CAJ | 학술논문

建立了同时检测烟草中多元酸(草酸、丙二酸、反丁烯二酸、琥珀酸、苹果酸和柠檬酸)和高级脂肪酸(棕榈酸、硬脂酸和亚油酸)的微波辅助甲酯化-快速气相色谱(GC)分析方法,并测定了烤烟及雪茄烟各10个烟叶样品中的多元酸和高级脂肪酸含量(质量分数).结果表明:①最优前处理条件为衍生化试剂10%硫酸-甲醇溶液,微波功率以20 W/s的速率升高至1200 W(保持1 min),萃取剂二氯甲烷.②快速GC分析时间为8.81 min,目标化合物标准曲线线性良好(r2>0.99),加标回收率在83.18%~114.17%之间,精密度(RSD)小于5%.③烤烟烟叶和雪茄烟烟叶中有机酸含量差异较大,其中烤烟烟叶中多元酸(除苹果酸外)含量低于雪茄烟烟叶,高级脂肪酸(除硬脂酸外)含量高于雪茄烟烟叶.该方法快速、准确,适用于测定烟草中的多元酸和高级脂肪酸含量.
건립료동시검측연초중다원산(초산、병이산、반정희이산、호박산、평과산화저몽산)화고급지방산(종려산、경지산화아유산)적미파보조갑지화-쾌속기상색보(GC)분석방법,병측정료고연급설가연각10개연협양품중적다원산화고급지방산함량(질량분수).결과표명:①최우전처리조건위연생화시제10%류산-갑순용액,미파공솔이20 W/s적속솔승고지1200 W(보지1 min),췌취제이록갑완.②쾌속GC분석시간위8.81 min,목표화합물표준곡선선성량호(r2>0.99),가표회수솔재83.18%~114.17%지간,정밀도(RSD)소우5%.③고연연협화설가연연협중유궤산함량차이교대,기중고연연협중다원산(제평과산외)함량저우설가연연협,고급지방산(제경지산외)함량고우설가연연협.해방법쾌속、준학,괄용우측정연초중적다원산화고급지방산함량.
A method combining microwave-assisted derivatization with fast gas chromatography (GC) was developed for rapidly determining the contents of polybasic acids (oxalic acid, malonic acid, fumaric acid, succinic acid, malic acid and citric acid) and higher fatty acids (palmitic acid, stearic acid and linoleic acid) in tobacco, and the contents of these acids in ten flue-cured tobacco samples and ten cigar filler tobacco samples were determined. The results showed that: 1) The optimal pretreatment conditions were using 10% sulfuric acid-methanol as esterification reagent and CH2Cl2 as extraction agent while the power of microwave increased at a rate of 20 W/s to 1200 W (remaining for 1 min). 2) The time for fast GC analysis was 8.81 min, the calibration curves of target compounds displayed good linearity (r2 > 0.99), the standard addition recoveries ranged from 83.18% to 114.17% with RSD less than 5%. 3) The contents of organic acids in flue-cured tobacco and cigar filler tobacco were quite different, the contents of polybasic acids (excluding malic acid) were higher in cigar filler tobacco, while the contents of higher fatty acids (excluding stearic acid) were higher in flue-cured tobacco. This method is rapid, accurate and suitable for the determination of polybasic acids and higher fatty acids in tobacco.