CN114184703A - Raspberry wine quality control method - Google Patents
Raspberry wine quality control method Download PDFInfo
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- CN114184703A CN114184703A CN202111512311.2A CN202111512311A CN114184703A CN 114184703 A CN114184703 A CN 114184703A CN 202111512311 A CN202111512311 A CN 202111512311A CN 114184703 A CN114184703 A CN 114184703A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
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Abstract
The invention discloses a quality control method of raspberry wine, which mainly comprises the following steps: (1) screening out two active ingredients in the raspberry wine, namely ellagic acid and raspberry ketone; (2) taking a raspberry wine sample, and carrying out appropriate treatment on the sample to obtain a test sample solution; (3) preparing ellagic acid and raspberry ketone mixed reference substance solutions with different concentration gradients; (4) establishing a high performance liquid chromatography analysis method, and carrying out chromatographic analysis on the test solution and the reference solution; (5) establishing a standard curve of ellagic acid and raspberry ketone, and calculating the concentration of each corresponding component in the test sample according to the standard curve; (6) collecting more than 10 batches of raspberry wine, detecting the content of ellagic acid and raspberry ketone in the raspberry wine, evaluating and formulating the internal control standard of the product. The quality control method established by the invention has very important significance for strengthening the health care and health preserving functions of the raspberry wine and ensuring the product quality, and has good application prospect.
Description
Technical Field
The invention relates to the field of quality control of wine products, in particular to a quality control method of raspberry wine.
Background
The raspberry wine is prepared by taking raspberries as basic raw materials and adopting fermentation or soaking extraction and other modes. The raspberry wine has the typical characteristics of the traditional white spirit, and because the raspberry wine uses the special raw material of the raspberry, the wine body also contains active ingredients in the raspberry. Enterprises generally establish the product standard of raspberry wine according to specific requirements in national standards such as liqueur, general rules of quality of prepared wine and the like, and mainly control the sensory indexes such as color, aroma, taste, format and the like, and the physicochemical indexes such as alcoholic strength, total acidity and the like. The quality of the raspberry wine is controlled only by the indexes, and the indexes are not enough to represent the characteristics of the raspberry wine. In fact, the choice of using raspberries as starting material is due, in addition to the typical style characteristics of the wine resulting from the use of this starting material, to the fact that raspberries contain a wide variety of active substances. Modern researches have proved that raspberry has the active functions of antioxidation, antibiosis, anticancer, anti-inflammatory, obesity inhibition, skin beautification and hair growth, etc., which are related to active ingredients in raspberry such as ellagic acid, superoxide dismutase (SOD), flavonoid, anthocyanin, procyanidine, raspberry ketone, etc., and the active ingredients are the material basis of raspberry with specific active function. However, it is unknown whether the raspberry wine contains active components of raspberry and how much content of the active components can be controlled by establishing relevant standards. Therefore, the establishment of the raspberry wine quality control method, the screening of the appropriate index components in the raspberry wine and the establishment of the detection method have very important significance for strengthening the health care and health preserving functions of the raspberry wine and ensuring the product quality.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a raspberry wine quality control method.
In order to achieve the above object, the present invention provides the following technical solutions:
a raspberry wine quality control method comprises the following steps:
(1) screening active ingredients in the raspberry wine, and determining ellagic acid and raspberry ketone as key active ingredients;
(2) taking a raspberry wine sample, and carrying out appropriate treatment on the sample to obtain a test sample solution;
(3) preparing ellagic acid and raspberry ketone mixed reference substance solutions with different concentration gradients;
(4) establishing a high performance liquid chromatography analysis method, and carrying out chromatographic analysis on the test solution and the reference solution;
(5) establishing a standard curve of ellagic acid and raspberry ketone, and calculating the concentration of each corresponding component in the test sample according to the standard curve;
(6) collecting more than 10 batches of raspberry wine, detecting the content of ellagic acid and raspberry ketone in the raspberry wine, evaluating and formulating the internal control standard of the product.
Preferably, the preparation of the health wine sample in the step (2) comprises the following steps: taking a proper amount of raspberry wine to be tested, and filtering the raspberry wine by using a 0.22 mu m needle filter.
Preferably, the preparation method of the mixed control solution in the step (3) comprises the following steps: respectively preparing ellagic acid and raspberry ketone reference substance solutions, then preparing a mixed reference substance solution, and diluting the mixed reference substance solution into a series of mixed reference substance solutions with different concentration gradients.
Preferably, the chromatographic conditions in step (4) are: the chromatographic column filled with octadecylsilane chemically bonded silica is used as an analytical chromatographic column, acetonitrile-0.2% phosphoric acid aqueous solution (21:79) is used as a mobile phase, and the detection is carried out by adopting variable wavelength.
Preferably, in the step (4), the flow rate is 1.0mL/min, the temperature of the chromatographic column is 30 ℃, and the detection wavelength is as follows: 254nm for 0-12 min and 222nm for 12-35 min.
Preferably, the internal control quality standard in the step (6) is formulated according to the following steps: analyzing and evaluating the content of ellagic acid and raspberry ketone in representative raspberry wine of more than 10 batches, and formulating the product internal control standard according to the content range.
Preferably, the product internal control standard is as follows: the content of ellagic acid is not less than 5mg/L, and the content of raspberry ketone is not less than 0.5 mg/L.
The method collects and arranges chemical components contained in the raspberry, and screens and confirms the components contained in the raspberry wine by using ultra-high performance liquid chromatography-tandem high resolution mass spectrometry. Through screening, the raspberry wine is found to contain two main active ingredients, namely ellagic acid and raspberry ketone. According to the search of the existing research situation, the fruit with the highest ellagic acid content is raspberry, and the fruit has the active functions of resisting cancer, resisting oxidation, resisting inflammation and the like; raspberry ketone is an important aromatic substance in raspberry, can promote basal metabolism of human body, reduce fat content of human body, and has obvious weight-reducing effect. The two components are key and representative active ingredients in the raspberry, and can be used as index ingredients in raspberry wine for control.
The content difference of ellagic acid and raspberry ketone in the raspberry wine is large, wherein the content of raspberry ketone is relatively low, other components in the raspberry wine may influence the detection of target components, in addition, the maximum absorption wavelengths of ellagic acid and raspberry ketone are different, and a certain difficulty exists in establishing a detection method for simultaneously detecting the two components. The method for simultaneously detecting the ellagic acid and the raspberry ketone in the raspberry wine, which is established by the invention, performs variable-wavelength detection under the maximum absorption wavelength of the ellagic acid and the raspberry ketone respectively, so that the interference is reduced, and the sensitivity and the accuracy of the detected components are improved.
The invention screens out two representative active ingredients in the raspberry wine, and the established detection method has the advantages of simple and convenient operation, strong applicability, and higher specificity, sensitivity and accuracy. The quality research and control of the raspberry wine are more comprehensive, effective and reliable.
Drawings
FIG. 1 is a chromatogram of a mixed control according to the invention;
FIG. 2 is a chromatogram of a raspberry wine sample of the present invention;
in the figure, 1 represents the peak position of ellagic acid, and 2 represents the peak position of raspberry ketone.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment provides a raspberry wine quality control method, which comprises the following steps:
(1) screening active ingredients in the raspberry wine:
respectively preparing reference substance solutions of ellagic acid, raspberry ketone, kaempferol-3-0-rutinoside, tilianin, quercetin, gallic acid and the like, analyzing the raspberry wine test sample solution and the reference substance solution by using an ultra-high performance liquid chromatography-tandem high resolution mass spectrometer, qualitatively screening according to the first-level and second-level mass spectrum data information of the compounds, and finally determining that the main active ingredients contained in the raspberry wine are ellagic acid and raspberry ketone.
(2) Preparation of a test solution:
taking a proper amount of raspberry wine sample, filtering with a 0.22 μm needle filter, and using as a test solution for later use.
(3) Preparation of control solutions:
precisely weighing 1.11mg of ellagic acid and 1.90mg of raspberry ketone as reference substances, respectively putting into 10mL volumetric flasks, adding methanol for dissolving, fixing the volume, and shaking up to obtain ellagic acid and raspberry ketone reference substance stock solutions. Precisely measuring 2.0mL of ellagic acid reference substance stock solution and 0.1mL of raspberry ketone reference substance stock solution in 10mL volumetric flasks, adding 70% methanol to a constant volume, and shaking up to obtain mixed reference substance solutions numbered as No. 1, No. 2, No. 3, No. 4 and No. 5, wherein the concentrations of the mixed reference substance solutions are shown in the following table.
Table 1: concentration of mixed control solution
(4) Chromatographic conditions
Acetonitrile-0.2% phosphoric acid aqueous solution (21:79) was used as a mobile phase, the flow rate was 1.0mL/min, the column chromatography was an Agilent ZORBAX SB-Aq C18 column (4.6 mm. times.250 mm, 5 μm), the column temperature was 30 ℃, the detection wavelength: 254nm for 0-12 min and 222nm for 12-35 min.
(5) Establishing a standard curve of each component reference substance
And (3) analyzing the mixed solution of the mixed reference substances with different concentration gradients in the step (2) according to the chromatographic conditions in the step (3) to obtain a mixed reference substance chromatogram, which is shown in figure 1. Further obtaining the chromatographic peak areas of ellagic acid and raspberry ketone in the reference substance solutions with various concentrations, respectively establishing a standard curve by taking the concentration of each reference substance solution as an abscissa and the corresponding chromatographic peak area as an ordinate, and obtaining the standard curve and a linear correlation coefficient R2The values are given in the following table.
Table 2: standard curve data
As can be seen from Table 2, the linear correlation coefficient R of the standard curve of ellagic acid and raspberry ketone2The values were all greater than 0.995, indicating that the components are in good linear relationship over the corresponding concentration ranges.
(6) Repeatability test
Taking the same raspberry wine, preparing 6 parts of test solution according to the method in the step (1), numbering 1-6, and analyzing according to the chromatographic conditions in the step (3), wherein the chromatogram of the test solution is shown in figure 2. And respectively calculating the concentrations of the ellagic acid and the raspberry ketone in the sample by using the established standard curve, and calculating the repeatability of the measurement result. The RSD values of the repeatability experiments of the ellagic acid and the raspberry ketone are less than 5%, which shows that the repeatability of the method is good. The data of the repeatability experiments are shown in the following table.
Table 3: data of repeatability experiments
(7) Test for recovery with addition of standard
Precisely measuring 5mL of raspberry wine, placing the raspberry wine in a 10mL volumetric flask, precisely adding 98.568mg/L ellagic acid reference substance solution 0.3mL, 0.4mL and 0.5mL, and 37.24mg/L raspberry ketone reference substance solution 0.08mL, 0.10mL and 0.12mL respectively, making 3 samples in each group, using 70% methanol solution to fix the volume, and shaking up to obtain 9 sample solutions.
And (4) analyzing according to the chromatographic conditions in the step (3), calculating the concentrations of ellagic acid and raspberry ketone in each test sample solution by using the established standard curve, and calculating the recovery rates of ellagic acid and raspberry ketone in the sample, wherein the recovery rates of ellagic acid and raspberry ketone are both more than 90%, which indicates that the accuracy of the method is good. The spiked recovery data are shown in the table below.
Table 4: normalized recovery data
(8) Sample detection
Taking 15 batches of raspberry wine, preparing a test solution according to the method in the step (1), analyzing according to the chromatographic conditions in the step (3), and respectively calculating the concentrations of ellagic acid and raspberry ketone in the sample by using the established standard curve. The results show that the contents of ellagic acid and raspberry ketone in 15 batches of raspberry wine are stable, the two indexes can be used as the quality control indexes of the raspberry wine, and the sample detection data are shown in the following table.
Table 5: sample detection data
(9) Internally controlled standard establishment
According to the detection result of the raspberry wine content in 15 batches of health care wine, through statistical analysis, the internal control quality standard of ellagic acid and raspberry ketone in raspberry wine can be customized as follows:
ellagic acid is more than or equal to 5 mg/L;
raspberry ketone is more than or equal to 0.5 mg/L.
The above-mentioned embodiments only express the embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (7)
1. A method for controlling the quality of raspberry wine is characterized by comprising the following steps:
(1) screening active ingredients in the raspberry wine, and determining ellagic acid and raspberry ketone as key active ingredients;
(2) taking a raspberry wine sample, and carrying out appropriate treatment on the sample to obtain a test sample solution;
(3) preparing ellagic acid and raspberry ketone mixed reference substance solutions with different concentration gradients;
(4) establishing a high performance liquid chromatography analysis method, and carrying out chromatographic analysis on the test solution and the reference solution;
(5) establishing a standard curve of ellagic acid and raspberry ketone, and calculating the concentration of each corresponding component in the test sample according to the standard curve;
(6) collecting more than 10 batches of raspberry wine, detecting the content of ellagic acid and raspberry ketone in the raspberry wine, evaluating and formulating the internal control standard of the product.
2. The method for controlling the quality of raspberry wine according to claim 1, wherein the preparation of the health wine sample in step (2) comprises: taking a proper amount of raspberry wine to be tested, and filtering the raspberry wine by using a 0.22 mu m needle filter.
3. The method for controlling the quality of raspberry wine according to claim 1, wherein the method for preparing the mixed control solution in step (3) comprises: respectively preparing ellagic acid and raspberry ketone reference substance solutions, then preparing a mixed reference substance solution, and diluting the mixed reference substance solution into a series of mixed reference substance solutions with different concentration gradients.
4. The method for controlling the quality of raspberry wine according to claim 1, wherein the chromatographic conditions in step (4) are: the chromatographic column filled with octadecylsilane chemically bonded silica is used as an analytical chromatographic column, acetonitrile-0.2% phosphoric acid aqueous solution (21:79) is used as a mobile phase, and the detection is carried out by adopting variable wavelength.
5. The method for controlling the quality of raspberry wine according to claim 4, wherein in step (4), the flow rate is 1.0mL/min, the temperature of the chromatographic column is 30 ℃, and the detection wavelength is as follows: 254nm for 0-12 min and 222nm for 12-35 min.
6. The method for controlling the quality of raspberry wine according to claim 1, wherein the internal control quality standard in step (6) is established according to the following criteria: analyzing and evaluating the content of ellagic acid and raspberry ketone in representative raspberry wine of more than 10 batches, and formulating the product internal control standard according to the content range.
7. The method for controlling the quality of raspberry wine of claim 6, wherein the product internal control standard is: the content of ellagic acid is not less than 5mg/L, and the content of raspberry ketone is not less than 0.5 mg/L.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101718690A (en) * | 2009-12-11 | 2010-06-02 | 天津市林业果树研究所 | Method for measuring content of ellagic acid substance in raspberry |
| CN104407087A (en) * | 2014-12-04 | 2015-03-11 | 广西壮族自治区兽医研究所 | Method for simultaneously detecting gallic acid and ellagic acid in radix rhodomyrti |
| CN110196290A (en) * | 2019-04-02 | 2019-09-03 | 贵州医科大学 | Ellagic acid content assaying method in a kind of Rosa roxburghii Tratt |
| CN110455961A (en) * | 2019-09-03 | 2019-11-15 | 劲牌有限公司 | Multicomponent high-flux detection method in a kind of health liquor |
| CN112126614A (en) * | 2020-09-30 | 2020-12-25 | 江南大学 | Method for preparing raspberry ketone by whole cell transformation |
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- 2021-12-07 CN CN202111512311.2A patent/CN114184703A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101718690A (en) * | 2009-12-11 | 2010-06-02 | 天津市林业果树研究所 | Method for measuring content of ellagic acid substance in raspberry |
| CN104407087A (en) * | 2014-12-04 | 2015-03-11 | 广西壮族自治区兽医研究所 | Method for simultaneously detecting gallic acid and ellagic acid in radix rhodomyrti |
| CN110196290A (en) * | 2019-04-02 | 2019-09-03 | 贵州医科大学 | Ellagic acid content assaying method in a kind of Rosa roxburghii Tratt |
| CN110455961A (en) * | 2019-09-03 | 2019-11-15 | 劲牌有限公司 | Multicomponent high-flux detection method in a kind of health liquor |
| CN112126614A (en) * | 2020-09-30 | 2020-12-25 | 江南大学 | Method for preparing raspberry ketone by whole cell transformation |
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