CN111443141B - Method for detecting content of effective components in health wine - Google Patents
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Abstract
The invention provides a method for detecting the content of effective components in health-care wine, which comprises the following steps: detecting by using a gas chromatography-mass spectrometer, and calculating to obtain the content of the effective components based on a standard curve method; the pretreatment of the sample specifically comprises the following steps: mixing a health wine sample to be detected with an isotope internal standard substance of effective components and water, adding sodium chloride until the solution is saturated, and extracting with an organic solvent to obtain a sample solution. The invention adopts gas chromatography-mass spectrometry for detection, takes the isotope of the effective component as an internal standard substance, improves the pretreatment of the sample, can effectively reduce the error and ensure the accuracy of the detection result. The method can simultaneously detect a plurality of effective components in the health care wine, has the detection limit of 11.73-75.75 mug/L, and has the advantages of wide application range, simple and convenient operation, low detection limit and high accuracy.
Description
Technical Field
The invention belongs to the field of health wine detection, and particularly relates to a method for detecting the content of effective components in health wine.
Background
The health wine is a kind of alcoholic beverage with changed original wine style, which is made by blending, mixing or reprocessing distilled wine, fermented wine or edible alcohol as wine base and edible or medicinal and edible auxiliary materials or food additives. The health care wine has health care function for human body, is suitable for specific people to eat, and has the function of regulating organism, but does not aim at treatment.
The health wine usually comprises linalool, camphor, cinnamaldehyde, borneol acetate, eugenol, ligustilide and other effective components, the specific content of the effective components is one of important indexes for evaluating the quality of the health wine, but no related effective component standard determination method exists in the health wine industry at present.
Compared with the detection of the effective components in the medicinal materials, the detection difficulty of the effective components in the health-care wine is obviously increased. The medicinal materials do not have organic solvent interference, the content can be detected after the medicinal materials are directly extracted by adopting an organic solvent with matched polarity, and the method is simple. However, the health-care wine contains a large amount of ethanol and water, active ingredients are dissolved in the solvent system, the ethanol and the water belong to solvents with large expansion coefficients, particularly, the water cannot be directly subjected to mass spectrometry, so that the ethanol and the water system must be replaced by proper solvents, the active ingredients have distribution problems in the solvent replacement process, and the replacement solvents cannot completely extract the active ingredients; in addition, the health wine generally contains macromolecular compounds such as sugar and pigment, and these substances also affect the replacement efficiency of the solvent.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for detecting the content of effective components in health-care wine.
The invention provides a method for detecting the content of effective components in health-care wine, which comprises the following steps: detecting by using a gas chromatography-mass spectrometer, and calculating to obtain the content of the effective components based on a standard curve method;
the pretreatment of the sample specifically comprises the following steps: mixing a health wine sample to be detected with an isotope internal standard substance of effective components and water, adding sodium chloride until the solution is saturated, and extracting with an organic solvent to obtain a sample solution.
The invention aims at the effective components in the health care wine, adopts a gas chromatography-mass spectrometer for analysis and detection, does not have the problems of easy occurrence of ghost peaks, small response value, large interference and incapability of accurate quantification in gas chromatography detection, and also does not have the problem of poor resolution of liquid chromatography, adopts gas chromatography-mass spectrometry for combination, and carries out quantification by selecting characteristic ion peaks, so that the result is quicker and more accurate.
According to the invention, the isotope of the effective component is used as the internal standard substance during sample pretreatment, the property and the distribution coefficient of the internal standard substance are basically consistent with those of the effective component to be detected, and the internal standard substance is used as a reference standard, so that the detection error can be reduced. In addition, the ethanol concentration in the system is diluted by adding water, and then sodium chloride is added to saturate the ethanol aqueous solution, so that the polarity of the aqueous solution is improved, the effective components are promoted to be transferred into the extracting agent, and the extraction efficiency is improved; and the method of liquid-liquid micro-extraction is adopted, only a small amount of organic solvent is used for extraction, the usage amount of the organic solvent is greatly reduced, the cost is reduced, and the pollution to the environment is reduced.
Further, the organic solvent is diethyl ether. The extraction effect and the on-machine detection effect of the ether are better, and the detection result is more accurate.
Further, the dosage ratio of the health wine sample to be tested, the isotope internal standard substance and water is 3-5 mL: 5-10 mug: 5-20 mL; the volume ratio of the health wine sample to be tested to the diethyl ether is 2: 1.
Further, the preparation of the standard solution specifically comprises: mixing a wine base, water, white granulated sugar and caramel pigment corresponding to the health-care wine sample to be detected to prepare a reference simulation solution with the alcoholic strength, sugar content and light transmittance consistent with those of the health-care wine sample to be detected;
and dissolving an effective component standard substance by using the reference simulated liquid as a solvent, and treating the obtained solution according to the method for treating the health-care wine sample to be detected to obtain the sample solution to obtain the standard solution.
The invention adopts the same solvent system as the health care wine sample to be tested to prepare the standard solution, which is beneficial to eliminating the matrix effect and reducing the error.
Further, when a standard curve is established, the ratio of the chromatographic peak area of the effective component in the standard solution to the chromatographic peak area of the internal standard substance is taken as the ordinate, and the ratio of the concentration of the effective component in the standard solution to the concentration of the internal standard substance is taken as the abscissa.
Further, the effective components are one or more of linalool, camphor, cinnamaldehyde, bornyl acetate, eugenol and ligustilide.
The health wine comprises common health wine in the market, such as strong wine, Coco island deer tortoise wine and the like. The method of the invention can detect one effective component in the health wine and can also detect a plurality of effective components simultaneously. Preferably, when one or more of the 6 effective components are detected, the effect is better, namely, the detection repeatability is good, the sensitivity is high, and the result is more accurate.
When the effective component is one, the isotope internal standard substance is preferably an isotope corresponding to the effective component; when the active ingredients are multiple, the isotope internal standard substance is preferably a eugenol isotope, so that the reagent source and the detection result accuracy are both considered.
Further, the eugenol isotope is eugenol-d3Namely deuterated eugenol.
Further wherein the gas chromatography detection conditions comprise:
the stationary phase of the chromatographic column is (5% -phenyl) -methyl polysiloxane, preferably a chromatographic column with the thickness of 30m multiplied by 0.25mm (inner diameter) multiplied by 0.25 mu m (film thickness) or equivalent performance; the temperature of a sample inlet is 280 ℃, the split ratio is 10:1, the constant flow mode is adopted, the flow rate is 1.5mL/min, and the sample injection amount is 1 mu L; the carrier gas is high-purity helium with the purity more than or equal to 99.999 percent; the initial column temperature is 50 deg.C, maintained for 5min, increased to 180 deg.C at 3.5 deg.C/min, increased to 320 deg.C at 30 deg.C/min, and maintained for 10 min.
Further wherein the mass spectrometric detection conditions comprise:
ionization mode: electron bombardment source with energy of 70 eV; temperature of the quadrupole rods: 150 ℃; ion source temperature: 230 ℃; solvent retardation: 5 min; the detection mode is as follows: and selecting ion scanning and collecting.
In a preferred embodiment of the present invention, the method specifically comprises:
a. mixing the health liquor sample to be tested with eugenol-d3Mixing the mixture with water according to the proportion of 3-5 mL to 5-10 mug to 5-20 mL to obtain a mixed solution, adding sodium chloride into the mixed solution until the mixed solution is saturated, then extracting the mixed solution with ether, wherein the volume of the ether is half of that of the sample of the health wine to be detected, and performing centrifugal separation to collect supernatant to obtain a sample solution;
b. mixing a wine base, water, white granulated sugar and caramel pigment corresponding to the health-care wine sample to be detected to prepare a reference simulation solution with the alcoholic strength, sugar content and light transmittance consistent with those of the health-care wine sample to be detected; dissolving an effective component standard substance by using the reference simulated liquid as a solvent, and processing the obtained solution according to the step a to obtain a standard solution;
c. respectively carrying out gas chromatography-mass spectrometry detection analysis on the sample solution obtained in the step a and the standard solution obtained in the step b;
d. mixing the effective components in standard solution with eugenol-d3The ratio of the chromatographic peak area of the extract to the chromatographic peak area of the eugenol-d is ordinate3The concentration ratio of (A) is an abscissa, and a standard curve is established;
e. mixing the effective components with eugenol-d in the sample solution3Substituting the chromatographic peak area ratio into a standard curve to calculate the content of the effective components in the health wine sample to be measured.
Further, during centrifugal separation, the mixture is centrifuged at 8000-10000 rpm for 7-10 min.
The invention has the beneficial effects that:
the invention adopts a gas chromatography-mass spectrometer for detection, takes the isotope of the effective component as an internal standard substance, improves the pretreatment of the sample, can effectively reduce the error and ensure the accuracy of the detection result. The method can simultaneously detect a plurality of effective components in the health care wine, has the detection limit of 11.73-75.75 mug/L, and has the advantages of wide application range, simple and convenient operation, low detection limit and high accuracy.
Drawings
FIG. 1 is a mass spectrum of a 6-effective-component mixed standard solution and an internal standard solution in example 1;
FIG. 2 is a graph of the linalool standard of example 1;
FIG. 3 is a graph showing the standard curve of camphor in example 1;
FIG. 4 is a cinnamaldehyde standard curve in example 1;
FIG. 5 is a graph of a standard bornyl acetate in example 1;
FIG. 6 is a standard graph of eugenol in example 1;
figure 7 is a graph of the standard ligustilide profile of example 1;
FIG. 8 is a mass spectrum of the sample (1) for testing the health wine in example 1;
FIG. 9 is a mass spectrum of the recovery rate test of the sample to be tested (1) of the health wine in example 1;
FIG. 10 is a mass spectrum of the sample (2) for testing health wine in example 2;
FIG. 11 is a mass spectrum of the sample (3) for testing health wine in example 3.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The reagents or instruments used are conventional products available from regular distributors, not indicated by the manufacturer.
Example 1
The embodiment provides a method for detecting the content of effective components (including linalool, camphor, cinnamaldehyde, bornyl acetate, eugenol and ligustilide) in health care wine, which comprises the following specific steps:
1. reagent
1.1 Anhydrous ethanol, Ether: carrying out chromatographic purification;
1.2 white granulated sugar, caramel pigment: and (4) food grade.
2. Sample to be tested and standard substance
Sample to be tested (1): chinese jin wine, alcohol content 35% (V/V), light transmittance 60%, offered by Jinpai limited;
linalool, camphor, cinnamaldehyde, bornyl acetate, eugenol and ligustilide standard substance: the purity is more than 97.8 percent, and the product is purchased from China institute for testing and testing food and drugs;
eugenol-d3And (3) standard substance: purity greater than 98.8% and purchased from TRC Canada.
3. Standard solution preparation
3.1 preparing an effective component single-standard stock solution: weighing appropriate amount of the above 6 effective component standard substances, placing in 10mL volumetric flask, dissolving with anhydrous ethanol to constant volume to scale to obtain single-standard stock solution of 6 effective components, and storing at-20 deg.C with specific concentration shown in Table 1.
3.2 preparing a standard simulation solution: absorbing 70mL of health wine base with the alcoholic strength of 50% (V/V) into a 100mL volumetric flask, adding 6g of white granulated sugar, shaking to dissolve, fixing the volume to a scale with water, adding caramel pigment to adjust the light transmittance to be 60%, so that the alcoholic strength, the sugar content and the light transmittance of the health wine base are consistent with those of a sample (1) to be detected, and storing at 4 ℃.
3.3 preparing an effective component mixed standard solution: absorbing single standard stock solutions of various active ingredients, using a standard simulation solution to fix the volume to 10mL, and storing at-20 ℃, wherein the specific concentration is shown in Table 1.
3.4 preparing an internal standard solution: weighing eugenol-d34mg, dissolving with absolute ethyl alcohol to a constant volume of 10mL to obtain 400mg/L eugenol-d3Internal standard solution is preserved at-20 ℃.
TABLE 16 individual and mixed standard concentrations of active ingredients
4. Sample processing procedure
Transferring 4mL of sample (1) to be detected into a 50mL centrifuge tube, and adding eugenol-d3Adding 10mL of water into 20 mu L of internal standard solution, adding 4g of sodium chloride, ultrasonically dissolving until saturation, adding 2mL of ether, performing vortex oscillation extraction for 1min, centrifuging for 5min at 8000r/min, sucking out 1mL of supernatant (namely sample solution) in a sample bottle, and performing GC/MS analysis.
5. Sample assay
5.1 apparatus conditions
Agilent 7890 and 5977B gas chromatography-mass spectrometer.
5.1.1 gas chromatography conditions
The stationary phase of the chromatographic column is (5% -phenyl) -methyl polysiloxane, and the stationary phase is a chromatographic column with the thickness of 30m multiplied by 0.25mm (inner diameter) multiplied by 0.25 mu m (film thickness) or equivalent performance; the temperature of a sample inlet is 280 ℃, the split ratio is 10:1, the constant flow mode is adopted, the flow rate is 1.5mL/min, and the sample injection amount is 1 mu L; the carrier gas is high-purity helium with the purity more than or equal to 99.999 percent; the initial column temperature is 50 deg.C, maintained for 5min, increased to 180 deg.C at 3.5 deg.C/min, increased to 320 deg.C at 30 deg.C/min, and maintained for 10 min.
5.1.2 Mass Spectrometry conditions
The ion source is an EI source, and the energy is 70 eV; the temperature of the quadrupole rods is 150 ℃; the ion source temperature is 230 ℃; the solvent delay was 5 min. The detection mode is selected ion scanning and collection; the monitoring ions are shown in Table 2.
Firstly, a full SCAN mode (SCAN) is adopted for qualitative analysis, instrument parameters are optimized, retention time and characteristic ions of each effective component and an internal standard substance are determined, then, compounds are grouped, and a Selective Ion Mode (SIM) is adopted for scanning detection, wherein the details are shown in a table 2.
The mass spectra of the 6 effective component mixed standard solution and the internal standard solution in this example are shown in fig. 1.
TABLE 26 gas chromatography-Mass Spectrometry parameters for active ingredients and internal standards
Remarking: ions are indicated in table 2.
5.2 preparation of Standard Curve
Taking 6 10mL volumetric flasks, respectively sucking 50 μ L, 100 μ L, 200 μ L, 500 μ L, 1000 μ L and 2000 μ L of the mixed standard solution containing the effective components in 3.3, diluting with 3.2 standard simulated solution to constant volume to scale, and preparing at the time of use.
Transferring 4mL of the prepared solution into 50mL centrifuge tubes, respectively, and adding eugenol-d 320 mu L of internal standard solution, 10mL of water, 4g of sodium chloride, ultrasonic dissolution, 2mL of ether, vortex oscillation extraction for 1min, centrifugation for 5min at 8000r/min, sucking out 1mL of supernatant in a sample bottle, making standard curves by taking the peak area ratio of the effective components and the internal standard substance as ordinate and the concentration ratio of the effective components and the internal standard substance as abscissa respectively after GC/MS analysis, wherein 6 effective component standard curve parameters are shown in Table 3, and 6 effective component standard curves are shown in figures 2-7.
Table 36 standard curve parameters of effective ingredients
5.3 determination
Measuring the sample solution and the standard solution under the same detection condition, and determining the mass spectrogram of the sample (1) to be detected as shown in FIG. 8, wherein the peak area A of the effective component is showniWith eugenol-d3Peak area of AfSubstituting into standard curve, and calculating content X of corresponding effective components in the samplei。
5.4 calculation of
The contents of 6 effective components in the sample are calculated according to the formula (1)
In the formula:
Xi- -the amount of the i-th active principle in the sample is in milligrams per liter or milligrams per kilogram (mg/L or mg/kg);
Xf- -eugenol-d in the sample3In milligrams per liter or milligrams per kilogram (mg/L or mg/kg);
Ai- -the area of the chromatographic peak of the i-th active ingredient in the sample;
Af- -eugenol-d in the sample3(ii) chromatographic peak area;
b- -intercept value of the standard curve;
k-slope of the standard curve.
The calculation results are expressed as the arithmetic mean of two independent measurements obtained under repetitive conditions, and are retained to the 3 th position after the decimal point.
6. Repeatability test
Taking 6 parts of the sample (1) to be tested, marking the sample as C-1-C-6, processing the sample solution according to the method, determining the content of the effective components, and calculating the repeatability of the determination results of the 6 effective components, wherein the RSD values are all less than 10 percent, which indicates that the method has good repeatability, and the specific calculation results are shown in Table 4.
Table 46 data results of the active ingredient reproducibility test
7. Limit of detection (LOD) and limit of quantitation (LOQ)
The limit of detection (LOD) is the corresponding sample concentration when the signal intensity (S)/baseline noise (N) is 3: 1;
the limit of quantitation (LOQ) is the sample concentration at which the signal intensity (S)/baseline noise (N) is 10: 1.
In this example, the detection Limit (LOD) of 6 kinds of active ingredients was 11.73. mu.g/L to 75.75. mu.g/L, the limit of quantitation (LOQ) was 39.10. mu.g/L to 252.50. mu.g/L, and the specific calculation results are shown in Table 5.
TABLE 56 effective constituent detection Limit (LOD) and quantitative Limit (LOQ) calculation results
8. Recovery rate test procedure
Accurately sucking 4mL of a sample (1) to be detected into a 50mL centrifuge tube, wherein 6 parts are respectively marked as R1-1 and R1-2, R2-1 and R2-2, R3-1 and R3-2;
mixing the effective components in 3.3 with standard solution, adding 0.05mL into R1-1 and R1-2, adding 0.1mL into R2-1 and R2-2, and adding 0.2mL into R3-1 and R3-2;
adding eugenol-d respectively320 mu L of internal standard substance liquid, 10mL of water, 4g of sodium chloride, ultrasonic dissolution, 2mL of ether, vortex oscillation extraction for 1min, centrifugation for 5min at 8000r/min, sucking 1mL of supernatant to a sample bottle, and mass spectrogram of recovery rate experiment of the sample (1) to be detected after GC/MS analysis is shown in figure 9.
Substituting the peak areas of the effective components and the internal standard substance into the standard curve, calculating the content and the recovery rate of each effective component, wherein the recovery rates of the 6 effective components are all more than 85%, and the RSD values are all less than 5%, which shows that the method has good accuracy, and the specific calculation results are shown in Table 6.
TABLE 66 detection results and recovery rates of effective components
Example 2
The embodiment provides a method for detecting the content of effective components (including linalool, camphor, cinnamaldehyde, bornyl acetate, eugenol and ligustilide) in health care wine, which comprises the following specific steps:
1. reagent: same as in example 1.
2. Sample to be tested (2): jinbianji jin wine, with an alcohol content of 38% (V/V) and a light transmittance of 70%, was offered by Jinpai Limited.
3. Reference simulation liquid: and (3) sucking 76mL of health wine base with the alcoholic strength of 50% (V/V) into a 100mL volumetric flask, adding 0.3g of white granulated sugar, shaking to dissolve, fixing the volume to a scale with water, adding caramel pigment to adjust the light transmittance to be 70%, so that the alcoholic strength, the total sugar content and the light transmittance are consistent with those of the sample (2) to be detected, and storing at 4 ℃.
4. And (3) sample treatment process: accurately sucking 4mL of sample to be detected into a 50mL centrifuge tube, and adding eugenol-d3Adding 11mL of internal standard solution, adding 11mL of water, adding 4g of sodium chloride, ultrasonically dissolving, adding 2mL of ether, performing vortex oscillation extraction for 1min, centrifuging for 5min at 8000r/min, and sucking out 1mL of supernatant to a sample bottle for GC/MS analysis.
5. Drawing a standard curve: the same as in example 1.
6. And (3) sample determination: the measurement conditions and method are the same as those in example 1, the mass spectrum of the obtained sample (2) to be measured is shown in fig. 10, the peak areas of the effective components and the internal standard substance are substituted into the standard curve, and the content of each effective component is calculated, and the calculation results of 6 effective components in the sample (2) to be measured in this example are shown in table 7.
TABLE 7 results of detection of 6 effective components in the sample (2) to be tested
Example 3
The embodiment provides a method for detecting the content of effective components (including linalool, camphor, cinnamaldehyde, bornyl acetate, eugenol and ligustilide) in health care wine, which comprises the following specific steps:
1. reagent: same as in example 1.
2. Sample to be tested (3): the alcohol content is 38% (V/V), the light transmittance is 65%, and the product is provided by Zhejiang neutralization wine industry.
3. Preparing a reference simulation liquid: sucking 76mL of health wine base with the alcoholic strength of 50% (V/V) into a 100mL volumetric flask, adding 11g of white granulated sugar, shaking to dissolve, adding water to a constant volume to a scale, adding caramel pigment to adjust the light transmittance to 65%, and storing at 4 ℃.
4. And (3) sample treatment process: accurately sucking 4mL of sample to be detected into a 50mL centrifuge tube, and adding eugenol-d3Adding 11mL of internal standard solution, adding 11mL of water, adding 4g of sodium chloride, ultrasonically dissolving, adding 2mL of ether, performing vortex oscillation extraction for 1min, centrifuging for 5min at 8000r/min, and sucking out 1mL of supernatant to a sample bottle for GC/MS analysis.
5. Drawing a standard curve: the same as in example 1.
6. And (3) sample determination: the measurement conditions and method are the same as those in example 1, the mass spectrum of the obtained sample (3) to be measured is shown in fig. 11, the peak areas of the effective components and the internal standard substance are substituted into the standard curve, and the content of each effective component is calculated, and the calculation results of 6 effective components in the sample (3) to be measured in this embodiment are shown in table 8.
TABLE 8 detection results of 6 effective components in the sample (3) to be tested
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (7)
1. A method for detecting the content of effective components in health wine is characterized by comprising the following steps: detecting by using a gas chromatography-mass spectrometer, and calculating to obtain the content of the effective components based on a standard curve method;
the pretreatment of the sample specifically comprises the following steps: mixing a health wine sample to be detected with an isotope internal standard substance of effective components and water, adding sodium chloride until the solution is saturated, and extracting with an organic solvent to obtain a sample solution;
the effective components are linalool, camphor, cinnamyl aldehyde, borneol acetate, eugenol and ligustilide, and the isotope internal standard substance is a eugenol isotope; the organic solvent is diethyl ether;
the dosage ratio of the health wine sample to be tested, the isotope internal standard substance and water is 3-5 mL to 5-10 mug to 5-20 mL; the volume ratio of the health wine sample to be tested to the diethyl ether is 2: 1;
wherein the gas chromatography detection conditions comprise: the stationary phase of the chromatographic column is (5% -phenyl) -methyl polysiloxane, the temperature of a sample inlet is 280 ℃, the split ratio is 10:1, the constant flow mode is adopted, the flow rate is 1.5mL/min, and the sample injection amount is 1 mu L; the initial column temperature is 50 deg.C, maintained for 5min, increased to 180 deg.C at 3.5 deg.C/min, increased to 320 deg.C at 30 deg.C/min, and maintained for 10 min.
2. The method of claim 1, wherein the preparing of the standard solution specifically comprises: mixing a wine base, water, white granulated sugar and caramel pigment corresponding to the health-care wine sample to be detected to prepare a reference simulation solution with the alcoholic strength, sugar content and light transmittance consistent with those of the health-care wine sample to be detected;
and dissolving an effective component standard substance by using the reference simulated liquid as a solvent, and treating the obtained solution according to the method for treating the health-care wine sample to be detected to obtain the sample solution to obtain the standard solution.
3. The method according to claim 2, wherein the standard curve is established by taking the ratio of the chromatographic peak areas of the effective component and the internal standard substance in the standard solution as the ordinate and the ratio of the concentration of the effective component and the internal standard substance in the standard solution as the abscissa.
4. The method of claim 1, wherein the eugenol isotope is eugenol-d3。
5. The method of claim 1, wherein the gas chromatography detection conditions comprise: the carrier gas is high-purity helium with the purity more than or equal to 99.999 percent.
6. The method of claim 1, wherein the mass spectrometric detection conditions comprise:
ionization mode: electron bombardment source with energy of 70 eV; temperature of the quadrupole rods: 150 ℃; ion source temperature: 230 ℃; solvent retardation: 5 min; the detection mode is as follows: and selecting ion scanning and collecting.
7. The method according to claim 1, characterized in that it comprises in particular:
a. mixing the health liquor sample to be tested with eugenol-d3Mixing the mixture with water according to the proportion of 3-5 mL to 5-10 mug to 5-20 mL to obtain a mixed solution, adding sodium chloride into the mixed solution until the mixed solution is saturated, then extracting the mixed solution with ether, wherein the volume of the ether is half of that of the sample of the health wine to be detected, and performing centrifugal separation to collect supernatant to obtain a sample solution;
b. mixing a wine base, water, white granulated sugar and caramel pigment corresponding to the health-care wine sample to be detected to prepare a reference simulation solution with the alcoholic strength, sugar content and light transmittance consistent with those of the health-care wine sample to be detected; dissolving an effective component standard substance by using the reference simulated liquid as a solvent, and processing the obtained solution according to the step a to obtain a standard solution;
c. respectively carrying out gas chromatography-mass spectrometry detection analysis on the sample solution obtained in the step a and the standard solution obtained in the step b;
d. to mark withThe effective component and eugenol-d in the quasi-solution3The ratio of the chromatographic peak area of the extract to the chromatographic peak area of the eugenol-d is ordinate3The concentration ratio of (A) is an abscissa, and a standard curve is established;
e. mixing the effective components with eugenol-d in the sample solution3Substituting the chromatographic peak area ratio into a standard curve to calculate the content of the effective components in the health wine sample to be measured.
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| CN110927269A (en) * | 2019-11-27 | 2020-03-27 | 宜宾五粮液股份有限公司 | Method for quantitatively detecting DL-2-hydroxy-4-methyl ethyl valerate in wine |
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