Detection method for detecting bad smell of 2,4,6-trichloroanisole (TCA) in port wine
A wine and detector technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of complicated operation, poor repeatability, poor sensitivity, etc., and achieve the effect of simplified operation steps, low cost and high sensitivity
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Embodiment 1
[0038] Column Selection and TCA Qualitative Analysis
[0039] There are many flavor components in wine, and ultra-trace TCA components are also easily interfered by other impurities when they are separated by chromatographic columns. Two chromatographic columns with different specifications and properties are selected, combined with GC chromatographic conditions optimization, to achieve TCA composition in wine.
[0040] Chromatographic column 1: DB-WAX capillary column (30m×0.25mm×0.25μm, film thickness 0.25μm, agilent technical)
[0041] Chromatographic column 2: DB-5 capillary column (30m×320μm×0.25μm, film thickness 0.25μm)
[0042] Chromatographic conditions:
[0043]Injection port temperature: 270°C, detector temperature: 330°C, nitrogen flow rate: 1ml / min, heating program: initial temperature 70°C, hold for 3min, rise to 180°C at a rate of 5°C / min, and then increase at a rate of 10°C / min Rise to 270°C and keep for 3min.
[0044] By configuring standard samples, the r...
Embodiment 2
[0047] Method evaluation:
[0048] With DCA as the internal standard, the linear correlation coefficient R2 of the TCA compound is greater than 0.997, and the detection limit of TCA is 0.5ng / L, wherein the relative standard deviation is less than 15%, which can meet the requirements of ultra-trace TCA analysis in wine. The present invention has made the recovery rate The results show that the recovery rate of the method is more than 90%, which meets the requirements of trace analysis, as shown in the table. According to the principle of the standard addition method, adding 60ng / L, 120ng / L and 240ng / L of TCA to the same wine respectively, a good linear curve was obtained, indicating that the determination of TCA in wine has a very good linear range. For details, see image 3 .
[0049] Table 1 Wine Sample Recovery Determination
[0050]
Embodiment 3
[0052] Determination of actual wine samples
[0053] This invention selects wines of major brands in my country as the target wine samples, and measures them according to the following conditions:
[0054] Sample preparation:
[0055] Take 5mL of wine sample into a 25mL headspace bottle, add 2gNaCl, then add 50μg / L DCA (internal standard) solution, and press the cap. Place in the sample tray and wait for the sample to be injected.
[0056] ITEX conditions:
[0057] Balance temperature: 60°C, balance time: 30min, balance speed: 500rpm;
[0058] Injection needle temperature: 40℃, extraction volume: 1000μl, extraction times: 30; injection volume: 700μl; extraction speed: 100μl / s; ITEX pyrolysis temperature: 200℃; pyrolysis speed: 100μl / s; ITEX cleaning temperature : 200℃, cleaning time: 10:00min
[0059] Chromatographic conditions:
[0060] Inlet temperature: 270°C Detector temperature: 330°C
[0061] Nitrogen flow rate: 1ml / min
[0062] Heating program: the initial tempe...
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