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.