Detection method of phenolic acids and / or phenol esters in wine and / or wine by-products
A detection method and by-product technology, applied in the field of chemical analysis, can solve the problems of difficult detection, weak column retention, complex components, etc., and achieve the effects of high sensitivity, extended column retention, and high detection sensitivity
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Embodiment 1
[0061] Example 1 Using the method of the present invention to detect phenolic acid / ester compounds in liquor
[0062] LC-QTOF (high performance liquid chromatography quadrupole time-of-flight mass spectrometry instrument) liquid chromatography conditions: mobile phase: A is ultrapure aqueous solution (0.1g / L formic acid), B is methanol, gradient elution: 0 -15 min: 5-100% v / v B (the instrument automatically realizes the gradient change); 15-20 min: 100% v / v B; 20-22 min: 5% v / v B; stop elution.
[0063] The chromatographic column is a ZORBAX Eclipse Plus C18 column with a column length of 100mm, an inner diameter of 2.1mm, a particle size of 1.8μm, a column temperature of 30°C, a flow rate of 0.2mL / min, and an injection volume of 2μL.
[0064] The mass spectrometry conditions of the LC-QTOF coupled instrument are: electrospray ion source, negative mode, drying gas temperature 325°C, drying gas flow rate 10L / min, atomizing gas pressure 40psig, capillary voltage 3500v, capillary...
Embodiment 2
[0076] Example 2 Using the method of the present invention to detect phenolic acid / ester compounds in distiller's grain yellow water
[0077] a. The drawing of the standard curve is the same as in Example 1; the conditions of the liquid chromatography of the LC-QTOF coupled instrument are the same as in Example 1.
[0078] b. Take three samples of distiller's grain yellow water respectively (provided by the Analysis and Research Office of Wuliangye Technology Research Center), each 1ml, two of which are respectively added with phenolic acid standard solution 200ug / L, 2000ug / L, loading HLB, 0.01%w / w rinse with formic acid water, elute with 90% methanol water solution, dry methanol water eluent with nitrogen gas, dissolve in 1ml methanol, and inject LC-QTOF as a test sample. The total ion chromatogram of distiller's grain yellow water sample is shown in image 3 (The abscissa in the figure represents time / min, and the ordinate represents ion intensity).
[0079] c. Analysis o...
Embodiment 3
[0083] Example 3 Using the method of the present invention to detect phenolic acid / ester compounds in distiller's grains
[0084] a. The drawing of the standard curve is the same as in Example 1; the conditions of the liquid chromatography of the LC-QTOF coupled instrument are the same as in Example 1.
[0085] b. Take three samples of distiller's grains (distiller's grains samples are provided by the Analysis and Research Office of Wuliangye Technology Research Center), each 10g, two of which are added to phenolic acid standard solution 200ug / L, 2000ug / L, 50ml methanol extraction, take 10ml Evaporate the extract at 90°C to remove methanol, apply HLB after dilution with water, rinse with 0.01% w / w formic acid water, elute with 90% methanol aqueous solution, dry methanol water eluent with nitrogen, dissolve in 1ml methanol, and use it as a test sample Inject LC-QTOF. The total ion chromatogram of the distiller's grain sample is shown in Figure 4 (The abscissa in the figure r...
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