Sriseadka Tinakorn, Wongpornchai Sugunya, Kitsawatpaiboon Pisan
Department of Chemistry, Faculty of Science, Chiang Mai University, Chiang Mai 50200, Thailand.
J Agric Food Chem. 2006 Oct 18;54(21):8183-9. doi: 10.1021/jf0614490.
A rapid method employing static headspace gas chromatography (HS-GC) has been developed and validated for quantitative analysis of the impact aroma compound, 2-acetyl-1-pyrroline (2AP), in grains of fragrant rice. This developed method excludes wet extraction, and the rice headspace volatiles are brought directly and automatically to GC analysis. The conditions of the static HS autosampler were optimized to achieve high recovery and sensitivity. The most effective amount of rice sample used was 1 g, which provided 51% recovery and a linear multiple headspace extraction (MHE) plot of the peak area of 2AP. The sensitivity of the method was enhanced by utilizing a megabore fused silica capillary column in conjunction with a nitrogen-phosphorus detector (NPD). Method validations performed for both static HS-GC-FID and HS-GC-NPD demonstrated linear calibration ranges of 20-10 000 (r(2) = 0.9997) and 5-8000 (r(2) = 0.9998) ng of 2AP/g of rice sample, respectively. The limits of detection for both systems were 20 and 5 ng of 2AP, and the limits of quantitation were 0.30 and 0.01 g of brown rice sample, respectively. Reproducibility calculated as intraday and interday coefficients of variation were 3.25% RSD (n = 15) and 3.92% RSD (n = 35), respectively, for SHS-GC-FID and 1.87% RSD (n = 15) and 2.85% RSD (n = 35), respectively, for SHS-GC-NPD. The method was found to be effective when applied to the evaluation of aroma quality, based on 2AP concentrations, of some fragrant rice samples.
已开发并验证了一种采用静态顶空气相色谱法(HS-GC)的快速方法,用于定量分析香稻籽粒中具有影响的香气成分2-乙酰基-1-吡咯啉(2AP)。该方法无需湿提取,可直接自动将稻粒顶空挥发物送入GC分析。对静态顶空自动进样器的条件进行了优化,以实现高回收率和灵敏度。所用最有效的稻样量为1 g,其2AP峰面积的回收率为51%,且具有线性多顶空萃取(MHE)图。通过使用大口径熔融石英毛细管柱结合氮磷检测器(NPD)提高了该方法的灵敏度。对静态HS-GC-FID和HS-GC-NPD进行的方法验证表明,2AP的线性校准范围分别为20 - 10000(r(2) = 0.9997)和5 - 8000(r(2) = 0.9998)ng/g稻样。两个系统的检测限分别为20和5 ng 2AP,定量限分别为0.30和0.01 g糙米样品。对于SHS-GC-FID,按日内和日间变异系数计算的重现性分别为3.25% RSD(n = 15)和3.92% RSD(n = 35),对于SHS-GC-NPD分别为1.87% RSD(n = 15)和2.85% RSD(n = 35)。基于2AP浓度,该方法在应用于一些香稻样品的香气品质评估时被证明是有效的。