CN113092570A - Method for rapidly measuring quality and picking wine based on in-situ direct mass spectrometry - Google Patents
Method for rapidly measuring quality and picking wine based on in-situ direct mass spectrometry Download PDFInfo
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Abstract
The invention discloses a method for quickly measuring and picking liquor based on in-situ mass spectrum, which comprises the following steps of (1) taking the in-situ mass spectrum as a real-time on-line monitoring sensor for liquor components; (2) simultaneously carrying out primary and secondary mass spectrum data acquisition on key trace components in the white spirit, and carrying out quantitative calculation; (3) respectively giving calculation weights to the key micro-component data acquired in the step (2) according to different requirements on the taste of the white spirit; (4) and after the calculation weight is given, establishing a mathematical model for the rapid grading identification of the white spirit. The method has the advantages that 7 trace components of glycolic acid, ethyl caproate, ethyl acetate, methanol, ethyl lactate, acetic acid and butyric acid in the white spirit can be detected simultaneously in real time and rapidly by using the in-situ mass spectrum, and the distilled white spirit can be accurately and rapidly divided into three different grades of the head, the body and the tail according to the variety and the content change of the components.
Description
Technical Field
The invention belongs to the technical field of food processing, and particularly relates to a method for quickly measuring quality and picking wine based on in-situ mass spectrometry.
Background
Quality measurement and liquor taking are important process links for producing white spirit. During the distillation of white spirit, the quality of the white spirit flowing out in different time periods is different, and workers need to classify the white spirit and pick the white spirit, so that a foundation is laid for subsequent flavor blending. At present, the liquor picking process mainly depends on subjective experiences of workers such as 'tasting and picking liquor', 'watching flowers and measuring' to pick liquor, and quality fluctuation is easily caused. The liquor has at least hundreds of flavor components and relatively low content. The current on-line analysis and detection of white spirit comprises spectroscopy and chromatography detection methods. The spectroscopic method cannot accurately and quantitatively detect trace components, and the chromatographic separation detection technology has a long detection period, so that the online and real-time detection requirements of liquor picking by a machine are difficult to meet. For a long time, due to the lack of high-sensitivity sensors, liquor is picked up by a machine with great challenges and breakthrough is not realized yet.
The principle of in situ direct mass spectrometry (DART-MS) is that under normal environmental conditions, a gas (e.g., helium or argon) instantaneously desorbs and ionizes compound molecules in a sample via excited-state atoms generated by an electrical discharge. Compared with the existing gas mass spectrometry combined technology, the direct mass spectrometry does not need complicated sample preparation and time-consuming chromatographic separation, and an analysis result can be obtained within 5-10 seconds, so that the sample analysis time is shortened rapidly. Although this technology is currently commercialized. However, the research on the rapid real-time online grading of distilled liquor by using the technology has not been reported. The difference of the white spirit components in different sections mainly depends on trace components. The DART-MS technology is innovatively utilized, meanwhile, the chemical knowledge of the flavor of the white spirit is utilized, and chemometrics modeling is combined, so that intelligent and rapid online recognition of the white spirits with different grades is finally achieved, research results inevitably improve the grading recognition efficiency of the white spirit greatly, and the method has great economic benefits especially for application in mechanical liquor picking. The intelligent and automatic white spirit production management system is very necessary for guaranteeing the quality of white spirit and realizing the intelligent and automatic management of the production process.
Disclosure of Invention
In order to solve the problem that the foreshot, the wine body and the feints in the existing high-concentration white spirit distillation technology cannot be effectively and quickly identified and intelligently classified by a machine, the invention provides a method for quickly picking the white spirit with quality based on an in-situ mass spectrum.
In order to achieve the purpose, the technical scheme of the invention is as follows: the invention provides a method for quickly measuring quality and taking wine, which comprises the following steps: (1) taking an in-situ mass spectrum as a real-time online monitoring sensor for white spirit components;
(2) simultaneously carrying out primary and secondary mass spectrum data acquisition on key trace components in the white spirit, and carrying out quantitative calculation;
(3) respectively giving calculation weights to the key micro-component data acquired in the step (2) according to different requirements on the taste of the white spirit;
(4) and after the calculation weight is given, establishing a mathematical model for the rapid grading identification of the white spirit.
Further, the in-situ MASs spectrometry (DART-MAS) in step (1) refers to an ionization source that generates plasma by high-pressure discharge of argon, helium or nitrogen in an atmospheric pressure environment, and the ionization source is connected with a MASs spectrometer detector in series.
Further, the key trace components in the step (2) are 7 trace components of glycolic acid, ethyl caproate, ethyl acetate, methanol, ethyl lactate, acetic acid and butyric acid.
Furthermore, according to the taste requirements of different white spirits, different weights are given to the key micro-component data in the step (2), wherein the weights are in the range of 1 for calculation of glycolic acid, 2-3 for ethyl hexanoate, 2-3 for ethyl acetate, 0.9-2 for methanol, 2-3 for ethyl lactate, 0.9-2 for acetic acid and 0.9-2 for butyric acid.
Further, the mathematical model in the step (4) is a partial least square or Fisher stepwise discriminant analysis or orthogonal partial least square discriminant analysis mathematical model.
By adopting the technical scheme, the invention has the beneficial effects that: the method can be used for rapidly detecting 7 trace components of glycolic acid, ethyl caproate, ethyl acetate, methanol, ethyl lactate, acetic acid and butyric acid in the white spirit by adopting an in-situ mass spectrum, and accurately and rapidly dividing the distilled white spirit into three sections of a spirit head, a spirit body and a spirit tail according to the variety and content change of the components.
Detailed Description
The present invention is described in further detail below with reference to specific examples. It should be noted that the examples are illustrative only and are not to be construed as limiting the invention. In addition, all reagents used in the following examples are commercially available or can be synthesized according to methods herein or known, and are readily available to those skilled in the art for reaction conditions not listed, if not explicitly stated.
The invention will be further explained by the following technical solutions.
The first embodiment is as follows: according to the method for quickly taking liquor with quality, provided by the invention, liquor in different distillation time periods is divided into three types of liquor head, liquor body and liquor tail by adopting a sensory evaluation mode. In an open typeThe in-situ mass spectrum is taken as a sensor, and argon is taken as working gas. (1) Calculating the contents of 7 trace components of glycolic acid, ethyl caproate, ethyl acetate, methanol, ethyl lactate, acetic acid and butyric acid in the three types of white spirits according to a first-level mass spectrum; (2) after the glycolic acid weight is given as 1, the ethyl caproate weight, the ethyl acetate weight and the ethyl lactate weight are given as 2, and the methanol weight, the acetic acid weight and the butyric acid weight are given as 0.9, the weight content calculation is carried out on the 7 components; (3) according to the weight content result, a partial least square discriminant analysis model (P is less than 0.05) is established, and through 100 times of random sampling diagnosis simulation, the accuracy of separating the three types of white spirits of the foreshot, the body and the tail is 90.7 +/-1.2%.
Example two: according to the method for quickly taking liquor with quality, provided by the invention, liquor in different distillation time periods is divided into three types of liquor head, liquor body and liquor tail by adopting a sensory evaluation mode. And (3) performing in-situ mass spectrometry by using dielectric barrier discharge and taking helium as a working gas. (1) Calculating the contents of 7 trace components of glycolic acid, ethyl caproate, ethyl acetate, methanol, ethyl lactate, acetic acid and butyric acid in the three types of white spirits according to second-level mass spectrum data; (2) after the glycolic acid weight 1, the ethyl caproate weight 3, the ethyl acetate weight 3 and the ethyl lactate weight 1.5 are given, the weight content of the 7 components is calculated; (3) according to the result of the empowerment content, a Fisher stepwise discriminant analysis model (P is less than 0.05) is established, and the accuracy of separating the three types of white spirits of the head, the body and the tail of the white spirits is 93.2 +/-2.3% through 100 times of random sampling diagnosis simulation.
Example three: according to the method for quickly taking liquor with quality, provided by the invention, liquor in different distillation time periods is divided into three types of liquor head, liquor body and liquor tail by adopting a sensory evaluation mode. And (3) dielectric barrier discharge in-situ mass spectrometry is adopted, and nitrogen is taken as a working gas. (1) Calculating the contents of 7 trace components of glycolic acid, ethyl caproate, ethyl acetate, methanol, ethyl lactate, acetic acid and butyric acid in the three types of white spirits according to second-level mass spectrum data; (2) glycolic acid weight 1, ethyl hexanoate, ethyl acetate and ethyl lactate weight 3, methanol, acetic acid, butyric acid weight 2. Performing weight-endowing content calculation on the 7 components; (3) an orthogonal partial least square discriminant analysis model (P is less than 0.05) is established, and through 100 times of random sampling diagnosis simulation, the accuracy of separating the three types of white spirits of the wine head, the wine body and the wine tail is 94.7 +/-3.2%.
Comparative example one:
different weight coefficients are adopted to endow glycolic acid weight 1, ethyl caproate, ethyl acetate and ethyl lactate weight 1, and methanol, acetic acid and butyric acid weight 1. The rest of the conditions were exactly the same as in the first example. Through 100 times of random sampling diagnosis simulation, the accuracy of separating the three types of white spirits of the foreshot, the body and the feints is only 60.7 +/-2.2%. The weight coefficient is proved to significantly influence the model identification rate.
Comparative example two:
the method adopts 8 trace components of glycolic acid, ethyl caproate, ethyl acetate, methanol, ethyl lactate, acetic acid, butyric acid and caproic acid for detection. The rest of the conditions were exactly the same as in the first example. Through 100 times of random sampling diagnosis simulation, the accuracy of separating the three types of white spirits of the foreshot, the body and the feints is only 73.3 +/-7.2%. The trace component calculation is proved to be added, so that the model identification rate can be obviously influenced.
Comparative example three:
the detection is carried out by 5 trace components of glycolic acid, ethyl caproate, ethyl acetate, methanol and ethyl lactate, and the rest conditions are completely the same as the first embodiment. Through 100 times of random sampling diagnosis simulation, the accuracy of separating the three types of white spirits of the foreshot, the body and the feints is only 63.8 +/-5.2%. The trace component calculation is reduced, and the model identification rate can be obviously influenced.
The technical solutions described above only represent the preferred technical solutions of the present invention, and some possible modifications to some parts of the technical solutions by those skilled in the art all represent the principles of the present invention, and fall within the protection scope of the present invention.
Claims (5)
1. A method for rapidly measuring quality of liquor based on in-situ mass spectrometry is characterized by comprising the following steps:
(1) taking an in-situ mass spectrum as a real-time online monitoring sensor for white spirit components;
(2) simultaneously carrying out primary and secondary mass spectrum data acquisition on key trace components in the white spirit, and carrying out quantitative calculation;
(3) respectively giving calculation weights to the key micro-component data acquired in the step (2) according to different requirements on the taste of the white spirit;
(4) and after the calculation weight is given, establishing a mathematical model for the rapid grading identification of the white spirit.
2. The method of claim 1, wherein the in-situ mass spectrometry of step (1) refers to an ionization source that generates plasma by high-pressure discharge of argon, helium or nitrogen in an atmospheric environment, and the ionization source is connected with a mass spectrometer detector in series.
3. The method according to claim 1, wherein the critical minor components in step (2) are 7 minor components selected from glycolic acid, ethyl hexanoate, ethyl acetate, methanol, ethyl lactate, acetic acid, butyric acid.
4. The method according to claim 1 or 3, wherein the key minor constituent data in step (2) are weighted differently according to the taste requirements of different white spirits, and the weighting ranges are that glycolic acid is given a calculation weight of 1, ethyl hexanoate is given a weight of 2-3, ethyl acetate is given a calculation weight of 2-3, methanol is given a calculation weight of 0.9-2, ethyl lactate is given a calculation weight of 2-3, acetic acid is given a calculation weight of 0.9-2, and butyric acid is given a calculation weight of 0.9-2.
5. The method according to claim 1, wherein the mathematical model in step (4) is a partial least squares or Fisher stepwise discriminant analysis or an orthogonal partial least squares discriminant analysis mathematical model.
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CN107894454A (en) * | 2017-11-14 | 2018-04-10 | 长春中医药大学 | A kind of mass spectral analysis model of quick nondestructive diagnosis of breast diseases |
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