Method for determining sulfide in spirit
A technology for sulfides and liquor, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of time-consuming and labor-intensive sensitivity, poor selectivity, and limited sensitivity, so as to improve accuracy, improve liquor quality, and avoid The effect of decomposition
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Embodiment 1
[0028] Dilute 53% (v / v) Moutai with deionized water to 14% alcohol (v / v), draw 5 mL of wine sample and place it in a 20 mL headspace bottle, add 100 μL of internal standard solution, and saturate with sodium chloride. , screw the lid tightly. Stir and equilibrate at 500 rpm in a 30 °C water bath for 30 min, insert an 85 μm Carboxen-PDMS fiber tip, and extract at 30 °C and 250 rpm for 15 min. Then the extraction head was inserted into the gas injection port and desorbed at 300 °C in splitless mode for 7 min. Using DB-FFAP, the column temperature was maintained at 35 °C for 3 min, raised to 150 °C at a heating rate of 10 °C / min, held for 5 min, and then raised to 220 °C at a heating rate of 20 °C / min, held for 3 min. Nitrogen was used as the carrier gas, and the constant flow was 2 mL / min. The detector temperature was 300°C and fed with 14 mL / min hydrogen, 17 mL / min air 1 and 10 mL / min air 2. The detector voltage is 500V, the gate delay is 6ms, and the gate width is 20ms.
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Embodiment 2
[0031] 52% (v / v) Wuliangye was detected, and the detection conditions were the same as those in Example 1. Fig. 2 is the gas chromatogram of this wine sample, the detected sulfide has hydrogen sulfide (H 2 S) 176.17 μg / L, methyl mercaptan (MeSH) 28.93 μg / L, dimethyl sulfide (DMS) 6.30 μg / L, methyl thioacetate (MeSOAc) 39.60 μg / L, dimethyl disulfide (DMDS) 1.68 μg / L, ethyl thioacetate (EtSOAc) 19.73 μg / L, diethyl disulfide (DEDS) 0.05 μg / L, dimethyl trisulfide (DMTS) 21.45 μg / L, 3 - Methylthiopropanol (methionol) 0.36 mg / L.
Embodiment 3
[0033] 46% (v / v) of Yanghe Daqu was detected, and the detection conditions were the same as those in Example 1. Fig. 3 is the gas chromatogram of this wine sample, the detected sulfide has hydrogen sulfide (H 2 S) 17.50μg / L, methyl mercaptan (MeSH) 14.46μg / L, dimethyl sulfide (DMS) 2.52μg / L, methyl thioacetate (MeSOAc) 1.60μg / L, dimethyl disulfide (DMDS) 1.52 μg / L, ethyl thioacetate (EtSOAc) 5.33 μg / L, diethyl disulfide (DEDS) 0.04 μg / L, dimethyl trisulfide (DMTS) 14.56 μg / L, 3 - Methylthiopropanol (methionol) 0.81 mg / L.
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