A method for detecting the content of polycyclic aromatic hydrocarbons in smokeless tobacco products
A technology of smokeless tobacco and polycyclic aromatic hydrocarbons, applied in measuring devices, instruments, scientific instruments, etc., to achieve high sensitivity, reduce pollution, and good selectivity
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Embodiment 1
[0050] Weigh 3g of snus as sample A and place it in a 25mL ground-mouth Erlenmeyer flask, add 250 μL of cyclohexane solution containing deuterated naphthalene (320ng / mL) and deuterated benzo[a]pyrene (320ng / mL) as Add 15mL cyclohexane as the extractant for the internal standard substance; shake and extract the conical flask at room temperature for 40min, pass the extract through a 0.22μm nylon 66 filter membrane, collect the filtrate in the chromatographic bottle, and wait for GC-MS / MS analyze.
[0051] GC-MS / MS analysis conditions:
[0052] Chromatographic inlet temperature: 260°C; sample volume: 1μL; sample injection method: splitless injection; chromatographic column: HP-5MS UI (30m*0.32mm*0.25μm); temperature program: initial temperature 40°C, keep 7min; rise to 100°C at 20°C / min; rise to 300°C at 4°C / min and hold for 10min; transfer line temperature: 280°C; mass spectrometry ionization mode: EI; ion source temperature: 280°C; mass spectrometry scanning mode: dynamic mult...
Embodiment 2
[0072] Repeat Example 1, with the following differences:
[0073] Weigh 10g of chewing tobacco as sample B and place it in a 100mL ground-necked Erlenmeyer flask, add 500 μL of methanol solution containing deuterated benzo[a]anthracene (200ng / mL) and deuterated phenanthrene (200ng / mL) as an internal standard substance , and then add 50mL of methanol as the extractant; shake the Erlenmeyer flask at room temperature for 60min, pass the extract through a 0.45μm polyethersulfone (PES) filter membrane, collect the filtrate in the chromatographic flask, and wait for GC-MS / MS analysis .
[0074] GC-MS / MS analysis conditions:
[0075] Chromatographic inlet temperature: 260°C; sample volume: 1μL; sample injection method: splitless injection; chromatographic column: DB-5MS capillary column (30m*0.25mm*0.25μm); temperature program: initial temperature 150°C , rise to 280°C at 5°C / min and hold for 10min; transfer line temperature: 280°C; mass spectrometry ionization mode: EI; ion source...
Embodiment 3
[0080] Repeat Example 1, with the following differences:
[0081] Weigh 10g of snuff as sample C and place it in a 50mL ground-mouth Erlenmeyer flask, add 500 μL of dichloromethane solution containing deuterated benzo[a]pyrene (320ng / mL) as an internal standard substance, and then add 20mL of dichloromethane as Extractant: Shake the Erlenmeyer flask at room temperature for 60 minutes, pass the extract through a 0.22 μm polyethersulfone (PES) filter membrane, collect the filtrate in a chromatographic bottle, and wait for GC-MS / MS analysis.
[0082] GC-MS / MS analysis conditions:
[0083] Chromatographic inlet temperature: 260°C; sample volume: 1μL; sample injection method: splitless injection; chromatographic column: HP-5MS capillary column (30m*0.25mm*0.25μm); temperature program: initial temperature 180°C , raised to 270°C at 3°C / min and kept for 20min; transfer line temperature: 280°C; mass spectrometry ionization mode: EI; ion source temperature: 250°C; mass spectrometry sc...
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