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    短柱气相色谱-质谱法快速测定烟草中西柏三烯二醇的含量

    Rapid Determination of Cembratriene-Diol in Tobacco by Gas Chromatography with Short Column-Mass Spectrometry

    • 摘要: 为克服YC/T 470—2013需衍生化处理、色谱运行时间长等弊端,设计了集提取、过滤与干燥功能于一体的样品前处理装置,优化了前处理条件,并采用题示方法测定西柏三烯二醇(CBD)的两种主要异构体α-CBD和β-CBD的总量。取0.100 g烟草样品,置于自主设计的样品前处理装置中,加入10 mL含10 mg·L−1 1-十七烷醇(内标)的二氯甲烷溶液,超声提取15 min,提取液注入短柱气相色谱-质谱仪。以DB-5 MS色谱柱(长度15 m)为固定相,在程序升温条件下分离CBD,用电子轰击离子源正离子模式电离,内标法定量。结果表明:CBD标准曲线的线性范围为10~1 500 mg·L−1,检出限(3S/N)为0.26 μg·g−1;按标准加入法进行回收试验,回收率为92.1%~101%,测定值的相对标准偏差(RSD,n=6)不大于4.0%。方法用于10个不同烟草以及烟草制品的分析,测定值和YC/T 470—2013的基本一致,测定值的RSD(n=5)低于YC/T 470—2013的。

       

      Abstract: In order to overcome the drawbacks of YC/T 470—2013,including requring derivatization treatment and long chromatographic operation time, the sample pretreatment device integrating extraction, filtration, and drying functions was designed. The pretreatment conditions were optimized, and the total amount of the 2 main isomers α-cembratriene-diol (CBD) and β-CBD of CBD was determined by the title method. An aliquot (0.100 g) of tobacco sample was taken and placed into the self-made sample pretreatment device. Then, 10 mL of dichloromethane solution containing 10 mg · L−1 1-heptadecanol (internal) was added, and the mixture was extracted by ultrasound for 15 min. The extraction solution was injected into the gas chromatograph with short column-mass spectrometer. With DB-5 MS column (the column length was 15 m) as the stationary phase, CBD was separated under the temperature programmed condition, ionized in the positive ion mode of the electron impact ion source, and quantified by the internal standard method. It was shown that the linear range of the standard curve for CBD was in the range of 10-1 500 mg · L−1, with detection limit (3S/N) of 0.26 μg · g−1. Test for recovery was conducted using the standard addition method, giving recoveries in the range of 92.1%-101%, and RSDs (n=6) of the determined values did not exceed 4.0%. The proposed method was used for the analysis of 10 different types of tobacco and tobacco products, with the determined values basically consistent with those given by YC/T 470—2013, and RSDs (n=5) of the determined values were lower than those of YC/T 470—2013.

       

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