Method for chirally analyzing nicotine and nornicotine in tobacco and tobacco products
A technology for tobacco products and analysis methods, which is applied in the field of tobacco chemical composition analysis, and achieves the effects of high sensitivity, simple and rapid analysis methods, and good repeatability.
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Embodiment 1
[0047] 1. Sample pretreatment
[0048] Take flue-cured tobacco leaves and grind them to obtain tobacco powder samples. Take 1g of tobacco powder samples and place them in a 15mL test tube, add 2mL of 10% NaOH aqueous solution and 4mL of methyl tert-butyl ether, screw the cap tightly, and shake fully for 5min. Stand at 25°C for 10-14h overnight. The supernatant was filtered through a 0.22 μm filter membrane and then diluted with methyl tert-butyl ether to obtain the test solution. The volume ratio of supernatant to methyl tert-butyl ether was 1:10. Each sample was measured three times in parallel.
[0049] 2. Determination
[0050] The test solution prepared in the above step 1 was subjected to ultra-high performance convergence chromatography-tandem mass spectrometry detection, and the relative content of the chiral composition of nicotine and nornicotine in the test solution was determined by peak area normalization method. Among them, the chiral components of nicotine in...
Embodiment 2
[0062] 1. Sample pretreatment
[0063] Tobacco powder samples are obtained after grinding tobacco and tobacco products. Tobacco and tobacco products are selected from any one of tobacco leaves, tobacco stems, tobacco sheets or shredded tobacco, wherein the tobacco leaves are selected from Burley tobacco leaves, oriental tobacco leaves or flue-cured tobacco leaves One of them, the shredded tobacco is cigarette shredded tobacco. Take 1g of smoke powder sample and place it in a 15mL test tube, add 1-5mL of 5-15% NaOH aqueous solution and 2-8mL of methyl tert-butyl ether, screw the cap tightly, shake fully for 1-10min, and let it stand at room temperature for 6-18h overnight. The supernatant was filtered through a 0.22 μm filter membrane and then diluted with methyl tert-butyl ether to obtain the test solution. The volume ratio of the supernatant to the added methyl tert-butyl ether is 1:1-100. Each sample was measured three times in parallel.
[0064] 2. Determination
[006...
Embodiment 3
[0077]Get the racemic nicotine standard sample and the racemic nornicotine standard sample and carry out pretreatment according to step 1 of embodiment 1, then measure by the conditions of step 3 of embodiment 1, take 3 times of signal-to-noise ratio as detection limit , the detection limit of the method was obtained, and the specific results are shown in Table 2. Among them, the racemic nicotine standard substance is a mixed standard substance of S-(-)-nicotine and R-(+)-nicotine, and the mixture of S-(-)-nicotine and R-(+)-nicotine The mass ratio is 1:1. Nornicotine standard substance is the mixed standard substance of S-(-)-nornicotine and R-(+)-nornicotine, S-(-)-nornicotine and R-(+)-nornicotine The mass ratio is 1:1. It can be seen from Table 2 that due to the good separation between the two enantiomers, the detection limit of the method is less than 0.064 μg / mL, and the method has high sensitivity.
[0078] Table 2 Methodological investigation: detection limit
[00...
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