SÜTLÜ ÇİKOLATA İÇİN KATI FAZ MİKROEKSTRAKSIYON YÖNTEMİNİN OPTİMİZASYONU

Abstract

Bu çalışmada, isomalt içeren sütlü çikolatalarda 2,3,5,6 tetra metal pirazin tayini için HS-SPME ekstraksiyonunun optimizasyonunda merkezi kompozit tasarım uygulanmıştır. SPME verimliliği etkileyen dengeleme süresi, ekstraksiyon süresi ve ekstraksiyon sıcaklığı için optimum koşullar olarak sırasıyla 10 dk, 40 dk ve 57 °C olarak belirlenmiştir. Çalışmada StableFlex fibere uygulanmış 100 µm polidimetilsiloksan, 65 µm polidimetilsiloksan/divinilbenzen, 75 µm karboksen/polidimetilsiloksan ve 50/30 µm divinilbenzen/karboksen/polidimetilsiloksan kaplamalar SPME fiberler olarak incelenmiştir. Çikolata örneklerinin hazırlama koşulları ayrıca tepe boşluğunun kaplama bileşimi üzerindeki etkileri ölçülerek de değerlendirilmiştir. Özellikle örneklerin kuru koşullarda 60 °C’de 30 dk örnek ekstraksiyonunda 50/30 µm divinilbenzen/karboksen/polidimetilsiloksan kaplı SPME fiber en yüksek ekstraksiyon verimliliğini sağlamıştır.

Keywords

• çikolata
• isomalt
• merkezi kompozit tasarım
• optimizasyon
• SPME

OPTIMIZATION OF SOLID-PHASE MICROEXTRACTION CONDITIONS OF MILK CHOCOLATE

Abstract

In the current study, the Central Composite Design was applied to optimize HS-SPME extraction in order to detect 2,3,5,6 tetramethyl pyrazine in isomalt contaning milk chocolate. The optimal conditions for the three experimental responses influencing SPME efficiency were 10 min, 40 min and 57 °C for equilibration time, extraction time and extraction temperature, respectively. SPME fibers coated with 100 m polydimethylsiloxane coating, 65 µm polydimethylsiloxane/divinylbenzene coating, 75 µm carboxen/polydimethylsiloxane coating and 50/30 µm divinylbenzene/carboxen/polydimethylsiloxane on a StableFlex fiber were investigated. The preparation conditions of the chocolate samples were also evaluated by measuring their effects on the coating composition of the head space. The SPME fiber coated with 50/30 µm divinylbenzene/carboxen-polydimethylsiloxane provided the highest extraction efficiency, especially when the samples were extracted at 60 °C for 30 min under dry conditions. Eighty-one blends were extracted and experimentally detected most of which have been formerly stated as odor-active components.

Keywords

• Chocolate
• isomalt
• central composite design
• optimization
• SPME

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