Method for detecting trigonelide in tobacco products and/or tobacco flavors and fragrances
A technology for fenugreek lactone and tobacco products, which is applied in the field of detection and analysis, can solve the problems of low detection threshold, difficulty, detection interference, etc., and achieves the effects of good repeatability and high accuracy
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Embodiment 1
[0074] Embodiment 1 Establishment of qualitative and quantitative method for trigonelline
[0075] 50 mg of trigonelactone (purity: 97.5% (W / W)) was dissolved in ethyl acetate to prepare a standard stock solution with a concentration of 1000 μg / mL.
[0076] Dissolve 220 mg of phenylethyl acetate standard product in ethyl acetate to prepare an internal standard stock solution with a concentration of 2200 μg / mL.
[0077] Pipette a certain volume of standard stock solution and internal standard stock solution to mix, dilute with ethyl acetate to obtain trigonelline concentrations of 1.0 μg / mL, 2.0 μg / mL, 5.0 μg / mL, 10.0 μg / mL, 20.0 μg / mL, 50.0μg / mL, 100.0μg / mL seven standard solutions, the internal standard concentration is 2.2μg / mL.
[0078] The standard solution was detected by gas chromatography-mass spectrometry (Agilent 7890A GC-5975C MSD).
[0079] Chromatographic conditions: Agilent DB-17ms quartz capillary column (60m×0.25mm×0.25μm); heating program: keep at 60°C for...
Embodiment 2
[0086] Determination of Trigonelactone in Embodiment 2 Essence for Tobacco
[0087] Weigh 0.20 g of tobacco essence, put it in a 50 mL Erlenmeyer flask, add 20 mL of ethyl acetate containing 2.2 μg / mL internal standard phenylethyl acetate and 10 mL of saturated saline, mix ultrasonically for 20 minutes, and filter to obtain the filtrate; The obtained filtrate was centrifuged at 6000 rpm for 10 minutes, left to stand, and the upper organic phase was taken, dried with anhydrous sodium sulfate, and then filtered with a 0.45 μm PTFE membrane to obtain the solution to be tested.
[0088] Adopt the gas chromatography-mass spectrometer of embodiment 1 to measure solution to be tested, detection condition is with embodiment 1, and the total ion current chromatogram that obtains is as follows Figure 4 shown. Substitute the ratio of the selected ion peak area of trigonelide to the internal standard into the standard working curve of Example 1 to calculate the mass concentration of...
Embodiment 3
[0096] The mensuration of trigonelide in embodiment 3 shredded tobacco
[0097] Take out shredded tobacco (flavored shredded tobacco) from a certain brand of cigarette, weigh 1.0g shredded tobacco sample and place it in a 50mL conical flask, add 20mL ethyl acetate solution containing 2.2μg / mL internal standard phenylethyl acetate and 10mL saturated salt Water, ultrasonically mixed for 20 minutes, filtered to obtain the filtrate; the obtained filtrate was centrifuged at 6000rpm for 10 minutes, left to stand, and the organic phase of the upper layer was taken, and 5g of anhydrous sodium sulfate and 150mg of graphitized carbon black were added to the organic phase. Shake and mix on a vortex shaker at 2000 rpm for 2 minutes, and then filter with a 0.45 μm PTFE membrane to obtain the solution to be tested.
[0098] Adopt the gas chromatography-mass spectrometer of embodiment 1 to measure solution to be tested, detection condition is with embodiment 1, and the total ion current ch...
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