Katı Faz Mikroekstraksiyon-Gaz Kromatografisi Metodu ile Malonaldehit ve Hegzanal Tayini

Year 2023, , 510 - 523, 31.08.2023

Tahir Yücel , İsa Cavidoğlu

https://doi.org/10.53433/yyufbed.1215854

Cited By: 1

Abstract

Bu çalışmada, ayçiçeği yağında Katı faz mikroekstraksiyon (SPME) tekniği ile ekstraksiyon süresi (20, 30 ve 40 dakika) ve sıcaklığının (40, 50 ve 60 °C) hegzanal (HE) ve malonaldehit (MA) ekstraksiyonu üzerindeki etkileri araştırılmıştır. HE ve MA’nın kantitatif analizi için İç Standart (IS) olarak 5-Metil 2-hegzanon (500 ppb) kullanılmıştır. HE ve MA’ın IS ile aralarındaki ilişkinin düzeyini belirlemek için ayçiçeği yağına farklı oranlarda HE ve MA (5 ppb, 10 ppb, 50 ppb, 100 ppb, 0.5 ppm, 1 ppm, 5 ppm ve 10 ppm) ve IS (500 ppb) eklenmiştir. Değişkenler arasındaki ilişki, regresyon denklemi (y = mx + n) ve değişkenler (x = HE veya MA’nın derişimi/IS’nin derişimi; y = HE veya MA’nın alanı/IS’nin alanı) arasındaki regresyon katsayılarının (R2) belirlenmesi ile değerlendirilmiştir. MA polar ve reaktif olduğu için MA ile IS arasındaki R2 değeri (0.015 ˂ R2 ˂ 0.606) oldukça düşük bulunmuş ve MA’nın nicel analizi için bu yöntemin uygun olmadığı tespit edilmiştir. HE ile IS arasındaki R2 göz önüne alındığında HE’nin analizi için en uygun ekstraksiyon sıcaklığı ve süresinin 60 °C ve 20 dakika olduğu tespit edilmiştir. Sonuç olarak, hızlı ve çözücü gerektirmeyen bir yöntem olan SPME’nin, HE’in ayçiçeği yağında tespitinde kullanılabilirken, MA'nın tespit edilebilmesi için SPME yöntemi ile saptanabileceği türevlerine dönüştürülmesi gerektiği saptanmıştır.

Keywords

Ekstraksiyon, Hegzanal, Katı faz mikroekstraksiyon, Malonaldehit

Quantification of Malonaldehyde and Hexanal by Solid Phase Microextraction-Gas Chromatography Method

Abstract

In the present study, the effects of extraction time (20, 30 and 40 minutes) and temperature (40, 50 and 60 °C) on the extraction of hexanal (HE) and malonaldehyde (MA) in sunflower oil with Solid Phase Micro-extraction technique (SPME) were investigated. For the quantification of HE and MA, 5-Methyl 2 hexanone (500 ppb) was added as Internal Standard (IS). In order to determine the level of relationship between HE and MA with IS, different ratios of HE and MA (5 ppb, 10 ppb, 50 ppb, 100 ppb, 0.5 ppm, 1 ppm, 5 ppm and 10 ppm) and IS (500 ppb) were added to sunflower oil. The relationship between the variables was evaluated by the regression equation (y = mx + n) and the determination of the correlation coefficients (R2) between the variables (x=HE or MA concentration/IS concentration; y = HE or MA area/IS area). Because of the high reactivity and polarity of MA, the correlation between MA and IS was not sufficient (0.015 ˂ R2 ˂ 0.606) to explain the linearity between MA and IS in the sunflower oil. Considering the R2 values between HE and IS, it was determined that the optimum extraction temperature and time for the analysis of HE was 60 °C and 20 minutes. As a result, SPME which is a fast and solvent-free technique, can be used in the determination of HE in sunflower oil, while for determination of MA, it must be derivatized for analysis by SPME.

Keywords

Extraction, Hexanal, Malonaldehyde, Solid phase microextraction

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