Publication: Bal örneklerinde Indoxacarb kalıntısının ve bozunma ürünlerinin tayini için yöntem geliştirilmesi
Abstract
BAL ÖRNEKLERİNDE INDOXACARB KALINTISININ VE BOZUNMA ÜRÜNLERİNİN TAYİNİ İÇİN YÖNTEM GELİŞTİRİLMESİ Pestisit kalıntısının izlenmesi, yiyecekler içindeki pestisitlere insanların maruziyetinin doğru olarak değerlendirilmesi açısından oldukça önemlidir. Bu nedenle gıda maddelerinde kalıntı düzeylerinin belirlenmesi ve kullanılan analitik yöntemlerin düşük düzeyde kalıntı ölçümü yapabilmesi önem kazanmaktadır. Balda kalıntı düzeyinde bulunan pestisitlerin izin verilen düzeyde olup olmadığının belirlenmesi gerekmektedir. Son yıllarda çeşitli çalışmalar yapılmış olmasına karşın ülkemizde ballarda pestisit kalıntı analizleriyle ilgili sınırlı sayıda çalışma mevcuttur. Çalışmamızda bal örneklerinde Indoxacarb ((S)-metil-7-kloro-2,5-dihidro-2- [(metoksikarbonil) [4-trifluorometoksi) fenil] amino] karbonil] indeno [1,2-e] [1,3,4] oksadiazin- 4a (3H)- karboksilat) kalıntısının tayini için analitik metod geliştirilmiştir. Indoxacarb içeren bal örnekleri diklormetan ile ekstrakte edildikten sonra, Indoxacarb’ ın ve ona ait bozunma ürününün tayini GC- MS ile yapılmıştır. Geliştirilen metodun tespit sınırı 0.03 mg. kg–1 ve tayin sınırı ise 0.11 mg. kg-1’dir. Ortalama geri kazanım % 78.7±5.5 (1.00 mg. kg-1) olarak hesaplanmıştır( % 95 güven aralığı, n= 6). Indoxacarb ile kirlenmiş bal içinde beşinci ayda tespit edilen bozunma ürünü 4-(trifluorometoksi) fenilizosiyanat Indoxacarb’ ın literatürde belirtilen bozunma ürünlerinden farklı bir bozunma ürünü oarak gözlenmiştir.
DEVELOPMENT OF AN ANALYSIS METHOD FOR INDOXACARB RESIDUES AND ITS DEGRADATION PRODUCTS IN HONEY SAMPLES Pesticide residue monitoring in foods is important from the viewpoint of evaluation of pesticide exposure of humans. Therefore, the determination of the residue levels in foods and, the analytical methods used for the trace level mesurements of the pesticide residues have gained more importance. It is necessary to determine if the pesticide residues in honey are in acceptable limits or not. Despite overseas various studies were done in recent years, there is limited research on pesticide analysis in honey in Turkey. An analytical method was developed to determine the residues of Indoxacarb ((S)-methyl 7-chloro-2,5- dihydro-2- [[(methoxycarbonyl) [4- (trifluoromethoxy) phenyl] amino]carbonyl] indeno [1,2-e] [1,3,4] oxadiazine- 4a (3H)-carboxylate) and degradation product 4- (Trifluoromethoxy) phenyl isocyanate in honey samples. Honey samples were extracted by dichlormetane. The determination of Indoxacarb and 4-(Trifluoromethoxy) phenyl isocyanate was performed by GC- MS. Limit of detection and quantification for the method were 0.03 mg. kg–1, 0.11 mg.kg-1 respectively. The average recoveryof Indoxacarb was calculated as 78.7% ± 5.5 (1.00 mg. kg-1) (95% confidence levels, n= 6). 4-(Trifluoromethoxy) phenyl isocyanate that has been determined in the Indoxacarb spiked honey at fifth month is a degradation product of Indoxacarb which is different from what was found in literature.
DEVELOPMENT OF AN ANALYSIS METHOD FOR INDOXACARB RESIDUES AND ITS DEGRADATION PRODUCTS IN HONEY SAMPLES Pesticide residue monitoring in foods is important from the viewpoint of evaluation of pesticide exposure of humans. Therefore, the determination of the residue levels in foods and, the analytical methods used for the trace level mesurements of the pesticide residues have gained more importance. It is necessary to determine if the pesticide residues in honey are in acceptable limits or not. Despite overseas various studies were done in recent years, there is limited research on pesticide analysis in honey in Turkey. An analytical method was developed to determine the residues of Indoxacarb ((S)-methyl 7-chloro-2,5- dihydro-2- [[(methoxycarbonyl) [4- (trifluoromethoxy) phenyl] amino]carbonyl] indeno [1,2-e] [1,3,4] oxadiazine- 4a (3H)-carboxylate) and degradation product 4- (Trifluoromethoxy) phenyl isocyanate in honey samples. Honey samples were extracted by dichlormetane. The determination of Indoxacarb and 4-(Trifluoromethoxy) phenyl isocyanate was performed by GC- MS. Limit of detection and quantification for the method were 0.03 mg. kg–1, 0.11 mg.kg-1 respectively. The average recoveryof Indoxacarb was calculated as 78.7% ± 5.5 (1.00 mg. kg-1) (95% confidence levels, n= 6). 4-(Trifluoromethoxy) phenyl isocyanate that has been determined in the Indoxacarb spiked honey at fifth month is a degradation product of Indoxacarb which is different from what was found in literature.