Development and Validation of Gas Chromatography - Mass Spectrometry Method for Determination of Aldrin and Dieldrin in Serum

Abstract

Aim: Exposure to many banned pesticides continues all over the world and in our country due to the long half-lives of pesticides. Therefore, the purpose of the study was to obtain a rapid, simple, and convenient method for the simultaneous determination of aldrin and dieldrin. Material and Methods: Method improving and validation assessment are the most important elements for establishing reference techniques and reliable analysis results. In order to analyze analytes, validation of the analytical method is carried out by checking the parameters of specificity, recovery, precision, linearity, the limit of detection (LOD), and the limit of quantification (LOQ). Results: In our study, an easily applicable, so rapid, effective, and safe GC-MS method was created for the determination of aldrin and dieldrin in serum. In the developed method, 4,4'-Dichlorobenzophenone (4,4-DBP) was used as the internal standard. Aldrin and dieldrin were analyzed in serum in a very short time of 4 minutes. Linear correlation coefficients (R2 ≥ 0.99) of the linear calibration curves between a range of 1-250 ng/mL of analytes in serum were established. The limit of detection for aldrin and dieldrin were 0.28 and 0.29 ng/mL, respectively. More than 80% recovery of aldrin and dieldrin were obtained at high concentrations, and consistent relative standard deviation (RSD ˂ 6.03%) values were found for both pesticides. Conclusion: This new method can reliably and quickly be used in routine analysis. The study showed that exposure to aldrin and dieldrin can be detected and monitored in such a short time as four minutes.

Keywords

• Aldrin
• dieldrin
• serum
• validation
• GC-MS

Serumda Aldrin ve Dieldrin Tayini için Gaz Kromatografisi - Kütle Spektrometresi Yönteminin Geliştirilmesi ve Doğrulanması

Abstract

Amaç: Tüm dünyada ve ülkemizde yasaklanmış pestisitlere maruziyet, pestisitlerin uzun yarılanma ömürleri nedeniyle devam etmektedir. Bu nedenle bu çalışmanın amacı, serumda aldrin ve dieldrin maruziyetinin eş zamanlı tayini için hızlı, basit ve kullanışlı bir yöntem elde etmektir. Gereç ve Yöntemler: Metot geliştirme ve doğrulama değerlendirmeleri; referans teknikleri oluşturmak ve güvenilir analiz sonuçları elde etmek için en önemli unsurlardır. Analitleri analiz etmek için, analitik yöntemin doğrulanması; özgüllük, geri kazanım, kesinlik, doğrusallık, saptama sınırı ve ölçüm sınırı parametrelerin kontrol edilmesiyle gerçekleştirilir. Bulgular: Çalışmamızda; serumda aldrin ve dieldrin tayini için kolaylıkla uygulanabilir, çok hızlı, etkili ve güvenli bir GC-MS yöntemi oluşturuldu. Geliştirilen yöntemde internal standart olarak 4,4'-Diklorobenzofenon (4,4-DBP) kullanıldı. Aldrin ve dieldrin, serumda 4 dakika gibi çok kısa bir sürede analiz edildi. Serumda 1-250 ng / mL analit aralığında doğrusal kalibrasyon eğrilerinin doğrusal korelasyon katsayıları (R2 ≥ 0,99) saptandı. Aldrin ve dieldrin için tespit limiti sırasıyla 0,28 ve 0,29 ng / mL idi. Yüksek konsantrasyonlarda aldrin ve dieldrinin % 80'den fazla geri kazanımı elde edildi ve her iki pestisit için tutarlı bağıl standart sapma (RSD ˂ % 6,03) değerleri bulundu. Sonuç: Bu yeni yöntem; rutin analizlerde güvenilir ve hızlı bir şekilde kullanılabilir. Çalışma, aldrin ve dieldrin maruziyetinin dört dakika gibi kısa bir sürede tespit edilebildiğini ve izlenebildiğini gösterdi.

Keywords

• Aldrin
• dieldrin
• serum
• doğrulama
• GC-MS

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