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  • Increasing the instrumental throughput of gas chromatography method using multiple injections in a single experimental run: application in determination of friedelan-3-ol and friedelin in Maytenus ilicifolia.

Increasing the instrumental throughput of gas chromatography method using multiple injections in a single experimental run: application in determination of friedelan-3-ol and friedelin in Maytenus ilicifolia.

Journal of chromatography. A (2013-01-02)
Jacqueline Pereira Vistuba, Marcel Piovezan, Moacir Geraldo Pizzolatti, Andrey Martinez Rebelo, Mônia Stremel Azevedo, Luciano Vitali, Ana Carolina Oliveira Costa, Gustavo Amadeu Micke
ABSTRACT

The aim of this study was to develop a separation method using multiple injections in a single experimental run (MISER) employing gas chromatography with flame ionization detection (GC-FID) for the first time, without instrument modification, to increase the instrumental throughput. The method was applied to the determination of the triterpenes friedelan-3-ol and friedelin in a plant extract obtained from Maytenus ilicifolia leaves. The column used in the chromatography system was a ZB-50 (30 m × 0.25 mm × 0.15 μm) with 50% phenyl-50% methyl-polysiloxane. The samples (1.0 μL) were injected using the split mode (1:90), with the injector at 280 °C and FID detector at 320 °C. The column temperature was programmed to isothermal mode at 300°C. Helium was used as the carrier gas with a constant flow of 1.5 mL min(-1). It was possible to perform three injections in the same run using the MISER method. An increase in the instrumental throughput by a factor of around 2.6 was observed when the use of multiple injections was compared with the single injection method. This method showed good linearity for both analytes with R(2)>0.99 and the values for the limit of detection were 0.24 mg L(-1) and 0.44 mg L(-1), for friedelan-3-ol and friedelin, respectively. Furthermore, the values for the limits of quantification were 0.79 mg L(-1) for friedelan-3-ol and 1.16 mg L(-1) for friedelin. The proposed method has potential for other GC applications, allowing an increase in the instrumental throughput of the methods by applying this separation technique.

MATERIALS
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Sigma-Aldrich
Friedelin, technical grade