Dumansız tütünde (Maraş otu) nikotinin elektrosprey iyonizasyon sıvı kromatografisi-tandem kütle spektrometrisi ile kantitatif tayini

Öz

Dumansız tütünde (Maraş otu) nikotin tayini için sıvı kromatografi-elektrosprey iyonizasyon tandem kütle spektrometresi kullanılarak hassas, hızlı, düşük maliyetli ve basit bir tayin yöntemi geliştirildi. Geliştirilen yöntem ile Maraş otu ve küllü Maraş otundaki nikotin miktarı belirlendi ve doğrulandı. Kromatografik ayırma, bir Hypersil Gold kolonu ile (2.1 mmx200 mm, 1.9 um) 30°C'de %0.2 asetik asitli su-asetonitril hareketli fazında 0.3 mLdak-1 akış hızında gerçekleştirildi. Toplam analiz süresi 10 dakikadır. Tandem kütle spektrometrik tayin SRM modunda pozitif elektrosprey iyonizasyon kullanılarak yapıldı. Yöntem spesifik ve duyarlı olup, LOD 0.057 mgL-1 ve LOQ 0.191 mgL-1 olarak hesaplandı. Doğrusallık, nikotin için 1 ila 10 mgL-1 arasında değişmiştir (R2=0.999, n=6). Yöntem Maraş otu örneklerine başarıyla uygulandı.

Anahtar Kelimeler

• Nikotin
• dumansız tütün
• maraş otu
• sıvı kromatografi-kütle spektrometrisi
• elektrosprey iyonizasyon

Quantitative determination of nicotine in smokeless tobacco (Maras powder) by liquid chromatography-tandem mass spectrometry with electrospray ionization

Öz

A sensitive, fast, low-cost and simple determination method was developed for the determination of nicotine in smokeless tobacco (Maras powder) using liquid chromatography-electrospray ionization tandem mass spectrometry. With the developed method, the amount of nicotine in Maras powder and ashy Maras powder was determined and confirmed. Chromatographic separation was performed on a Hypersil Gold (2.1 mmx200 mm, 1.9 um) at 30 ◦C with a gradient of 0.2% acetic acid in water and acetonitrile at a flow rate of 0.3 mLmin-1; total run time was 10 min. Tandem mass spectrometric detection was used in positive electrospray ionization in SRM mode. The method was specific and sensitive; LOD was 0.057 mgL-1 and LOQ was 0.191 mgL-1; linearity ranged from 1 to 10 mgL-1 for nicotine (R2=0.999, n=6). The method was successfully applied to Maras powder samples.

Anahtar Kelimeler

• Nicotine
• smokeless tobacco
• maras powder
• liquid chromatography-mass spectrometry
• electrospray ionization

Kaynakça

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