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加速溶剂萃取GC-MS快速分析烟叶中的西柏三烯二醇
蔡长春,任晓红,冯吉,邓建强,李章海,饶雄飞,王洪炜,杨俊
0
(湖北省烟草科学研究院,武汉 430030;湖北省烟草公司恩施州公司,恩施 445000;中国科学技术大学先进技术研究院,合肥 230088)
摘要:
采用加速溶剂萃取(ASE)结合衍生化气相色谱质谱(GC-MS)检测,建立烤烟烟叶中α-西柏三烯二醇(α-CBD)和β-西柏三烯二醇(β-CBD)两种化合物的定量分析方法。对比研究了液固萃取(LSE)、超声辅助萃取(UAE)、索氏提取(SE)和ASE 4种不同样品前处理方法对目标物萃取效果的影响,优选出ASE方法应用于烟叶中CBD的提取。优化设定ASE的工作参数,萃取剂为二氯甲烷,萃取温度50 ℃,静态萃取时间5 min,循环萃取次数为2次。对分析方法的线性范围、检出限、定量限、回收率和精密度等进行了实验验证,结果表明,目标成分α-CBD和β-CBD的线性关系良好,线性范围分别为1.0 ~ 200.0 μg·g−1和1.0 ~ 160.0 μg·g−1,相关系数(R)分别为0.999 2和0.999 6。两种目标物的最低检出限(LOD)和最低定量限(LOQ)分别为0.3 μg·g−1、0.2 μg·g−1和0.85 μg· g−1、0.66 μg·g−1。回收率分别在93.2% ~ 103.3% 和91.6% ~ 99.1% 之间。检测α-CBD和β-CBD的相对标准偏差(RSDs,n = 5)分别在2.59% ~ 3.13%和2.11% ~ 2.84% 范围内。方法快速、准确,在对不同地区、不同部位烤烟烟叶中西柏三烯二醇含量的比较分析中取得良好结果,适用于烟叶中西柏三烯二醇的分析检测。
关键词:  加速溶剂萃取  气相色谱质谱  西柏三烯二醇  烟叶
DOI:10.13610/j.cnki.1672-352x.20220325.018
基金项目:中国烟草总公司湖北省公司科技项目(027Y2021-016)资助。
Rapid analysis of cembratrien-diols in tobacco leaves by accelerated solvent extraction and GC-MS detection
CAI Changchun,REN Xiaohong,FENG Ji,DENG Jianqiang,LI Zhanghai,RAO Xiongfei,WANG Hongwei,YANG Jun
(Tobacco?Research?Institute?of?Hubei?Province,?Wuhan?430030;Enshi Tobacco Company of Hubei Province, Enshi 445000;Institute of Advanced Technology, University of Science and Technology of China,?Hefei 230088)
Abstract:
A quantitative analysis method of α-cembratriene-diol (α-CBD) and β-cembratriene-diol (β-CBD) in flue-cured tobacco leaves was established by using accelerated solvent extraction (ASE) combined with derivatization gas chromatography-mass spectrometry (GC-MS) detection. The effects of four different sample pretreatment methods such as liquid-solid extraction, ultrasonic-assisted extraction, soxhlet extraction and ASE on the extraction rates of target compounds were compared, and the ASE method was selected to extract CBDs from flue-cured tobacco leaves. The working parameters of ASE were optimized as follows: dichloromethane was used as extraction solvent, extraction temperature was 50℃, static extraction time was 5 min, and number of cycles were 2 times. Performance characteristics such as linearity, limit of detection (LOD), limit of quantitation (LOQ), recovery and precision were studied. The linear ranges for α-CBD and β-CBD were 1.0 - 200.0 μg·g-1 and 1.0 -160.0 μg·g-1, and the correlation coefficients (R) were 0.999 2 and 0.999 6, respectively. LOD and LOQ of the two target substances were 0.3 μg·g-1, 0.2 μg·g-1 and 0.85 μg·g-1, 0.66 μg·g-1, respectively. Average recoveries of α-CBD and β-CBD were 93.2% - 103.3% and 91.6% - 99.1%, while the relative standard deviations (RSDs, n = 5) ranged from 2.59% to 3.13% and 2.11% to 2.84%, respectively. The proposed method is rapid and accurate and has achieved good results in the comparative analysis of the content of CBDs in flue-cured tobacco leaves from different regions and different parts. It is suitable for the analysis and detection of CBDs in tobacco leaves samples.
Key words:  accelerated solvent extraction  GC-MS (gas chromatography-mass spectrometer)  cembratrien-diols  tobacco leaves

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