CN113252589B - Detection method for content of sodium carboxymethylcellulose in wine - Google Patents
Detection method for content of sodium carboxymethylcellulose in wine Download PDFInfo
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- 239000001768 carboxy methyl cellulose Substances 0.000 title claims abstract description 66
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 title claims abstract description 65
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 title claims abstract description 65
- 235000014101 wine Nutrition 0.000 title claims abstract description 65
- 238000001514 detection method Methods 0.000 title abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 94
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 93
- 238000002835 absorbance Methods 0.000 claims abstract description 46
- 239000012224 working solution Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 20
- 235000020095 red wine Nutrition 0.000 claims abstract description 14
- 235000020097 white wine Nutrition 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims description 105
- 238000002156 mixing Methods 0.000 claims description 56
- 238000006243 chemical reaction Methods 0.000 claims description 42
- DFQICHCWIIJABH-UHFFFAOYSA-N naphthalene-2,7-diol Chemical compound C1=CC(O)=CC2=CC(O)=CC=C21 DFQICHCWIIJABH-UHFFFAOYSA-N 0.000 claims description 32
- 238000000502 dialysis Methods 0.000 claims description 25
- 239000011521 glass Substances 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 241000219095 Vitis Species 0.000 claims description 17
- 235000009754 Vitis X bourquina Nutrition 0.000 claims description 17
- 235000012333 Vitis X labruscana Nutrition 0.000 claims description 17
- 235000014787 Vitis vinifera Nutrition 0.000 claims description 17
- 238000009835 boiling Methods 0.000 claims description 17
- 230000031700 light absorption Effects 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000010200 folin Substances 0.000 claims description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- YMKDRGPMQRFJGP-UHFFFAOYSA-M cetylpyridinium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+]1=CC=CC=C1 YMKDRGPMQRFJGP-UHFFFAOYSA-M 0.000 claims description 10
- 229960001927 cetylpyridinium chloride Drugs 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 8
- 239000012295 chemical reaction liquid Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 5
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 5
- 229940074439 potassium sodium tartrate Drugs 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- 238000006467 substitution reaction Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 8
- 238000011002 quantification Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000011088 calibration curve Methods 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 description 13
- 238000005303 weighing Methods 0.000 description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000012491 analyte Substances 0.000 description 5
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000001502 supplementing effect Effects 0.000 description 4
- 238000007865 diluting Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 239000011550 stock solution Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002562 thickening agent Substances 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- 229940106681 chloroacetic acid Drugs 0.000 description 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000001476 sodium potassium tartrate Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for detecting the content of sodium carboxymethylcellulose in wineThe measuring method comprises the following steps: (1) the concentration of the standard working solution is taken as the abscissa, and the absorbance difference delta (A) 540 ‑A 420 ) As ordinate, a calibration curve L of the sodium carboxymethylcellulose concentration is plotted 1 (ii) a (2) Drawing a standard curve L of the MI reagent by taking the concentration of the MI reagent as an abscissa and taking an absorbance value at 640nm as an ordinate 2 (ii) a (3) Taking MI reagent concentration as abscissa and absorbance values at 420nm and 540nm as ordinate, and drawing MI reagent standard curve L at 420nm and 540nm 3 、L 4 (ii) a And detecting the content of sodium carboxymethylcellulose in white wine, red wine and pink wine. The detection method can detect the content of sodium carboxymethylcellulose in red wine and pink wine, and enlarges the detection range; the detection limit and the quantification limit in white wine detection are reduced; the detection time is shortened, the recovery rate is improved, and the waste of water resources is reduced.
Description
Technical Field
The invention relates to the technical field of wine, in particular to a method for detecting the content of sodium carboxymethylcellulose in wine.
Background
Sodium carboxymethylcellulose (carboxymethylcellulose) is a water-soluble cellulose ether, a derivative obtained by chemically modifying natural cellulose and chloroacetic acid. The water solution has the functions of thickening, film forming, binding, water retention, emulsification and the like, and is often used as an emulsifier, a thickener and a water retention agent to be widely applied to the fields of food, medicine, pesticide, leather, plastic daily chemical industry and the like. In China, the GB 2760-2014 stipulates sodium carboxymethylcellulose to be used as a stabilizer (1) only in cream (CNS number 20.003); (2) the thickener can be used in various foods according to requirements (Table A.2), and GB/T15037-; while in foreign countries sodium carboxymethylcellulose as a stabilizer (usually added in a maximum amount of 100mg/L) is allowed by many countries and organizations to be used in wine to prevent the wine from producing tartaric acid precipitates.
At present, in the national wine import regulation, official inspection standards of the content of sodium carboxymethylcellulose in wine are not available, only an official recommended detection method (OIV-MA-AS315-22) of the international grape and wine organization is available internationally, and the application range only includes white wine, and no national standard detection method for measuring the content of sodium carboxymethylcellulose in red wine is available.
The OIV official recommendation method used by my technology center was approved by CNAS, but this method has two problems: firstly, the method has the problem of applicability, the OIV method only aims at white wine, and in foreign countries, the maximum usage amount of sodium carboxymethylcellulose in the wine is usually 100mg/L, and the initial purpose of establishing the method is to see whether the maximum limit amount is exceeded or not; the second method is the sensitivity problem, the detection limit of the OIV method is 20mg/L, and the quantification limit is 60 mg/L.
OIV is particularly suitable for countries where the addition of sodium carboxymethylcellulose is acceptable, i.e. where there is no excess, for countries where the use of sodium carboxymethylcellulose is not acceptable, the use of OIV results in undetected or very low detection rates, since the quantitation of the OIV method is limited to 60mg/L, which is precisely around the actual maximum amount of sodium carboxymethylcellulose.
The prior detection technology has the following defects: in the prior art, only the content of sodium carboxymethylcellulose in white wine can be detected, and whether the sodium carboxymethylcellulose is added in red wine and pink wine cannot be detected; the existing detection method limits the detection limit and the quantitative limit of the content of sodium carboxymethylcellulose in white wine; the existing detection method has low recovery rate and long detection time; the existing detection method has large water resource consumption.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the defects of the existing detection method for the content of sodium carboxymethylcellulose in wine, the invention provides the detection method for the content of sodium carboxymethylcellulose in wine, which shortens the detection time, improves the recovery rate and reduces the waste of water resources.
The technical scheme is as follows: a method for detecting the content of sodium carboxymethylcellulose in wine comprises the following steps:
(1) preparing sodium carboxymethylcellulose solutions with different concentration gradients by using deionized water, respectively placing the sodium carboxymethylcellulose solutions with different concentrations in a dialysis bag for dialysis for 15h, then placing in a glass test tube with a plug, adding a 2, 7-dihydroxynaphthalene solution, uniformly mixing in a vortex manner, placing in a boiling water bath for 2.5h, shaking the test tube at intervals of 0.5h, cooling to room temperature after the reaction is finished, adjusting to zero by taking 0mg/L reaction solution as a blank, and respectively measuring absorbance values A at 420nm and 540nm 420 And A 540 The absorbance difference Delta (A) is plotted on the abscissa by the concentration of the standard working solution 540 -A 420 ) As ordinate, a calibration curve L of the sodium carboxymethylcellulose concentration is plotted 1 Wherein the volume ratio of the sodium carboxymethylcellulose solution after dialysis to the 2, 7-dihydroxynaphthalene solution is 1: 9;
(2) preparing MI reagent solutions with different concentration gradients, respectively placing the MI reagent solutions with different concentrations in a glass test tube with a plug, sequentially adding a reagent A, uniformly mixing in a vortex mode, placing in a water bath at 25 ℃ for reaction for 10min, sequentially adding a Folin phenol reagent, uniformly mixing within 2s, reacting in the water bath at 25 ℃ for 30min, adjusting to zero by using water, and drawing a standard curve L of the MI reagent by taking the MI reagent concentration as an abscissa and the light absorption value at 640nm as an ordinate 2 Wherein the volume ratio of the MI reagent solution to the first reagent to the second reagent is 5:5: 1;
(3) preparing MI reagent solutions with different concentration gradients, respectively placing the MI reagent solutions with different concentrations into a glass test tube with a plug, sequentially adding a 2, 7-dihydroxynaphthalene solution, uniformly mixing in a vortex manner, placing the mixture into a boiling water bath for 2.5 hours, shaking the test tube at intervals of 0.5 hour, cooling to room temperature after the reaction is finished, zeroing by taking 0mg/L reaction liquid as a blank, taking the MI reagent concentration as an abscissa and taking light absorption values at 420nm and 540nm as ordinate, and drawing MI reagent standard curves L under 420nm and 540nm 3 、L 4 Wherein the MI reagent solution,The volume ratio of the 2, 7-dihydroxynaphthalene solution is 1: 9;
(4) when the grape wine is white grape wine, firstly, the pH value of the white grape wine sample is adjusted to 2-3 by concentrated hydrochloric acid, then the white grape wine sample is put into a centrifuge tube, absolute ethyl alcohol is added into the centrifuge tube, the centrifuge tube is swirled and then stands for 30min, the white grape wine sample is centrifuged for 15min at the rotating speed of 12000r/min, liquid is removed, the white grape wine sample is drained, water is added for redissolving and precipitating, the redissolved liquid is transferred into a dialysis bag, the dialysis bag is placed into water for dialysis for 15h to obtain white grape wine to-be-detected liquid, the white grape wine to-be-detected liquid is placed into a glass test tube with a plug, 2, 7-dihydroxynaphthalene solution is added, the reaction conditions are the same as the step (1), and the absorbance values A at 420nm and 540nm are respectively measured 420 I and A 540 II, comparing the absorbance difference delta (A) 420 Ⅰ-A 540 II) substitution into L 1 Obtaining the concentration of sodium carboxymethylcellulose in the sample, and performing parallel determination for at least two times, wherein the volume ratio of the white wine sample, the absolute ethyl alcohol, the redissolving water and the dialysis water is 1:9:1:1000, and the volume ratio of the white wine to-be-detected liquid and the 2, 7-dihydroxynaphthalene solution is 1: 9;
(5) when the wine is red wine or pink wine, the preparation method of the wine to be detected and the step of centrifuging, redissolving and precipitating in the step (4) are carried out twice, finally the wine to be detected is obtained, the wine to be detected is placed in a glass test tube with a plug, 2, 7-dihydroxynaphthalene solution is added, the reaction conditions are the same as the step (1), and the light absorption values A at 420nm and 540nm are respectively measured 420 III and A 540 IV, taking the wine to-be-detected liquid again, placing the wine to-be-detected liquid in a glass test tube with a plug, adding the reagent A, performing vortex mixing, placing in a water bath at 25 ℃ for reacting for 10min, sequentially adding the folin phenol reagent, mixing within 2s, performing reaction in the water bath at 25 ℃ for 30min, adjusting zero with water to obtain an absorbance value at the wavelength of 640nm, and substituting the absorbance value into the standard curve L 2 The concentration C of the sample corresponding to the MI reagent is obtained, and C is respectively substituted into the standard curve L 3 、L 4 The obtained sample corresponds to the light absorption value A of the MI reagent at the wavelengths of 420nm and 540nm 420 V and A 540 VI, calculating the difference Delta A between the light absorption values 420 ＝A 420 Ⅲ－A 420 Ⅴ、ΔA 540 ＝A 540 Ⅳ－A 540 VI, finding out the light absorption between different wavelengthsThe difference Δ ═ Δ a 540 -ΔA 420 Substituting Δ into the standard curve L 1 And (3) obtaining the concentration of the sodium carboxymethylcellulose to be detected in the sample, and performing parallel determination for at least two times, wherein the volume ratio of the wine sample, the absolute ethyl alcohol, the redissolution water and the dialysis water is 1:9:1:1000, the volume ratio of the wine to be detected to the 2, 7-dihydroxynaphthalene solution is 1:9, and the volume ratio of the wine to be detected to the reagent A and the Foregrin phenol reagent is 5:5: 1.
The concentration of the sodium carboxymethyl cellulose solution with different concentration gradients in the step (1) is 0.0mg/L, 10.0mg/L, 30.0mg/L, 50.0mg/L, 70.0mg/L and 90.0 mg/L.
The concentrations of the MI reagent solutions with different concentration gradients in the step (2) are 30mg/L, 60mg/L, 90mg/L, 120mg/L, 150mg/L and 300 mg/L.
Mixing an equal volume of 8% sodium carbonate solution and 0.4mol/L sodium hydroxide solution to obtain a reagent I, mixing an equal volume of 4% potassium sodium tartrate solution and 2% copper sulfate pentahydrate solution to obtain a reagent II, mixing the reagent I and the reagent II immediately, mixing the reagent I and the reagent II according to the volume ratio of 50:1, and quickly shaking uniformly to obtain the reagent A in the step (2).
The concentrations of the MI reagent solutions with different concentration gradients in the step (3) are 0mg/L, 120mg/L, 240mg/L, 360mg/L, 480mg/L and 600 mg/L.
The detection principle of the invention is as follows: the content can be calculated by adding MI reagent solution to settle sodium carboxymethylcellulose, dialyzing, centrifuging, separating sodium carboxymethylcellulose from wine, hydrolyzing sodium carboxymethylcellulose into glycolic acid in acidic medium (concentrated sulfuric acid), degrading glycolic acid to form formaldehyde, reacting with 2, 7-dihydroxynaphthalene in concentrated sulfuric acid at 100 deg.C to generate 2,2,7, 7-tetrahydroxy dinaphthyl methane with violet blue color, characteristic absorption at 540nm, and substituting into standard curve.
Cetyl pyridinium chloride in the MI reagent solution can settle sodium carboxymethyl cellulose.
Has the beneficial effects that: the method for detecting the content of sodium carboxymethylcellulose in wine provided by the invention has the following beneficial effects:
1. the detection method can detect the content of sodium carboxymethylcellulose in red wine and pink wine, and enlarges the detection range;
2. the detection method reduces detection limit and quantification limit in white wine detection;
3. the detection method shortens the detection time, improves the recovery rate and reduces the waste of water resources.
Detailed Description
The present invention is described in further detail below by way of specific embodiments, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention.
The reagents and materials used in the following examples are as follows:
sodium carboxymethylcellulose: the average viscosity is 400-1000 mPas, the substitution degree is 0.60-0.95, and the purity is more than or equal to 99%;
2, 7-dihydroxynaphthalene: the chromatogram is pure, and the purity is more than or equal to 98 percent;
concentrated sulfuric acid;
absolute ethyl alcohol;
folin phenol reagent: the concentration is 1 mol/L.
0.05% (mass concentration) 2, 7-dihydroxynaphthalene solution: weighing 0.500g of 2, 7-dihydroxynaphthalene, diluting to 1L with concentrated sulfuric acid, placing in a water bath at 28 ℃ in a dark place for 4h (normally, light blue gray, if reddish, re-preparation is needed), transferring to a brown reagent bottle, and storing at 4 ℃ for 1 month.
0.2mol/L sodium chloride solution: weighing 11.7g of sodium chloride, and fixing the volume to 1L by using water; 0.4mol/L sodium hydroxide solution: weighing 16.0g of sodium hydroxide, and adding water to a constant volume of 1L; 8% (mass concentration) sodium carbonate solution: weighing 80.0g of sodium carbonate, and fixing the volume to 1L by using water; 0.05mol/L hydrochloric acid: taking 4.17mL of concentrated hydrochloric acid (mass fraction: 37.5%), and adding water to a constant volume of 1L; 4% (mass concentration) potassium sodium tartrate solution: weighing 4.0g of sodium potassium tartrate, and adding water to a constant volume of 100 mL; 2% (mass concentration) copper sulfate pentahydrate solution: weighing 2.0g of blue vitriol, and fixing the volume to 100mL by using water; 0.1% cetylpyridinium chloride solution: 1.0g of cetylpyridinium chloride was weighed out and made to volume of 1L with sodium chloride solution (0.2 mol/L).
Cetyl pyridinium chloride: c 21 H 38 ClN·H 2 O, the purity is more than or equal to 99 percent;
reagent A: mixing the equal volume of 0.4mol/L sodium hydroxide solution and 8% sodium carbonate solution to obtain a reagent I, and preparing and using the reagent I; mixing the equal volume of the 4% potassium sodium tartrate solution and the 2% copper sulfate pentahydrate solution to obtain a reagent II, and preparing the reagent II for use; and uniformly mixing the reagent I and the reagent II according to the volume ratio of 50:1 to obtain a reagent A, wherein the effective period is 1 day.
Sodium carboxymethylcellulose standard stock solution: weighing 0.1000g of sodium carboxymethylcellulose in a 100mL volumetric flask, adding 2/3 volumes of water, placing in a water bath at 25 ℃, completely dissolving, and then fixing the volume with water, namely, the concentration of a stock solution is 1mg/mL, storing at 4 ℃, and the validity period is 1 month.
Sodium carboxymethyl cellulose solution: respectively sucking 0mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL of sodium carboxymethylcellulose stock solution, diluting to 100mL with water, respectively setting the corresponding solution mass concentrations to be 0mg/L, 10.0mg/L, 20.0mg/L, 30.0mg/L, 40.0mg/L and 50.0mg/L, storing at 4 ℃ and keeping the effective period for 1 month.
MI reagent: taking 1.0mL of a wine sample (bubbling wine needs ultrasonic degassing for 5.0min), adding 1.5mL of 0.1% cetylpyridinium chloride solution, uniformly mixing, standing for 20min at room temperature, adding absolute ethyl alcohol until the volume fraction of the ethyl alcohol in the mixed solution is 65%, standing for 15min, centrifuging for 15min at the rotating speed of 9000r/min, discarding all the liquid, draining, redissolving a precipitate by using 2.0mL of 0.05mol/L hydrochloric acid solution, transferring the redissolved precipitate into a dialysis bag, dialyzing for 15h in 2.0L of water, concentrating the dialyzed sample under reduced pressure until the sample is nearly dry, and drying in vacuum until the weight is constant to obtain MI; then 0.100g of MI is weighed, the volume is determined to be 100mL by water, and the mixture is stored at 4 ℃ with the validity period of 1 month. Red wine (pink wine) and white wine need to be prepared separately.
MI reagent solution: respectively sucking 0mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL and 10.00mL of matrix interfering substance mother liquor, diluting to 100mL with water, respectively setting the corresponding mass concentrations to 0mg/L, 20.0mg/L, 40.0mg/L, 60.0mg/L, 80.0mg/L and 100.0mg/L, storing at 4 ℃, and keeping the validity period for 1 month.
Dialysis bag (molecular weight cut-off 6000-8000 Da, MD: 44 mm): cutting into small segments with length of 8.0 + -0.5 cm before use, adding appropriate amount of water, boiling for 10min, changing water, and storing at 4 deg.C.
Instruments and equipment: an ultraviolet spectrophotometer; a centrifuge; a constant-temperature water bath kettle; an electronic balance; a vortex mixer; a rotary evaporator.
Example 1
And (3) detecting the content of sodium carboxymethylcellulose in the dry white wine.
Take 1.0mL (V) 1 1500mL) of dry white wine sample is put into a 10mL centrifuge tube, 1.5mL of 0.1% cetylpyridinium chloride solution is added, the mixture is evenly mixed and kept stand for 20min at room temperature, 5.0mL of absolute ethyl alcohol is added, the mixture is kept stand for 15min, 9000r/min is centrifuged for 15min, all liquid is discarded, precipitate is redissolved by 2.0mL of 0.05mol/L hydrochloric acid solution and is transferred into a dialysis bag, 2.0L of water is dialyzed for 15h, the dialyzed sample is transferred into a test tube, and the recorded volume is recorded as V 2 ＝1750mL。
Taking 2.0mL of standard working solution of sodium carboxymethylcellulose with series concentration, dialyzing in 2.0L of water for 15h, taking 0.5mL of dialyzed working solution, adding 4.5mL of 0.05% 2, 7-dihydroxynaphthalene solution into a 20mL glass test tube with a plug, uniformly mixing by vortex, placing in a boiling water bath for 2.0h, shaking the test tube every 0.5h in the period, and cooling to room temperature after the reaction is finished. Adjusting to zero with 0mg/L reaction solution, and measuring absorbance A at 420nm and 540nm respectively 420 And A 540 The absorbance difference Delta (A) is plotted on the abscissa by the concentration of the standard working solution 540 -A 420 ) As an ordinate, a standard curve L of sodium carboxymethylcellulose is plotted 1 (y＝0.004 2x-0.000 8)。
Taking 0.50mL of series MI working solution, supplementing water to 1.0mL, sequentially adding 1.0mL of reagent A, uniformly mixing by vortex, reacting in a water bath at 25 ℃ for 10min, sequentially adding 0.2mL of Fulinfen reagent, uniformly mixing within 2s, reacting in a water bath at 25 ℃ for 30min, adjusting zero by using 0mg/L of reaction solution, taking MI concentration as a horizontal coordinate and an absorbance value at 640nm as a vertical coordinate, and drawing a working curve L 2 (y＝0.001 5x-0.000 6)。
Adding 0.50mL of series MI working solution into 20mL of glass test tube with plug, sequentially adding 4.5mL of 2, 7-dihydroxynaphthalene solution, back-vortex mixing, and placingThe reaction solution is put in a boiling water bath for 2.0h, the test tube is shaken every 0.5h in the period, and the reaction solution is cooled to room temperature after the reaction is finished; zeroing the reaction solution at 0mg/L, plotting MI concentration as abscissa and absorbance values at 420nm and 540nm as ordinate respectively to obtain working curves L at 420nm and 540nm 3 (y ═ 0.0017 x-0.0012) and L 4 (y＝0.002 9x-0.002 4)。
Taking 0.5mL of dialyzed sample, adding 4.5mL of 2, 7-dihydroxynaphthalene solution into a 20mL glass test tube with a plug, back-swirling, mixing uniformly, placing in a boiling water bath for 2.0h, shaking the test tube every 0.5h, cooling to room temperature after the reaction is finished, and obtaining light absorption values A at 420nm and 540nm respectively 1 0.355 and a 2 ＝0.464。
Taking 0.5mL of dialyzed sample, adding 1.0mL of reagent A, vortex uniformly mixing, reacting for 10min in water bath at 25 ℃, then sequentially adding 0.2mL of Folin phenol reagent, mixing uniformly within 2s, reacting for 30min in water bath at 25 ℃, zeroing with 0mg/L of reaction liquid, measuring the absorbance value at the wavelength of 640nm, and substituting into a standard curve L 2 To obtain a matrix interference concentration C corresponding to MI in the sample MI Mixing C with MI Respectively substituted into the standard curve L 3 、L 4 Obtaining the absorbance A of matrix interference in the sample at the wavelengths of 420nm and 540nm 3 ＝0.0605、A 4 ＝0.1028。
Calculating the difference between the absorbance at the same wavelength of the matrix interference in the test sample and the sample (A) 1 -A 3 ) And (A) 2 -A 4 ) Respectively denoted as Δ A 420 And Δ A 540 Then, the absorbance difference Δ ═ Δ A is determined 540 -ΔA 420 When equal to 0.06668, Δ is substituted into the standard curve L 1 The concentration c of the analyte in the dialyzed sample was 18.7444 mg/L, which is less than the limit of quantitation, by volume conversion, and it was judged that sodium carboxymethylcellulose was added to the wine sample, but it was not quantitated.
According to the above operation steps, the addition experiment was performed simultaneously, and the recovery rate was 78.7%.
Example 2
And (3) detecting the content of sodium carboxymethylcellulose in the dry red wine.
Take 1.0mL (V) 1 1500mL) dry red wine sample in a 10mL centrifuge tube, addAdding 1.5mL of 0.1% cetylpyridinium chloride solution, uniformly mixing, standing at room temperature for 20min, adding 5.0mL of absolute ethyl alcohol, standing for 15min, centrifuging at 9000r/min for 15min, discarding all liquid, redissolving the precipitate with 2.0mL of 0.05mol/L hydrochloric acid solution, transferring into a dialysis bag, dialyzing in 2.0L of water for 15h, transferring the dialyzed sample into a test tube, and recording the volume as V 2 ＝1 500mL。
Taking 2.0mL of standard working solution of sodium carboxymethylcellulose with series concentration, dialyzing in 2.0L of water for 15h, taking 0.5mL of dialyzed working solution, adding 4.5mL of 0.05% 2, 7-dihydroxynaphthalene solution into a 20mL glass test tube with a plug, uniformly mixing by vortex, placing in a boiling water bath for 2.0h, shaking the test tube every 0.5h in the period, and cooling to room temperature after the reaction is finished. Adjusting to zero with 0mg/L reaction solution, and measuring absorbance A at 420nm and 540nm respectively 420 And A 540 The absorbance difference Delta (A) is plotted on the abscissa by the concentration of the standard working solution 540 -A 420 ) Drawing a standard curve L of sodium carboxymethylcellulose as an ordinate 1 (y＝0.004 2x-0.000 8)。
Taking 0.50mL of series MI working solution, supplementing water to 1.0mL, sequentially adding 1.0mL of reagent A, uniformly mixing by vortex, reacting in a water bath at 25 ℃ for 10min, sequentially adding 0.2mL of Fulinfen reagent, uniformly mixing within 2s, reacting in a water bath at 25 ℃ for 30min, adjusting zero by using 0mg/L of reaction solution, taking MI concentration as a horizontal coordinate and an absorbance value at 640nm as a vertical coordinate, and drawing a working curve L 2 (y＝0.002 2x+0.002 1)。
Then taking 0.50mL of series MI working solution into a 20mL glass test tube with a plug, sequentially adding 4.5mL of 2, 7-dihydroxynaphthalene solution, carrying out back vortex mixing, placing in a boiling water bath for 2.0h, shaking the test tube every 0.5h, and cooling to room temperature after the reaction is finished; zeroing the reaction solution at 0mg/L, plotting MI concentration as abscissa and absorbance values at 420nm and 540nm as ordinate respectively to obtain working curves L at 420nm and 540nm 3 (y ═ 0.0024 x-0.0002) and L 4 (y＝0.003 5x-0.007 1)。
Taking 0.5mL of dialyzed sample, adding 4.5mL of 2, 7-dihydroxynaphthalene solution into a 20mL glass test tube with a plug, back-swirling, mixing uniformly, placing in a boiling water bath for 2.0h, shaking the test tube every 0.5h, cooling to room temperature after the reaction is finished, and obtaining light absorption values A at 420nm and 540nm respectively 1 ＝0.588 and A 2 ＝0.722。
Taking 0.5mL of dialyzed sample, adding 1.0mL of reagent A, uniformly mixing by vortex, reacting in a water bath at 25 ℃ for 10min, sequentially adding 0.2mL of Folin phenol reagent, uniformly mixing within 2s, reacting in a water bath at 25 ℃ for 30min, adjusting to zero by 0mg/L of reaction liquid, measuring the absorbance at the wavelength of 640nm, substituting into a standard curve L 2 To obtain a matrix interference concentration C corresponding to MI in the sample MI Mixing C with MI Respectively substituted into the standard curve L 3 、L 4 Obtaining the absorbance A of matrix interference in the sample at the wavelengths of 420nm and 540nm 3 ＝0.1569、A 4 ＝0.2356。
Calculating the difference between the absorbance at the same wavelength of the matrix interference in the test sample and the sample (A) 1 -A 3 ) And (A) 2 -A 4 ) Respectively denoted as Δ A 420 And Δ A 540 And calculating the absorbance difference Delta A 540 -ΔA 420 When equal to 0.0553, Δ is substituted into the standard curve L 1 The concentration c of the analyte in the sample after dialysis was 13.3571mg/L, which was obtained by volume conversion, and it was judged that the analyte was not detected because the concentration did not reach the detection limit.
According to the above operation steps, the addition experiment was performed simultaneously, and the recovery rate was 88.1%.
Example 3
And (3) detecting the content of sodium carboxymethylcellulose in the dry red wine.
Take 1.0mL (V) 1 1500mL) of dry red wine sample is put into a 10mL centrifuge tube, 1.5mL of 0.1% cetylpyridinium chloride solution is added, the mixture is evenly mixed and kept stand for 20min at room temperature, 5.0mL of absolute ethyl alcohol is added, the mixture is kept stand for 15min, 9000r/min is centrifuged for 15min, all liquid is discarded, precipitate is redissolved by 2.0mL of 0.05mol/L hydrochloric acid solution and is transferred into a dialysis bag, 2.0L of water is dialyzed for 15h, the dialyzed sample is transferred into a test tube, and the recorded volume is recorded as V 2 ＝1 900mL。
Taking 2.0mL of standard working solution of sodium carboxymethylcellulose with series concentration, dialyzing in 2.0L of water for 15h, taking 0.5mL of dialyzed working solution, adding 4.5mL of 0.05% 2, 7-dihydroxynaphthalene solution into a 20mL glass test tube with a plug, uniformly mixing by vortex, placing in a boiling water bath for 2.0h, shaking the test tube every 0.5h in the period, and reactingThen cooling to room temperature. Adjusting to zero with 0mg/L reaction solution, and measuring absorbance A at 420nm and 540nm respectively 420 And A 540 The absorbance difference Delta (A) is plotted on the abscissa by the concentration of the standard working solution 540 -A 420 ) Drawing a standard curve L of sodium carboxymethylcellulose as an ordinate 1 (y＝0.004 2x-0.000 8)。
Taking 0.50mL of series MI working solution, supplementing water to 1.0mL, sequentially adding 1.0mL of reagent A, uniformly mixing by vortex, reacting in a water bath at 25 ℃ for 10min, sequentially adding 0.2mL of Fulinfen reagent, uniformly mixing within 2s, reacting in a water bath at 25 ℃ for 30min, adjusting zero by using 0mg/L of reaction solution, taking MI concentration as a horizontal coordinate and an absorbance value at 640nm as a vertical coordinate, and drawing a working curve L 2 (y＝0.002 2x+0.002 1)。
Then taking 0.50mL of series MI working solution into a 20mL glass test tube with a plug, sequentially adding 4.5mL of 2, 7-dihydroxynaphthalene solution, carrying out back vortex mixing, placing in a boiling water bath for 2.0h, shaking the test tube every 0.5h, and cooling to room temperature after the reaction is finished; zeroing the reaction solution at 0mg/L, plotting MI concentration as abscissa and absorbance values at 420nm and 540nm as ordinate respectively to obtain working curves L at 420nm and 540nm 3 (y ═ 0.0024 x-0.0002) and L 4 (y＝0.003 5x-0.007 1)。
Taking 0.5mL of dialyzed sample, adding 4.5mL of 2, 7-dihydroxynaphthalene solution into a 20mL glass test tube with a plug, back-swirling, mixing uniformly, placing in a boiling water bath for 2.0h, shaking the test tube every 0.5h, cooling to room temperature after the reaction is finished, and obtaining light absorption values A at 420nm and 540nm respectively 1 0.564 and A 2 ＝0.817。
Taking 0.5mL of dialyzed sample, adding 1.0mL of reagent A, uniformly mixing by vortex, reacting in a water bath at 25 ℃ for 10min, sequentially adding 0.2mL of Folin phenol reagent, uniformly mixing within 2s, reacting in a water bath at 25 ℃ for 30min, adjusting to zero by 0mg/L of reaction liquid, measuring the absorbance at the wavelength of 640nm, substituting into a standard curve L 2 To obtain a matrix interference concentration C corresponding to MI in the sample MI And C is prepared by MI Respectively substituted into the standard curve L 3 、L 4 Obtaining the absorbance A of matrix interference in the sample at the wavelengths of 420nm and 540nm 3 ＝0.1219、A 4 ＝0.1846。
Calculating test samplesAnd the difference between the absorbance of the sample at the same wavelength of the matrix interference (A) 1 -A 3 ) And (A) 2 -A 4 ) Respectively denoted as Δ A 420 And Δ A 540 And calculating the absorbance difference Delta A 540 -ΔA 420 When equal to 0.0627, Δ is substituted into the standard curve L 1 The concentration c of the analyte in the sample after dialysis was 57.6333mg/L, which exceeds the detection limit but does not reach the quantification limit, and it was determined that sodium carboxymethylcellulose was added to the wine sample and could not be quantified.
According to the above operation steps, the addition experiment was performed simultaneously, and the recovery rate was 86.3%.
Example 4
And (3) detecting the content of sodium carboxymethylcellulose in the dry red wine.
Take 1.0mL (V) 1 1500mL) of dry red wine sample is put into a 10mL centrifuge tube, 1.5mL of 0.1% cetylpyridinium chloride solution is added, the mixture is evenly mixed and kept stand for 20min at room temperature, 5.0mL of absolute ethyl alcohol is added, the mixture is kept stand for 15min, 9000r/min is centrifuged for 15min, all liquid is discarded, precipitate is redissolved by 2.0mL of 0.05mol/L hydrochloric acid solution and is transferred into a dialysis bag, 2.0L of water is dialyzed for 15h, the dialyzed sample is transferred into a test tube, and the recorded volume is recorded as V 2 ＝1 750mL。
Taking 2.0mL of standard working solution of sodium carboxymethylcellulose with series concentration, dialyzing in 2.0L of water for 15h, taking 0.5mL of dialyzed working solution, adding 4.5mL of 0.05% 2, 7-dihydroxynaphthalene solution into a 20mL glass test tube with a plug, uniformly mixing by vortex, placing in a boiling water bath for 2.0h, shaking the test tube every 0.5h in the period, and cooling to room temperature after the reaction is finished. Adjusting to zero with 0mg/L reaction solution, and measuring absorbance A at 420nm and 540nm respectively 420 And A 540 The absorbance difference Delta (A) is plotted on the abscissa by the concentration of the standard working solution 540 -A 420 ) Drawing a standard curve L of sodium carboxymethylcellulose as an ordinate 1 (y＝0.004 2x-0.000 8)。
Taking 0.50mL of series MI working solution, supplementing water to 1.0mL, sequentially adding 1.0mL of reagent A, mixing uniformly in a vortex mode, reacting for 10min in a water bath at 25 ℃, sequentially adding 0.2mL of Folin phenol reagent, mixing uniformly within 2s, reacting for 30min in a water bath at 25 ℃, and reacting with 0mg/L of reaction solutionZeroing, taking MI concentration as abscissa and light absorption value at 640nm as ordinate, and drawing working curve L 2 (y＝0.001 8x+0.008 1)。
Then taking 0.50mL of series MI working solution into a 20mL glass test tube with a plug, sequentially adding 4.5mL of 2, 7-dihydroxynaphthalene solution, carrying out back vortex mixing, placing in a boiling water bath for 2.0h, shaking the test tube every 0.5h, and cooling to room temperature after the reaction is finished; zeroing the reaction solution at 0mg/L, plotting MI concentration as abscissa and absorbance values at 420nm and 540nm as ordinate respectively to obtain working curves L at 420nm and 540nm 3 (y-0.0021 x-0.0022) and L 4 (y＝0.003 2x-0.001 7)。
Taking 0.5mL of dialyzed sample, adding 4.5mL of 2, 7-dihydroxynaphthalene solution into a 20mL glass test tube with a plug, back-swirling, mixing uniformly, placing in a boiling water bath for 2.0h, shaking the test tube every 0.5h, cooling to room temperature after the reaction is finished, and obtaining light absorption values A at 420nm and 540nm respectively 1 0.376 and A 2 ＝0.44。
Taking 0.5mL of dialyzed sample, adding 1.0mL of reagent A, uniformly mixing by vortex, reacting in a water bath at 25 ℃ for 10min, sequentially adding 0.2mL of Folin phenol reagent, uniformly mixing within 2s, reacting in a water bath at 25 ℃ for 30min, adjusting to zero by 0mg/L of reaction liquid, measuring the absorbance at the wavelength of 640nm, substituting into a standard curve L 2 To obtain a matrix interference concentration C corresponding to MI in the sample MI Mixing C with MI Respectively substituted into the standard curve L 3 、L 4 Obtaining the absorbance A of matrix interference in the sample at the wavelengths of 420nm and 540nm 3 ＝0.044、A 4 ＝0.082。
Calculating the difference between the absorbance at the same wavelength of the matrix interference in the test sample and the sample (A) 1 -A 3 ) And (A) 2 -A 4 ) Respectively denoted as Δ A 420 And Δ A 540 Then, the absorbance difference Δ ═ Δ A is determined 540 -ΔA 420 When equal to 0.0248, Δ is substituted into the standard curve L 1 The concentration c of the analyte in the sample after dialysis was 6.7134mg/L, which was obtained by volume conversion, and it was not detected because the concentration c did not exceed the detection limit.
According to the above operation steps, the addition experiment was performed simultaneously, and the recovery rate was 87.3%.
While the embodiments of the present invention have been described in detail, those skilled in the art will recognize that the embodiments of the present invention can be practiced without departing from the spirit and scope of the claims.
Claims (4)
1. A method for detecting the content of sodium carboxymethylcellulose in wine is characterized by comprising the following steps:
(1) preparing sodium carboxymethylcellulose solutions with different concentration gradients by using deionized water, respectively placing the sodium carboxymethylcellulose solutions with different concentrations in a dialysis bag for dialysis for 15h, then placing in a glass test tube with a plug, adding a 2, 7-dihydroxynaphthalene solution, uniformly mixing in a vortex manner, placing in a boiling water bath for 2.5h, shaking the test tube at intervals of 0.5h, cooling to room temperature after the reaction is finished, adjusting to zero by taking 0mg/L reaction solution as a blank, and respectively measuring absorbance values A at 420nm and 540nm 420 And A 540 The absorbance difference Delta (A) is plotted on the abscissa by the concentration of the standard working solution 540 -A 420 ) As ordinate, a standard curve L of the sodium carboxymethylcellulose concentration is plotted 1 Wherein the volume ratio of the dialyzed sodium carboxymethylcellulose solution to the dialyzed 2, 7-dihydroxynaphthalene solution is 1: 9;
(2) preparing MI reagent solutions with different concentration gradients, respectively placing the MI reagent solutions with different concentrations in a glass test tube with a plug, sequentially adding a reagent A, uniformly mixing in a vortex mode, placing in a water bath at 25 ℃ for reaction for 10min, sequentially adding a Folin phenol reagent, uniformly mixing within 2s, reacting in the water bath at 25 ℃ for 30min, adjusting to zero by using water, and drawing a standard curve L of the MI reagent by taking the MI reagent concentration as an abscissa and the light absorption value at 640nm as an ordinate 2 Wherein the volume ratio of the MI reagent solution to the reagent A to the folin phenol reagent is 5:5:1,
the preparation method of the MI reagent comprises the following steps: taking 1.0mL of a wine sample, adding 1.5mL of 0.1% cetylpyridinium chloride solution, uniformly mixing, standing for 20min at room temperature, adding absolute ethyl alcohol until the volume fraction of the ethyl alcohol in the mixed solution is 65%, standing for 15min, centrifuging for 15min at the rotating speed of 9000r/min, discarding all liquid, draining, redissolving a precipitate by using 2.0mL of 0.05mol/L hydrochloric acid solution, transferring into a dialysis bag, dialyzing for 15h in 2.0L of water, concentrating the dialyzed sample under reduced pressure until the sample is nearly dry, and drying in vacuum until the MI is constant in weight to obtain the MI; then 0.100g of MI is weighed, water is used for fixing the volume to 100mL, and the compound preparation is obtained,
mixing an equal volume of 8% sodium carbonate solution and 0.4mol/L sodium hydroxide solution to obtain a reagent I, mixing an equal volume of 4% potassium sodium tartrate solution and 2% copper sulfate pentahydrate solution to obtain a reagent II, mixing the reagent I and the reagent II at a volume ratio of 50:1, and quickly shaking uniformly to obtain the reagent A;
(3) preparing MI reagent solutions with different concentration gradients, respectively placing the MI reagent solutions with different concentrations into a glass test tube with a plug, sequentially adding a 2, 7-dihydroxynaphthalene solution, uniformly mixing in a vortex manner, placing the mixture into a boiling water bath for 2.5 hours, shaking the test tube at intervals of 0.5 hour, cooling to room temperature after the reaction is finished, zeroing by taking 0mg/L reaction liquid as a blank, taking the MI reagent concentration as an abscissa and taking light absorption values at 420nm and 540nm as ordinate, and drawing MI reagent standard curves L under 420nm and 540nm 3 、L 4 Wherein the volume ratio of the MI reagent solution to the 2, 7-dihydroxynaphthalene solution is 1:9, and the preparation method of the MI reagent is the same as that in the step (2);
(4) when the grape wine is white grape wine, firstly, the pH value of the white grape wine sample is adjusted to 2-3 by concentrated hydrochloric acid, then the white grape wine sample is put into a centrifuge tube, absolute ethyl alcohol is added into the centrifuge tube, the centrifuge tube is swirled and then stands for 30min, the white grape wine sample is centrifuged for 15min at the rotating speed of 12000r/min, liquid is removed, the white grape wine sample is drained, water is added for redissolving and precipitating, the redissolved liquid is transferred into a dialysis bag, the dialysis bag is placed into water for dialysis for 15h to obtain white grape wine to-be-detected liquid, the white grape wine to-be-detected liquid is placed into a glass test tube with a plug, 2, 7-dihydroxynaphthalene solution is added, the reaction conditions are the same as the step (1), and the absorbance values A at 420nm and 540nm are respectively measured 420 I and A 540 II, comparing the absorbance difference delta (A) 420 Ⅰ-A 540 II) substitution into L 1 Obtaining the concentration of sodium carboxymethylcellulose in the sample, and performing parallel determination for at least two times, wherein the volume ratio of the white wine sample, the absolute ethyl alcohol, the redissolving water and the dialysis water is 1:9:1:1000, and the volume ratio of the white wine to-be-detected liquid and the 2, 7-dihydroxynaphthalene solution is 1: 9;
(5) when the wine is red wine or pink wine, the preparation method of the wine to be detected and the step of centrifuging, redissolving and precipitating in the step (4) are carried out twice, finally the wine to be detected is obtained, the wine to be detected is placed in a glass test tube with a plug, 2, 7-dihydroxynaphthalene solution is added, the reaction conditions are the same as the step (1), and the light absorption values A at 420nm and 540nm are respectively measured 420 III and A 540 IV, taking the wine to-be-detected liquid again, placing the wine to-be-detected liquid in a glass test tube with a plug, adding the reagent A, performing vortex mixing, placing in a water bath at 25 ℃ for reacting for 10min, sequentially adding the folin phenol reagent, mixing within 2s, performing reaction in the water bath at 25 ℃ for 30min, adjusting zero with water to obtain an absorbance value at the wavelength of 640nm, and substituting the absorbance value into the standard curve L 2 The concentration C of the sample corresponding to the MI reagent is obtained, and C is respectively substituted into the standard curve L 3 、L 4 The obtained sample corresponds to the light absorption value A of the MI reagent at the wavelengths of 420nm and 540nm 420 V and A 540 VI, calculating the difference Delta A between the light absorption values 420 ＝A 420 Ⅲ－A 420 Ⅴ、ΔA 540 ＝A 540 Ⅳ－A 540 VI, obtaining the difference value delta between different wavelengths 540 -ΔA 420 Substituting Δ into the standard curve L 1 And (3) obtaining the concentration of the sodium carboxymethylcellulose to be detected in the sample, and performing parallel determination for at least two times, wherein the volume ratio of the wine sample, the absolute ethyl alcohol, the redissolution water and the dialysis water is 1:9:1:1000, the volume ratio of the wine to be detected to the 2, 7-dihydroxynaphthalene solution is 1:9, and the volume ratio of the wine to be detected to the reagent A and the Foregrin phenol reagent is 5:5: 1.
2. The method for detecting the content of sodium carboxymethylcellulose in wine according to claim 1, wherein the method comprises the following steps: the concentration of the sodium carboxymethyl cellulose solution with different concentration gradients in the step (1) is 0.0mg/L, 10.0mg/L, 30.0mg/L, 50.0mg/L, 70.0mg/L and 90.0 mg/L.
3. The method for detecting the content of sodium carboxymethylcellulose in wine according to claim 1, wherein the method comprises the following steps: the MI reagent solutions with different concentration gradients in the step (2) have the concentrations of 30mg/L, 60mg/L, 90mg/L, 120mg/L, 150mg/L and 300 mg/L.
4. The method for detecting the content of sodium carboxymethylcellulose in wine according to claim 1, wherein the method comprises the following steps: the MI reagent solutions with different concentration gradients in the step (3) have the concentrations of 0mg/L, 120mg/L, 240mg/L, 360mg/L, 480mg/L and 600 mg/L.
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