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| Content Provider | World Health Organization (WHO)-Global Index Medicus |
|---|---|
| Author | Belmonte Valles, N. Mezcua, M. Fernández-Alba, A. R. Retamal, M. |
| Description | Country affiliation: Spain Author Affiliation: Belmonte Valles N ( European Union Reference Laboratory for Pesticide Residues in Fruits and Vegetables, Pesticide Residue Research Group, University of Almería, 04120 Almería, Spain. nbelmonte@ual.es) |
| Abstract | Multiresidue methods (MRMs) for pesticides residues determination in fruit and vegetables, based on GC-MS, are mainly performed in electron impact ionization mode. However an important group of them provide much better response working in negative chemical ionization mode due to the elimination of a high percentage of background signal. Considering that a selective and sensitive method has been developed for the determination of multiclass pesticide residues in different commodities by GC-MS with a triple stage quadrupole analyzer (GC-TSQ-MS); the pesticide signal has been optimized in MS-MS whilst working in negative chemical ionization mode using methane as the reagent gas. The proposed method was fully validated for 53 compounds in tomato, apple and orange matrices. The obtained limits of determination were lower than 0.1 µg/kg for more than 50% of the pesticides studied, and lower than 1 µg/kg for all pesticides studied, except for cypermethrin, boscalid, bifenthrin and deltamethrin. Linearity was studied in the 0.5-50 µg/kg range and a linear response was obtained for all pesticides in all matrices. Recoveries were evaluated at two different levels (1 and 50 µg/kg) and recoveries were ranged between 70 and 120% in tomato, apple and orange, except in the cases of chlorfenapyr, ofurace, chlozolinate, chlorothalonil, tolylfluanid and dichlofluanid with recovery values close to 60% at 1 µg/kg fortification levels. Repetitivity was evaluated and the relative standard deviation (RSD%) was lower than 10% in all cases. The developed method was employed in the analysis of real samples intended for baby food and the obtained results showed that 50% of the samples were positive for different pesticide residues. The concentration range detected was between 5 and 100 µg/kg. The positive detection of OCs was particularly noticeable; these included chlorothalonil, fenhexamide, clorpyrifos and lambda cyhalothrin, which are very persistent and toxic with low acute reference dose. Endosulfan sulfate, which is not approved, was detected at a low concentration. |
| ISSN | 00219673 |
| Volume Number | 1264 |
| e-ISSN | 18733778 |
| Journal | Journal of Chromatography A |
| Language | English |
| Publisher | Elsevier |
| Publisher Date | 2012-11-16 |
| Publisher Place | Netherlands |
| Access Restriction | One Nation One Subscription (ONOS) |
| Subject Keyword | Fruit Chemistry Gas Chromatography-mass Spectrometry Methods Pesticides Analysis Sensitivity And Specificity Tandem Mass Spectrometry Journal Article Research Support, Non-u.s. Gov't Discipline Analytical Chemistry |
| Content Type | Text |
| Resource Type | Article |
| Subject | Organic Chemistry Medicine Analytical Chemistry Biochemistry |
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