Estimation of the validation parameters for a fast analysis of herbicide residues by LC-MS/MS.
Due to strict regulatory requirements for pesticide residue analysis, only the results of residue analysis with acceptable quality should be reported. As a consequence proper validation of the measurement method is required. In this context, accuracy, precision, specificity, limit of determination (LOQ), matrix effect, linearity, uncertainty calculation and ruggedness become increasingly important. This paper reports a description of the validation parameters of a fast method for the determination of five phenoxy acid herbicides (2,4-D, MCPA, MCPP, haloxyfop and fluazifop) in food crops. The recoveries were performed in the concentration range from 0.05 to 0.5 mg kg⁻¹ for apples, pears, carrots and celeriac with five replicates at each level. The mean recoveries ranged from 70% to 95% for all crops. The precision of the method expressed as a relative standard deviation (RSD%) was found to be in the range 3-14%. For all herbicides, the linearity response of the detector was tested by correlation coefficients (r² > 0.99) in the concentration range from 0.05 to 0.5 mg kg⁻¹. The LOQ was determined as the lowest spiked level meeting the requirement of accuracy (70-120%) and precision (RSD% < 20% according to European Union guidelines. The uncertainty and robustness were calculated. On the basis of the results, the method can be considered fast, simple and robust and is suitable to be applied to the analysis of studied herbicides in routine testing laboratories.
a Department of Environmental and Primary Prevention, Pesticide Unit , National Institute of Health , Rome , Italy.
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Santilio
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Girolimetti
D Attard
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Barbini
D015084:2,4-Dichlorophenoxyacetic Acid / Q000032:analysis / Q000737:chemistry; D008456:2-Methyl-4-chlorophenoxyacetic Acid / Q000031:analogs & derivatives / Q000032:analysis / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid; D018556:Crops, Agricultural / Q000737:chemistry*; D004095:Dihydropyridines / Q000032:analysis / Q000737:chemistry; D005062:European Union; D005506:Food Contamination; D005513:Food Inspection / Q000379:methods*; D005638:Fruit / Q000737:chemistry; D006540:Herbicides / Q000032:analysis* / Q000737:chemistry; D007558:Italy; D057230:Limit of Detection; D008956:Models, Chemical; D010573:Pesticide Residues / Q000032:analysis* / Q000737:chemistry; D010642:Phenoxyacetates / Q000032:analysis* / Q000737:chemistry; D011725:Pyridines / Q000032:analysis / Q000737:chemistry; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry; D014675:Vegetables / Q000737:chemistry
D004095:Dihydropyridines; D006540:Herbicides; D010573:Pesticide Residues; D010642:Phenoxyacetates; D011725:Pyridines; C054176:haloxyfop; D015084:2,4-Dichlorophenoxyacetic Acid; C008340:mecoprop; C050582:fluazifop; D008456:2-Methyl-4-chlorophenoxyacetic Acid
LC-MS/MS; pesticide residue; phenoxy acid herbicides; validation