Detection method of synthetic phenol antioxidants in flavors and fragrances for cigarettes
A technology of phenolic antioxidants and tobacco flavors, applied in the field of liquid chromatography analytical chemistry, to achieve method safety, intuitive qualitative and quantitative determination, and improve detection sensitivity
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Embodiment 1
[0020] The invention is used to detect the content of synthetic phenolic antioxidants in water-soluble flavors and fragrances.
[0021] 1. Production of working curve:
[0022] Take 1 mL of standard solutions with PG, TBHQ, BHA, and BHT concentrations of 1.0, 20.0, 40.0, 60.0, 80.0, and 100.0 μg / mL respectively, add 0.75 mL of nonionic surfactant TMN-6, and dilute to 5 mL with deionized water , placed in a water bath at 45°C for 25 minutes, centrifuged at 3000 rpm for 10 minutes, discarded the upper aqueous phase, diluted the lower surfactant phase with methanol to 1 mL, and measured the peak area at a wavelength of 280 nm; the flow rate of the mobile phase was: 1.0 mL / min, The mobile phase is: 0.1% acetic acid aqueous solution (A), methanol (B); 0-5min, B is 40%, A is 60%, 5-10min, B is linearly increased from 40% to 70%, and A is from 60% Decrease to 30%, 10-25min, B rises to 90%, A drops to 10%, no need to run. Among them, the retention time of PG is 6.0 min, that of TBHQ...
Embodiment 2
[0028] The invention is used to detect the content of synthetic phenolic antioxidants in water-soluble flavors and fragrances.
[0029] 1. Production of working curve:
[0030] Take PG, TBHQ, BHA, BHT concentration of 5.0, 50.0, 100.0, 150.0, 200.0, 250.0, 300.0μg / mL standard solution 1mL, add 0.25mL of NP-7 and 0.5mL of NP-9 non-ionic surfactant placed in a water bath at 50°C for 35 minutes, centrifuged at 4000 rpm for 8 minutes, discarded the upper aqueous phase, diluted the lower surfactant phase with methanol to 1 mL, and measured the peak area at 280 nm; the flow rate of the mobile phase was 1.0 mL / min, and the Phase: 0.1% acetic acid aqueous solution (A), methanol (B); 0-4.5min, B rises linearly from 50% to 85%, A drops from 50% to 15%, 4.5-6.5min, B rises to 90% %, A drops to 10%, 6.5-9.0min, B drops to 50%, A rises to 50%, no need to run after. Among them, the retention time of PG is 3.2min, the retention time of TBHQ is 4.1min, the retention time of BHA is 6.0min, a...
Embodiment 3
[0037] The invention is used to detect the content of synthetic phenolic antioxidants in fat-soluble flavors and fragrances.
[0038] 1. According to step 1 of example 1.
[0039] 2. Sample processing
[0040] Take 1.0g of water-soluble flavors and fragrances in a 10mL centrifuge tube, add 1mL of methanol to extract the antioxidants twice, combine the extracts, transfer to a 5mL centrifuge tube, shake well, add 1.0mL of non-ionic surfactant TMN-6, and use Dilute the deionized water to 5mL, place in a water bath at 50°C for 10min, centrifuge at 5000rpm for 4min, discard the upper aqueous phase, dilute the lower surfactant phase with methanol to 1mL, measure the peak area at 280nm, and substitute it into Table 3. According to the curve, the contents of BHA and BHT in water-soluble flavors and fragrances are obtained to be 57.94 μg / mL and 460.46 μg / mL, respectively.
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