RESUMO
We carried out a collaborative study in six laboratories to confirm the universality of the enhancing effect of co-existing reference pesticides on the GC-MS peak response to a target pesticide (malathion, procymidone, or flucythrinate). First, we confirmed the response enhancement of the target pesticides with increasing numbers of co-existing reference pesticides in solution. Then, using diluted green soybean matrix, we analyzed the target pesticides with two types of matrix-matched calibration, containing the target pesticides or 166 other pesticides. In both cases, the response-enhancing effect of co-existing pesticides was confirmed in all laboratories. The enhancement was reduced by addition of green soybean matrix to the sample and calibration solutions. Our results show that it is necessary to estimate the peak response-enhancing effect of co-existing pesticides in the calibration solution to obtain accurate results with GC-MS determination. The enhancing effect could be reduced by addition of food matrix to the sample and calibration solutions.
Assuntos
Análise de Alimentos/métodos , Resíduos de Praguicidas/análise , Praguicidas/análise , Calibragem , Cromatografia Gasosa-Espectrometria de MassasRESUMO
A validation study was carried out on a rapid method for the simultaneous determination of pesticide residues in vegetables and fruits by LC-MS/MS. Preparation of the test solution was performed by a solid-phase extraction technique with QuEChERS (STQ method). Pesticide residues were extracted with acetonitrile using a homogenizer, followed by salting-out and dehydration at the same time. The acetonitrile layer was purified with C18 and PSA mini-columns. The method was assessed for 130 pesticide residues in 14 kinds of vegetables and fruits at the concentration level of 0.01 µg/g according to the method validation guideline of the Ministry of Health, Labour and Welfare of Japan. As a result 75 to 120 pesticide residues were determined satisfactorily in the tested samples. Thus, this method could be useful for a rapid and simultaneous determination of multi-class pesticide residues in various vegetables and fruits.
Assuntos
Cromatografia Líquida/métodos , Análise de Alimentos/métodos , Contaminação de Alimentos/análise , Frutas/química , Resíduos de Praguicidas/análise , Espectrometria de Massas em Tandem/métodos , Verduras/química , Acetonitrilas , Órgãos Governamentais , Guias como Assunto , Japão , Resíduos de Praguicidas/isolamento & purificação , Extração em Fase Sólida/métodosRESUMO
A highly sensitive and simple method for the analysis of chlorothalonil was presented using a liquid chromatograph/mass spectrometer equipped with an atmospheric pressure photoionization (APPI) source. Chlorothalonil is one of the most extensively used fungicides. The major degraded product of chlorothalonil, 4-hydroxy-2,5,6-trichloroisonaphthonitrile (4OH-TPN), was also quantified with sensitivity similar to that of chlorothalonil. The method was applied to the determination of chlorothalonil in aqueous environment and food samples. The method detection limits (MDLs) of chlorothalonil for aqueous samples and cucumber were determined to be 0.18 and 3.2 ng g(-1), respectively. At several estuarial locations, chlorothalonil was detected with a maximum of 1.1 ng L(-1). On the other hand, 4OH-TPN was detected not from estuaries but from rivers with a maximum of 14 ng L(-1).
