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Baglio D, Kotzias D, Larsen BR: Atmospheric pressure ionisation multiple mass spectrometric analysis of pesticides. J Chromatogr A. 1999 Aug 27;854(1-2):207-20.
Liquid chromatography-multiple mass spectrometry (LC-MS") has been investigated for analysis of polar pesticides in water using an ion-trap instrument and atmospheric pressure ionisation. Carbamate, triazine and phenylurea pesticides were best ionised as positive ions with atmospheric pressure chemical ionisation, while phenoxy acid herbicides, nitrophenols and bentazone yielded stronger signals as negative ions with pneumatically assisted electrospray. The ion fragmentation processes and pathways were studied in detail by MS, MS2, MS3 and MS4. All compounds were observed as their protonised or deprotonised molecular ions by MS and in the successive fragmentation by MS" the structures of typical (diagnostic) product ions were tentatively identified for each class of pesticide. Phenylureas yield an ion at m/z 72 by MS2, corresponding to O=C=N+(CH3) 2. Carbamates produce [M+H-CONCH3]+ fragments by MS2 from neutral loss of methylisocyanate. Characteristic fragmentation pathways for triazine pesticides are [M+H]+--> m/z 174--> m/z 146--> m/z 110 and [M+H]+--> m/z 174--> m/z 132--> m/z 104 by MS-MS2-MS3-MS4 from cleavage of lateral chains in the triazine ring followed by ring opening. Phenoxy acid herbicides produce peculiar fragments by MS2 from loss of the acidic group possibly as the corresponding lactone. Nitrophenols are subject to loss of both *OH radical and NO groups thereby forming the correspondent phenols and quinones. The performance of the method with respect to quantitation compares favourably with traditional methods. With the ion-trap run in a time scheduled single ion monitoring mode, typical limits of detection (LODs) are in the low pg range and the repeatability standard deviations are between 3 and 15%. Assuming extraction of 1-l water samples and 1 ml final volumes the injection of 50-microl aliquots corresponds to LODs well below the requirement for the European Union water directive (EC/80/778). |
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