A processing method for smokeless tobacco products and a method for determining small molecular aldehydes in smokeless tobacco products
A technology of smokeless tobacco and a determination method is applied in the field of physical and chemical inspection of smokeless tobacco products, which can solve the problems of long analysis time and high detection limit, and achieve the effects of short analysis time, low detection limit and rapid extraction.
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Embodiment 1
[0071] The processing method of the smokeless tobacco sample of the present embodiment comprises the following steps:
[0072] Weigh 0.5g of a Swedish smoke-containing sample in bulk, add 20mL of ammonium formate buffer, 1mL of DNPH in acetonitrile, and 5mL of isohexane in sequence, seal it and ultrasonicate for 20min, then let it stand for stratification, and transfer 1mL of the upper organic phase to a brown sample bottle ,spare.
[0073] The determination method of small molecule aldehydes in the smokeless tobacco product of the present embodiment comprises the following steps:
[0074] 1) Weigh 0.5g of a Swedish smoke-containing sample in bulk, add 20mL of ammonium formate buffer, 0.1mL of internal standard solution, 1mL of DNPH in acetonitrile, 5mL of isohexane, seal and ultrasonicate for 20min, then let it stand for stratification, and take 1mL The upper organic phase was transferred to the brown sample bottle to obtain the test solution, which was set aside;
[0075] ...
Embodiment 2
[0088] The collected bags of Swedish tobacco (No. 1), bulk Swedish tobacco (No. 2), American tobacco (No. 3), bulk chewing tobacco (No. 4), block chewing tobacco (No. 5), dry One each of snuff (No. 6), tobacco lozenge (No. 7), and gum-based tobacco candy (No. 8) was processed and measured by the method of Example 1, and the results are shown in Table 4.
[0089] Table 4 Determination values of 6 kinds of small molecule aldehyde contents in smokeless tobacco products
[0090]
[0091] Note: N.D. is not detected.
[0092] In other embodiments of the present invention, the internal standard solution in the assay method can be a single formaldehyde-d2 solution, and the standard working solution is a formaldehyde solution with different concentration gradients, formaldehyde, acetaldehyde, propionaldehyde, acrolein, butyraldehyde and croton All aldehydes were quantified using formaldehyde-d2 as an internal standard, and other determination steps were the same as in Example 1. ...
experiment example
[0095] The standard working solution sample with the lowest concentration was analyzed by UPLC-HRMS, and the limit of detection (LOD) was calculated by three times the signal-to-noise ratio (S / N=3), and the limit of detection was 0.02-0.27 ng / mL. Carry out standard addition recovery experiment, measure in parallel 5 times, the average value of the results is shown in Table 5. The results showed that the recoveries of the six aldehydes ranged from 81.1% to 107.6%, and the average relative standard deviation (RSD) was less than 13%.
[0096] Table 5 Analysis performance parameters of small molecule aldehydes
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