Determination of the residue levels of some insecticide, commonly used in apple orchards in Isparta province, by HPLe

Abstract

In this study, determination of some insecticides (chlorpyrifos, diazinon and diclorvos) and degredation products of chlorpyrifos (chlorpyrifos-oxon and 3,5,6-triklor-2-pyridinol) by HPLC was performed. Residue levels of chlorpyrifos and diazinon in apple samples, obtained from the orchards in Isparta province during harvest time, were also determined. With respect to their apple production amounts, 2-5 samples were taken from each district and a total of 35 samples were collected. Apple samples were immediately taken to the laboratory and kept at - 18°C until analysis. The mobile phase was consisted of 60 % asetonitrile and 50 mM phosphoric acide. pH of the mobile phase was adjusted to 3,5 with 0,5 M NaOH. Column temperature was
30°C and flow rate was 1 mL/minute. Luna C8 column (150X4.6mm. I.D) was used. Spectrums of the peaks of the standarts and the samples were compared by using DAD dedector. A randomly selected representative apple sample was homojenized and insecticides were obtained by ethyl acetate extraction. Organic phase was evaporated and the residue was diluted with 2 mI mobile phase and injected for HPLC analysis. Elution order was dichlorvos, 3,5,6-triklor-2-pyridinol, chlorpyrifos-oxon, diazinon and chlorpyrifos. Chlorpyrifos residue was found on 22.86 % of the apple samples while diazinon residue was determined on 71.42 % of the samples.

Keywords

• Residue
• apple
• chlorpyrifos-oxon
• 3,5,6- triklor-2-pyridinol (TCP)
• dichlorvos

Isparta Ilindeki elma bahcelerinde yayqm kullarulan chlorpyrifos ve diazinon'un kahnti duzeylerinin HPLC He belirlenmesi

Abstract

Bu cahsmada bazi insektisit aktif maddelerinin (chlorpyrifos, diazinon ve dichlorvos) ve chlorpyrifos'un parcalanma urunlerinin (chlorpyrifos-oxon ve TCP) HPLC ile kromatografik aynmlan yapilrrustir. Chlorpyrifos ve diazinon'un Isparta'da hasat sirasmda ahnan elma orneklerlndeki kalmti dtizeyleri HPLC ile belirlenmistir. Bu amacla Isparta ve ilcelerinden hasat strasmda elma uretim miktanna bagh olarak her ilcenin 2 ile 5 farkh bahcesinden olmak tizere toplam 35 elma bahcesinden elma ornekleri almrrustir. Elma ornekleri dogrudan laboratuvara getirilerek analize kadar derin dondurucuda -18°C'de saklanrmstir. Analizlerde kullarulan mobil fazda % 60 iv/v) asetonitril bulunmaktadir. Bu mobil faz, 50 mM fosforik asit icerecek sekilde hazirlanrmstir. Mobil fazm pH'sl 0.5 M NaOH eklenerek 3.5'e ayarlanrmstir. Kolon sicakhgr 30°C, akis hizi 1 mlz/dakikadir. Kolon olarak luna C8 (ISO X 4.6 mm. I.D) kullamlmistir. Bu cahsmada DAD dedektor kullanilarak standartlarla orneklerdeki piklerin spektrumlanrun karsilastmlrnasi saglanml~tlr. insektisitlerin kalmtilanru belirlemek icin toplanan elma orneklerinden bir tanesi tesadufen secilerek homojenize edilmis ve bu homojen kansimdan insektisitler etil asetat ekstraksiyonu He ahnrruslardir. Organik faz buharlastmlrms ve kahnti 2 ml mobil fazla seyre1tilip HPLC'ye uyqulanrrustir. Cahsmalar 3 tekerrurlu olarak yurutulmustur. Elusyon srrasi dichlorvos, 3, 5, 6-triklor-2-pyridinol, chlorpyrifos-oxon, diazinon ve chlorpyrifos seklindedir. Analiz edilen elma omeklerinin % 22.86'mda chlorpyrifos, % 71'inde de diazinon kalmtisi behrlenmistir.

Keywords

• Kahnn
• elma
• chlorpyrifos-oxon
• 3,5,6- triklor-2-pyridinol (TCP)
• dichlorvos