, National Institute of Health, Rome, Italy. angela.santilio@iss.it
authors.forename: Angela
authors.initials: A
authors.lastname: Santilio
authors.forename: Patrizia
authors.initials: P
authors.lastname: Stefanelli
authors.forename: Roberto
authors.initials: R
authors.lastname: Dommarco
mesh_terms: D015084:2,4-Dichlorophenoxyacetic Acid / Q000032:analysis*; D002853:Chromatography, Liquid; D018552:Daucus carota / Q000737:chemistry*; D005504:Food Analysis / Q000379:methods*; D006540:Herbicides / Q000032:analysis*; D027845:Malus / Q000737:chemistry*; D013058:Mass Spectrometry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012997:Solvents / Q000737:chemistry; D013997:Time Factors
chemical_list: D006540:Herbicides; D012997:Solvents; D015084:2,4-Dichlorophenoxyacetic Acid