不同生态区烟叶新植二烯含量的反吹气相色谱法检测与分析
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作者:王冰 赵乐 余晶晶 蔡君兰 丁美宙 彭斌 赵俊伟 赵晓东 秦亚琼 刘克建 刘绍锋 谢复炜
摘 要:榭焖俨舛ㄑ桃缎轮捕烯含量,构建了5 m DB-5ms预分离柱结合10 m DB-5ms分析柱的反吹柱系统,确立了反吹压力103 kPa,反吹时间4.5 min的色谱条件及采用10 mL二氯甲烷涡旋提取0.5 g烟粉5 min的前处理方法,并对114个国内外代表性烟样进行了分析。结果表明:①新植二烯在10~200 ?g/mL范围内线性良好(相关系数r?0.999 9)。新植二烯定量限为16 ?g/g,加标回收率在98%~101%之间,日间、日内相对标准偏差分别为1.81%和1.76%,长期(两年)相对标准偏差小于5%。每个样品分析时间仅为8 min。②将国内5个生态区烟叶与代表性进口烟叶中新植二烯含量进行对比分析,西南高原生态区烟叶与代表性进口烟叶无显著性差异;其余4个生态区(武陵秦巴、南岭丘陵、武夷丘陵、沂蒙丘陵)烟叶与代表性进口烟叶有显著性差异。③无论从整体还是从每个生态区分析烟叶新植二烯含量,上部烟叶与中部烟叶无显著性差异,与下部烟叶相比,均有显著性差异,下部烟叶新植二烯含量较高。本研究通过反吹气相色谱-火焰离子化检测器检测烟叶新植二烯含量,所建方法简单、快速、灵敏度高、重复性好,可用于不同产区、不同部位烟叶中新植二烯含量的批量定量检测。
关键词:烟叶;新植二烯;反吹技术;气相色谱
Abstract: In order to rapidly analyze neophytadiene in tobacco leaves, a back blowing column system (5 m DB-5ms pre separation column combined with 10 m DB-5ms analysis column) was developed. Chromatographic conditions (back blowing pressure of 103 kPa and back blowing time of 4.5 min) and pretreatment method (extracting 0.5 g tobacco powder with 10 mL dichloromethane vortexing for 5 min) were established, 114 representative tobacco samples at home and abroad were analyzed. The results showed that: 1) In a range of 10-200 μg/mL, neophytadiene had good linear relationship (r?0.999 9). The limit of quantitation of neophytadiene was 16 ?g/g. The spiked recoveries ranged from 98% to 101%, the relative standard deviations (RSD) of inter day and intra day were 1.8% and 1.76% respectively and the long-term (Two-year) RSD was less than 5%. The analysis time of each sample was only 8 min; 2) The contents of neophytadiene in tobacco leaves from five domestic ecological regions and abroad were compared, and no significant differences were found between the southwest plateau ecological region and abroad, but significant differences were observed between the other four domestic ecological regions (Wuling Qinba, Nanling hills, Wuyi hills, Yimeng hills) and abroad; 3) By analyzing the neophytadiene in tobacco leaves from the whole or each individual ecological region, no significant differences were found between the upper and middle leaves, but when compared with the lower leaves, there were significant differences and the content of neophytadiene in the lower leaves was higher. In this study, neophytadiene in tobacco leaves was detected by back blowing gas chromatography and flame photometric detector. The method was simple, rapid, sensitive and reproducible. It can be used for batch quantitative determination of neophytadiene in different parts of tobacco leaves from different production regions.
Keywords: tobacco; neophytadiene; back-flush technique; gas chromatography
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