Method for rapidly analyzing total ester content in raw liquor
By directly determining the ester content in raw baijiu using gas chromatography and combining it with calculation formulas, this method solves the problems of long processing time and environmental unfriendliness associated with traditional methods, achieving rapid and accurate detection of total ester content, and is applicable to baijiu with different alcohol contents.
Patent Information
- Application Number
- CN202511544846.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-28
- Publication Date
- 2026-01-23
AI Technical Summary
Traditional methods for detecting total ester content in baijiu are time-consuming and cumbersome, making it difficult to meet the needs for rapid detection. In particular, they can easily lead to incomplete saponification in high-alcohol-content raw baijiu, and the use of multiple chemical reagents is not environmentally friendly.
The main ester content in the raw liquor of baijiu is directly determined by gas chromatography. Combined with the total ester content calculation formula, the ester content is detected by gas chromatography and the total ester content is derived, avoiding the complicated operation of chemical titration.
It enables rapid detection of total ester content in baijiu raw liquor, achieving success within 30 minutes on the first attempt. It is highly accurate, applicable to alcohol content ranges of 25% vol to 75% vol, environmentally friendly, and reduces testing costs.
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Figure CN121385141A_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of liquor testing technology, and in particular to a method for rapidly analyzing the total ester content in raw liquor. Background Technology
[0002] Traditional methods for detecting total ester content in baijiu (Chinese liquor) primarily employ chemical titration or potentiometric titration, based on the principles of acid-base neutralization and ester saponification. The specific procedure involves: first, using phenolphthalein as an indicator, neutralizing free acids in the baijiu sample with a standard sodium hydroxide solution; then, accurately adding excess sodium hydroxide solution and heating under reflux to induce saponification of the esters; finally, back-titering the remaining sodium hydroxide with a standard sulfuric acid solution, and calculating the volume of sulfuric acid consumed to determine the total ester content. This entire process takes approximately 4 hours, is quite cumbersome, requires multiple chemical reagents such as sodium hydroxide, sulfuric acid, and phenolphthalein indicator, and demands extremely high accuracy in the concentration of the standard solutions. Furthermore, the reflux apparatus is complex and difficult to operate, especially when testing raw baijiu with an alcohol content exceeding 68% vol; insufficient sodium hydroxide can lead to incomplete saponification and experimental failure. Therefore, this method is insufficient to meet the practical needs of baijiu producers for rapid testing of large quantities of raw baijiu samples. Summary of the Invention
[0003] The purpose of this application is to provide a method for rapidly analyzing the total ester content in raw baijiu (Chinese liquor) to solve the above-mentioned problems.
[0004] To achieve the above objectives, this application adopts the following technical solution: This application provides a method for rapidly analyzing the total ester content in raw Baijiu (Chinese liquor), the method comprising: The content of target esters in the raw liquor of baijiu is determined; the total ester content in the raw liquor of baijiu is calculated according to the formula for calculating total ester content; The formula for calculating the total ester content is as follows: ; in, X The total ester content in the raw liquor of the aforementioned baijiu is expressed in g / L. C i The content of the target esters in the raw liquor of the baijiu is expressed in g / L. M i The molar mass of the target ester in the raw liquor of the baijiu is expressed in g / mol. M 乙酸乙酯 The value represents the molar mass of ethyl acetate, expressed in g / mol.
[0005] Optionally, the target esters include ethyl acetate, ethyl butyrate, ethyl hexanoate, and ethyl lactate.
[0006] Optionally, gas chromatography is used to detect the content of the target esters in the raw liquor of the baijiu: The chromatographic column has dimensions of 30m × 0.250mm × 0.25μm; The detector temperature is 255-265℃, the injection port temperature is 235-245℃, the carrier gas flow rate is 0.8-1.2mL / min, the injection volume is 0.39-0.41μL, and the split ratio is 28-32:1. The temperature conditions for the chromatographic column are as follows: initial temperature 33-37℃, hold for 1-3 min, increase to 58-62℃ at 1-3℃ / min, increase to 110℃ at 9℃ / min, increase to 230℃ at 6℃ / min, and hold for 4 min.
[0007] Optionally, the derivation process of the formula for calculating the total ester content includes: S1: The volume of the raw liquor sample is V 1. The content of the target ester C i Calculate the amount of the target ester; S2: The theoretical value of the amount of sodium hydroxide standard solution consumed by the original liquor sample is obtained based on the amount of sodium hydroxide standard solution consumed per mole of ester group. S3: Based on the concentration of the sodium hydroxide standard solution, substitute the theoretical value of the amount of sodium hydroxide standard solution into the equation to obtain the theoretical value of the volume of sodium hydroxide standard solution consumed by the baijiu raw liquor sample. S4: The actual volume of sodium hydroxide standard solution consumed is obtained based on the volume relationship coefficient of the sodium hydroxide standard solution actually consumed in the total ester detection; S5: Based on the concentration of the sodium hydroxide standard solution, the actual volume of the sodium hydroxide standard solution consumed, and M 乙酸乙酯 The formula for calculating the total ester content in the original liquor sample is obtained.
[0008] Optionally, the formula for calculating the amount of the target ester is: .
[0009] Optionally, in step S2, the theoretical formula for calculating the amount of sodium hydroxide standard solution consumed by the raw liquor sample is as follows: .
[0010] Optionally, in step S3, the concentration of the sodium hydroxide standard solution is: C The theoretical formula for calculating the volume of sodium hydroxide standard solution required for the raw liquor sample is as follows: .
[0011] Optionally, in step S4, the volume relationship coefficient is 1.02; the formula for calculating the actual volume of the sodium hydroxide standard solution consumed is: .
[0012] Optionally, the total ester content in the raw liquor sample of the baijiu X The calculation formula is: ; The simplified formula for calculating the total ester content is as follows: .
[0013] Optionally, the alcohol content of the raw liquor is 25-75 vol.
[0014] Compared with the prior art, the beneficial effects of this application include: This application provides a rapid method for analyzing the total ester content in raw baijiu (Chinese liquor). The technical solution requires only a sample of the raw baijiu for direct detection of the main esters. The entire process takes approximately 30 minutes and is successful on the first attempt, offering speed and accuracy. Firstly, this method effectively solves the problem of rapid detection of total ester content in raw baijiu with an alcohol content exceeding 68% vol, and is also applicable to the detection of total esters in packaged finished baijiu with an alcohol content between 25% vol and 68% vol, no longer limited to the alcohol content range of titration methods. Secondly, this method does not use chemical reagents, making it more environmentally friendly and saving on testing costs. Detailed Implementation
[0015] As used in this article: "Prepared from" is synonymous with "comprising". The terms "comprising", "including", "having", "containing", or any other variations thereof as used herein are intended to cover non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that includes the listed elements is not necessarily limited to those elements, but may include other elements not expressly listed or elements inherent to such composition, step, method, article, or apparatus.
[0016] The conjunction "composed of..." excludes any unspecified elements, steps, or components. If used in a claim, this phrase makes the claim closed, excluding materials other than those described, except for associated conventional impurities. When the phrase "composed of..." appears in a clause of the body of a claim rather than immediately following it, it limits only the elements described in that clause; other elements are not excluded from the claim as a whole.
[0017] When a quantity, concentration, or other value or parameter is expressed as a range, a preferred range, or a range defined by a series of upper and lower preferred values, this should be understood as specifically disclosing all ranges formed by any pair of any upper or preferred value with any lower or preferred value, regardless of whether the range is disclosed individually. For example, when the range “1–5” is disclosed, the described range should be interpreted as including ranges “1–4”, “1–3”, “1–2”, “1–2 and 4–5”, “1–3 and 5”, etc. When numerical ranges are described herein, unless otherwise stated, the range is intended to include its endpoints and all integers and fractions within that range.
[0018] In these embodiments, unless otherwise specified, the portions and percentages are all by weight.
[0019] "Parts by mass" refers to the basic unit of measurement that expresses the mass ratio of multiple components. One part can represent any unit mass, such as 1g or 2.689g. If we say that component A has "a" parts by mass and component B has "b" parts by mass, it means the ratio of the mass of component A to the mass of component B is a:b. Alternatively, it can mean that the mass of component A is aK and the mass of component B is bK (where K is any number representing a multiplier). It is important to understand that, unlike parts by mass, the sum of the mass parts of all components is not limited to 100 parts.
[0020] "And / or" is used to indicate that one or both of the described situations may occur, for example, A and / or B includes (A and B) and (A or B).
[0021] To better explain the technical solution provided in this application, the technical solution will be described in its entirety before proceeding with specific implementation methods.
[0022] This application provides a method for rapidly analyzing the total ester content in raw Baijiu (Chinese liquor), the method comprising: The content of target esters in the raw liquor of baijiu is determined; the total ester content in the raw liquor of baijiu is calculated according to the formula for calculating total ester content; The formula for calculating the total ester content is as follows: ; in, X The total ester content in the raw liquor of the aforementioned baijiu is expressed in g / L. C i The content of the target esters in the raw liquor of the baijiu is expressed in g / L. M i The molar mass of the target ester in the raw liquor of the baijiu is expressed in g / mol. M 乙酸乙酯The value represents the molar mass of ethyl acetate, expressed in g / mol.
[0023] Furthermore, the target esters include ethyl acetate, ethyl butyrate, ethyl hexanoate, and ethyl lactate.
[0024] Furthermore, the content of the target esters in the raw liquor of the baijiu was detected using gas chromatography.
[0025] The chromatographic column has dimensions of 30m × 0.250mm × 0.25μm; The detector temperature is 255-265℃, the injection port temperature is 235-245℃, the carrier gas flow rate is 0.8-1.2mL / min, the injection volume is 0.39-0.41μL, and the split ratio is 28-32:1. The temperature conditions for the chromatographic column are as follows: initial temperature 33-37℃, hold for 1-3 min, increase to 58-62℃ at 1-3℃ / min, increase to 110℃ at 9℃ / min, increase to 230℃ at 6℃ / min, and hold for 4 min.
[0026] Optionally, the detector temperature can be 255℃, 256℃, 257℃, 258℃, 259℃, 260℃, 261℃, 262℃, 263℃, 264℃, 265℃, or any value between 255℃ and 265℃; the injection port temperature can be 235℃, 236℃, 237℃, 238℃, 239℃, 240℃, 241℃, 242℃, 243℃, 244℃, 245℃, or any value between 235℃ and 245℃; the injection volume can be 0.39μL, 0.40℃, 0.41℃, or any value between 0.39℃ and 0.41℃; the split ratio can be 28:1, 29:1, 30:1, 31:1, 32:1, or any value between 28℃ and 32:1.
[0027] Optionally, the first temperature of the chromatographic column can be 33℃, 34℃, 35℃, 36℃, 37℃, or any value between 33℃ and 37℃; the holding time at the first temperature can be 1 min, 2 min, 3 min, or any value between 1 min and 3 min. The heating rate to the second temperature can be 1℃ / min, 2℃ / min, 3℃ / min, or any value between 1℃ and 3℃ / min; the second temperature can be 58℃, 59℃, 60℃, 61℃, 62℃. The heating rate to the third temperature can be 8℃ / min, 9℃ / min, 10℃ / min, or any value between 8℃ and 10℃ / min; the third temperature can be 108℃, 109℃, 110℃, 111℃, 112℃, or any value between 108℃ and 112℃. The heating rate to the fourth temperature can be 5℃ / min, 6℃ / min, 7℃ / min, or any value between 5℃ / min; the fourth temperature can be 225℃, 226℃, 227℃, 228℃, 229℃, 230℃, 231℃, 232℃, 233℃, 234℃, 235℃, or any value between 225℃ and 235℃; the holding time of the fourth temperature can be 3 min, 4 min, 5 min, or any value between 3 min and 5 min.
[0028] Furthermore, the derivation process of the formula for calculating the total ester content includes: S1: The volume of the raw liquor sample is V 1. The content of the target ester C i Calculate the amount of the target ester; S2: The theoretical value of the amount of sodium hydroxide standard solution consumed by the original liquor sample is obtained based on the amount of sodium hydroxide standard solution consumed per mole of ester group. S3: Based on the concentration of the sodium hydroxide standard solution, substitute the theoretical value of the amount of sodium hydroxide standard solution into the equation to obtain the theoretical value of the volume of sodium hydroxide standard solution consumed by the baijiu raw liquor sample. S4: The actual volume of sodium hydroxide standard solution consumed is obtained based on the volume relationship coefficient of the sodium hydroxide standard solution actually consumed in the total ester detection; S5: Based on the concentration of the sodium hydroxide standard solution, the actual volume of the sodium hydroxide standard solution consumed, and M 乙酸乙酯 The formula for calculating the total ester content in the original liquor sample is obtained.
[0029] Furthermore, take a sample volume of the raw liquor. V1 (unit: L), analyzed by gas chromatography, the contents of the main esters, including ethyl acetate, ethyl butyrate, ethyl hexanoate, and ethyl lactate, were as follows: C 1. C 2. C 3. C 4 (unit: g / L), the corresponding molar masses are respectively M 1. M 2. M 3. M 4 (unit: g / mol). The formula for calculating the amount of the target ester is: .
[0030] Furthermore, in step S2, since each mole of ester group consumes 1 mole of sodium hydroxide standard solution, the theoretical formula for calculating the amount of sodium hydroxide standard solution consumed by the baijiu raw liquor sample is as follows: .
[0031] Furthermore, in step S3, the concentration of the sodium hydroxide standard solution is... C The theoretical formula for calculating the volume of sodium hydroxide standard solution required for the raw liquor sample is as follows: .
[0032] Furthermore, in step S4, since the composition of total esters in the raw baijiu is not limited to ethyl acetate, ethyl butyrate, ethyl hexanoate, and ethyl lactate, and the saponification reaction needs to be carried out under alkaline conditions, the actual volume of sodium hydroxide standard solution added is greater than the calculated volume. Through extensive experimental data collection, the theoretical volume of sodium hydroxide standard solution consumed for the four esters (ethyl acetate, ethyl butyrate, ethyl hexanoate, and ethyl lactate) detected by gas chromatography was found to be 1.02, which is the relationship coefficient between the volume of sodium hydroxide standard solution actually consumed in the detection of total esters in the raw baijiu. The formula for calculating the actual volume of sodium hydroxide standard solution consumed is as follows: .
[0033] Furthermore, the total ester content in the raw spirit of Baijiu was deduced. X (g / L), according to the calculation requirements of section 7.1.5 of the national standard GB / T 10345-2022 "Analytical Methods for Baijiu", the total ester test result is calculated as ethyl acetate, and the total ester content in the baijiu raw liquor sample is... X The calculation formula is: ; The simplified formula for calculating the total ester content is as follows: .
[0034] Furthermore, the alcohol content of the raw liquor is 25-75 vol.
[0035] Optionally, the alcohol content of the raw liquor can be 25 vol%, 30 vol%, 35 vol%, 40 vol%, 45 vol%, 50 vol%, 55 vol%, 60 vol%, 65 vol%, 70 vol%, 75 vol%, or any value between 25 and 75 vol%.
[0036] It is understandable that the total esters in baijiu (Chinese white liquor) mainly consist of several major esters, including ethyl acetate, ethyl butyrate, ethyl hexanoate, and ethyl lactate. This application, based on the fundamental principle of total ester detection in baijiu, establishes a ratio of ester group hydrolysis consuming sodium hydroxide standard solution, with each mole of ester group consuming one mole of sodium hydroxide standard solution. By determining the content of each major ester component in baijiu using gas chromatography and combining this with the molar mass of each ester, the relationship between total esters and the amount of sodium hydroxide standard solution added is established, thereby deriving the total ester content in the raw liquor.
[0037] The implementation schemes of this application will be described in detail below with reference to specific embodiments. However, those skilled in the art will understand that the following embodiments are only for illustrating this application and should not be regarded as limiting the scope of this application. Unless otherwise specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments used without specified manufacturers are all conventional products that can be purchased commercially.
[0038] The baijiu used in the examples and comparative examples was produced by Sichuan Mianyang Fenggu Winery Co., Ltd.
[0039] Example 1 This embodiment provides a method for rapidly analyzing the total ester content in raw Baijiu (Chinese liquor). The specific steps are as follows: The alcohol content of the raw baijiu used was 37.6% vol. 10 mL of the raw baijiu was taken, and the contents of ethyl acetate, ethyl butyrate, ethyl hexanoate, and ethyl lactate in the raw baijiu were determined by gas chromatography. The gas chromatography measurement conditions were as follows: Agilent GC8890, column model DB-WAX UI, column length × inner diameter × film thickness 30 μm × 0.250 mm × 0.25 μm; detector temperature 260℃, injection port temperature 240℃, carrier gas flow rate 1.0 mL / min, injection volume 0.4 μL, split ratio 30:1; column temperature: initial temperature 35℃, hold for 2 min, increase to 60℃ at 2℃ / min, increase to 110℃ at 9℃ / min, increase to 230℃ at 6℃ / min, hold for 4 min.
[0040] The contents of ethyl acetate, ethyl butyrate, ethyl hexanoate, and ethyl lactate detected in the raw baijiu are substituted into the formula for calculating the total ester content to calculate the total ester content in the raw baijiu. The formula for calculating the total ester content is as follows: ; Substituting the molar mass of ethyl acetate (in g / mol), we obtain the formula for calculating the total ester content: .
[0041] Input the main ester content detected by gas chromatograph to calculate the total ester content in the raw liquor of baijiu. X (g / L), as shown in Table 1: Table 1 Calculation of Total Ester Content in Baijiu Base Wine
[0042] Example 2 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference from Embodiment 1 is that the alcohol content of the raw baijiu is 38% vol.
[0043] Example 3 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. Compared with Example 1, the only difference is that the alcohol content of the raw baijiu is 38.1% vol.
[0044] Example 4 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. Compared with Example 1, the only difference is that the alcohol content of the raw baijiu is 42.1% vol.
[0045] Example 5 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. Compared with Example 1, the only difference is that the alcohol content of the raw baijiu is 45.2% vol.
[0046] Example 6 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference from Embodiment 1 is that the alcohol content of the raw baijiu is 47.9% vol.
[0047] Example 7 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. Compared with Example 1, the only difference is that the alcohol content of the raw baijiu is 51.9% vol.
[0048] Example 8 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. Compared with Example 1, the only difference is that the alcohol content of the raw baijiu is 52.2% vol.
[0049] Example 9 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. Compared with Example 1, the only difference is that the alcohol content of the raw baijiu is 52.0% vol.
[0050] Example 10 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. Compared with Example 1, the only difference is that the alcohol content of the raw baijiu is 63.9% vol.
[0051] Example 11 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. Compared with Example 1, the only difference is that the alcohol content of the raw baijiu is 64.1% vol.
[0052] Example 12 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference from Embodiment 1 is that the alcohol content of the raw baijiu is 65.5% vol.
[0053] Example 13 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. Compared with Example 1, the only difference is that the alcohol content of the raw baijiu is 69.9% vol.
[0054] Example 14 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. Compared with Example 1, the only difference is that the alcohol content of the raw baijiu is 71.3% vol.
[0055] Example 15 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. Compared with Example 1, the only difference is that the alcohol content of the raw baijiu is 73.4% vol.
[0056] Comparative Example 1 This comparative example provides a national standard method for detecting the total ester content in raw Baijiu (Chinese liquor). The specific steps are as follows: 1. Accurately pipette 50 mL of sample into a 250 mL reflux bottle, add 2 drops of 10 g / L phenolphthalein indicator, and titrate with sodium hydroxide standard solution until a faint red color persists for 30 seconds.
[0057] 2. Accurately add 25 mL of sodium hydroxide standard solution (the volume of sodium hydroxide standard solution can be increased if the total ester content is high), shake well, attach the condenser, place it on a boiling water bath for reflux for 30 min, remove it, and cool it (if the solution is colorless, the experiment fails, repeat the experiment by increasing the volume of sodium hydroxide standard solution).
[0058] 3. Titrate with standard sulfuric acid solution until the red color just disappears, and record the volume of standard sulfuric acid solution consumed. Simultaneously, pipette 50 mL (40%, volume fraction) of ester-free ethanol to replace the sample, and record the volume of standard sulfuric acid solution consumed for the blank sample using the same method.
[0059] 4. Calculate the total ester content according to the formula.
[0060] The alcohol content of the raw liquor used is 37.6% vol.
[0061] Comparative Example 2 This comparative example provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference between this comparative example and Comparative Example 1 is that the alcohol content of the raw baijiu is 38% vol.
[0062] Comparative Example 3 This comparative example provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference between this comparative example and Comparative Example 1 is that the alcohol content of the raw baijiu is 38.1% vol.
[0063] Comparative Example 4 This embodiment provides a method for rapidly analyzing the total ester content in raw baijiu. Compared with Comparative Example 1, the only difference is that the alcohol content of the raw baijiu is 42.1% vol.
[0064] Comparative Example 5 This comparative example provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference between this comparative example and Comparative Example 1 is that the alcohol content of the raw baijiu is 45.2% vol.
[0065] Comparative Example 6 This comparative example provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference between this comparative example and Comparative Example 1 is that the alcohol content of the raw baijiu is 47.9% vol.
[0066] Comparative Example 7 This comparative example provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference between this comparative example and Comparative Example 1 is that the alcohol content of the raw baijiu is 51.9% vol.
[0067] Comparative Example 8 This comparative example provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference between this comparative example and Comparative Example 1 is that the alcohol content of the raw baijiu is 52.2% vol.
[0068] Comparative Example 9 This comparative example provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference between this comparative example and Comparative Example 1 is that the alcohol content of the raw baijiu is 52.0% vol.
[0069] Comparative Example 10 This comparative example provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference between this comparative example and Comparative Example 1 is that the alcohol content of the raw baijiu is 63.9% vol.
[0070] Comparative Example 11 This comparative example provides a method for rapidly analyzing the total ester content in raw baijiu. Compared with Comparative Example 1, the only difference is that the alcohol content of the raw baijiu is 64.1% vol.
[0071] Comparative Example 12 This comparative example provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference between this comparative example and Comparative Example 1 is that the alcohol content of the raw baijiu is 65.5% vol.
[0072] Comparative Example 13 This comparative example provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference between this comparative example and Comparative Example 1 is that the alcohol content of the raw baijiu is 69.9% vol.
[0073] Comparative Example 14 This comparative example provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference between this comparative example and Comparative Example 1 is that the alcohol content of the raw baijiu is 71.3% vol.
[0074] Comparative Example 15 This comparative example provides a method for rapidly analyzing the total ester content in raw baijiu. The only difference between this comparative example and Comparative Example 1 is that the alcohol content of the raw baijiu is 73.4% vol.
[0075] The total ester content test results for each embodiment are shown in Table 2: Table 2 Results of the detection of total ester content in Baijiu in the examples
[0076] The total ester detection results for each comparative example are shown in Table 3: Table 3. Results of comparative analysis of total ester content in raw Baijiu.
[0077] Table 4. Precision of Total Ester Content Detection Results for Examples and Comparative Examples
[0078] According to the precision requirements of 7.1.6 in the national standard GB / T 10345-2022 "Analytical Methods for Baijiu", the absolute value of the difference between the test results of this application and the test results of the national standard method does not exceed 2% of their arithmetic mean.
[0079] As shown in the examples, comparative examples, and Table 4, the main ester content of the raw liquor can be directly detected by gas chromatography. The entire process takes about 30 minutes and can be successful in one attempt, which is fast and accurate. Furthermore, it effectively solves the problem of rapid detection of total ester content in raw liquor with an alcohol content exceeding 68% vol. Experiments have proven that this method is also applicable to the detection of total esters in packaged finished liquor with an alcohol content between 25% vol and 68% vol, and is not limited to the alcohol content range specified in the national standard method. The results of the detection using the method of this application and the indicator method specified in Section 7.1 of GB / T 10345-2022 "Analytical Methods for Baijiu" were compared using 15 samples covering the common alcohol content range. The errors in the comparison results were all within the precision range (≤2%) required for total ester detection in GB / T 10345-2022 "Analytical Methods for Baijiu".
[0080] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application.
[0081] Furthermore, those skilled in the art will understand that although some embodiments herein include certain features included in other embodiments but not others, combinations of features from different embodiments are intended to be within the scope of this application and form different embodiments. For example, in the foregoing claims, any of the claimed embodiments can be used in any combination. The information disclosed in this background section is intended only to enhance the understanding of the general background of this application and should not be construed as an admission or in any way implying that such information constitutes prior art known to those skilled in the art.
Claims
1. A method for rapidly analyzing the total ester content in raw Baijiu (Chinese liquor), characterized in that, include: The content of target esters in the raw liquor of baijiu is determined; the total ester content in the raw liquor of baijiu is calculated according to the formula for calculating total ester content; The formula for calculating the total ester content is as follows: ; in, X The total ester content in the raw liquor of the aforementioned baijiu is expressed in g / L. C i The content of the target esters in the raw liquor of the baijiu is expressed in g / L. M i The molar mass of the target ester in the raw liquor of the baijiu is expressed in g / mol. M 乙酸乙酯 The value represents the molar mass of ethyl acetate, expressed in g / mol.
2. The method for rapid analysis of total ester content in raw Baijiu (Chinese liquor) according to claim 1, characterized in that, The target esters include ethyl acetate, ethyl butyrate, ethyl hexanoate, and ethyl lactate.
3. The method for rapid analysis of total ester content in raw Baijiu (Chinese liquor) according to claim 1, characterized in that, The content of the target esters in the raw liquor of the baijiu was determined by gas chromatography, and at least one of the following conditions was met: a. The chromatographic column has the following specifications: 30m × 0.250mm × 0.25μm; b. The detector temperature is 255-265℃, the injection port temperature is 235-245℃, the carrier gas flow rate is 0.8-1.2mL / min, the injection volume is 0.39-0.41μL, and the split ratio is 28-32:1; c. The temperature conditions for the chromatographic column are as follows: First temperature 33-37℃, hold for 1-3 min; heat at 1-3℃ / min to the second temperature 58-62℃; heat at 8-10℃ / min to the third temperature 108-112℃; heat at 5-7℃ / min to the fourth temperature 225-235℃, hold for 3-5 min.
4. The method for rapid analysis of total ester content in raw Baijiu (Chinese liquor) according to claim 1, characterized in that, The derivation process of the formula for calculating the total ester content includes: S1: The volume of the raw liquor sample is V 1. The content of the target ester C i Calculate the amount of the target ester; S2: The theoretical value of the amount of sodium hydroxide standard solution consumed by the original liquor sample is obtained based on the amount of sodium hydroxide standard solution consumed per mole of ester group. S3: Based on the concentration of the sodium hydroxide standard solution, substitute the theoretical value of the amount of sodium hydroxide standard solution into the equation to obtain the theoretical value of the volume of sodium hydroxide standard solution consumed by the baijiu raw liquor sample. S4: The actual volume of sodium hydroxide standard solution consumed is obtained based on the volume relationship coefficient of the sodium hydroxide standard solution actually consumed in the total ester detection; S5: Based on the concentration of the sodium hydroxide standard solution, the actual volume of the sodium hydroxide standard solution consumed, and M 乙酸乙酯 The formula for calculating the total ester content in the original liquor sample is obtained.
5. The method for rapid analysis of total ester content in raw Baijiu (Chinese liquor) according to claim 4, characterized in that, The formula for calculating the amount of the target ester is as follows: 。 6. The method for rapid analysis of total ester content in raw Baijiu (Chinese liquor) according to claim 4, characterized in that, In step S2, the theoretical formula for calculating the amount of sodium hydroxide standard solution consumed by the raw liquor sample is as follows: 。 7. The method for rapid analysis of total ester content in raw Baijiu (Chinese liquor) according to claim 4, characterized in that, In step S3, the concentration of the sodium hydroxide standard solution is: C The theoretical formula for calculating the volume of sodium hydroxide standard solution required for the raw liquor sample is as follows: 。 8. The method for rapid analysis of total ester content in raw Baijiu (Chinese liquor) according to claim 4, characterized in that, In step S4, the volume relationship coefficient is 1.02; the formula for calculating the actual volume of the sodium hydroxide standard solution consumed is: 。 9. The method for rapid analysis of total ester content in raw Baijiu (Chinese liquor) according to claim 4, characterized in that, Total ester content in the baijiu raw liquor sample X The calculation formula is: ; The simplified formula for calculating the total ester content is as follows: 。 10. The method for rapid analysis of total ester content in raw Baijiu (Chinese liquor) according to any one of claims 1-9, characterized in that, The alcohol content of the raw liquor is 25-75 vol.