title: Determination of pesticide residues in samples of green minor crops by gas chromatography and ultra performance liquid chromatography coupled to tandem quadrupole mass spectrometry.
abstract: A method was developed for pesticide analysis in samples of high chlorophyll content belonging to the group of minor crops. A new type of sorbent, known as ChloroFiltr, was employed for dispersive-solid phase extraction cleanup (dispersive-SPE) to reduce the unwanted matrix background prior to concurrent analysis by gas chromatography and ultra-performance liquid chromatography coupled to tandem quadrupole mass spectrometry (GC-MS/MS and UPLC-MS/MS). Validation experiments were carried out on green, unripe plants of lupin, white mustard and sorghum. The overall recoveries at the three spiking levels of 0.01, 0.05 and 0.5 mg kg(-1) fell in the range between 68 and 120% (98% on average) and 72-104% (93% on average) with relative standard deviation (RSD) values between 2 and 19% (7% on average) and 3-16% (6% on average) by GC-MS/MS and UPLC-MS/MS technique, respectively. Because of strong enhancement or suppression matrix effects (absolute values >20%) which were exhibited by about 80% of the pesticide and matrix combinations, acceptably accurate quantification was achieved by using matrix-matched standards. Up to now, the proposed method has been successfully used to study the dissipation patterns of pesticides after application on lupin, white mustard, soya bean, sunflower and field bean in experimental plot trials conducted in Poland.
authors.affiliation: Institute of Plant Protection-National Research Institute, Władysława Węgorka 20, 60-318 Poznań, Poland. Electronic address: s_walorczyk@tlen.pl.
authors.forename: Stanisław
authors.initials: S
authors.lastname: Walorczyk
authors.affiliation: Institute of Plant Protection-National Research Institute, Władysława Węgorka 20, 60-318 Poznań, Poland.
authors.forename: Dariusz
authors.initials: D
authors.lastname: Drożdżyński
authors.affiliation: Institute of Plant Protection-National Research Institute, Władysława Węgorka 20, 60-318 Poznań, Poland.
authors.forename: Roman
authors.initials: R
authors.lastname: Kierzek
mesh_terms: D002849:Chromatography, Gas; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D018556:Crops, Agricultural / Q000737:chemistry*; D005506:Food Contamination / Q000032:analysis; D006540:Herbicides / Q000032:analysis*; D057230:Limit of Detection; D031297:Lupinus / Q000737:chemistry; D009149:Mustard Plant / Q000737:chemistry; D010755:Organophosphates / Q000032:analysis; D010573:Pesticide Residues / Q000032:analysis*; D012015:Reference Standards; D012839:Simazine / Q000032:analysis; D052616:Solid Phase Extraction / Q000295:instrumentation / Q000379:methods*; D045868:Sorghum / Q000737:chemistry; D053719:Tandem Mass Spectrometry
chemical_list: D006540:Herbicides; D010755:Organophosphates; D010573:Pesticide Residues; D012839:Simazine; C005445:triphenyl phosphate
keywords: Chromatography; Dispersive solid phase extraction; Minor crops; Pesticide residue analysis; Tandem mass spectrometry