CN115453022B - Method for rapidly judging formaldehyde content in white spirit - Google Patents
Method for rapidly judging formaldehyde content in white spirit Download PDFInfo
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- CN115453022B CN115453022B CN202211095261.7A CN202211095261A CN115453022B CN 115453022 B CN115453022 B CN 115453022B CN 202211095261 A CN202211095261 A CN 202211095261A CN 115453022 B CN115453022 B CN 115453022B
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 177
- 238000000034 method Methods 0.000 title claims abstract description 20
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 62
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 31
- 235000019253 formic acid Nutrition 0.000 claims abstract description 31
- 238000001514 detection method Methods 0.000 claims abstract description 26
- 239000000796 flavoring agent Substances 0.000 claims abstract description 7
- 235000019634 flavors Nutrition 0.000 claims abstract description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 51
- 239000000243 solution Substances 0.000 claims description 24
- 239000000523 sample Substances 0.000 claims description 23
- 239000012488 sample solution Substances 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000002347 injection Methods 0.000 claims description 8
- 239000007924 injection Substances 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 230000001419 dependent effect Effects 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 238000001212 derivatisation Methods 0.000 claims description 3
- 238000013499 data model Methods 0.000 claims description 2
- 238000010829 isocratic elution Methods 0.000 claims description 2
- 238000012417 linear regression Methods 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000004811 liquid chromatography Methods 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract 1
- HORQAOAYAYGIBM-UHFFFAOYSA-N 2,4-dinitrophenylhydrazine Chemical compound NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HORQAOAYAYGIBM-UHFFFAOYSA-N 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 4
- 239000007853 buffer solution Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 235000015096 spirit Nutrition 0.000 description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000001632 sodium acetate Substances 0.000 description 2
- 235000017281 sodium acetate Nutrition 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- ZGFPIGGZMWGPPW-UHFFFAOYSA-N formaldehyde;formic acid Chemical compound O=C.OC=O ZGFPIGGZMWGPPW-UHFFFAOYSA-N 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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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
-
- 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
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for rapidly judging formaldehyde content in white spirit, which utilizes liquid chromatography to detect formic acid and formaldehyde in white spirit with the same flavor in different years, establishes a corresponding relation model of formic acid and formaldehyde content, and can rapidly judge formaldehyde content in the white spirit by utilizing a formic acid content detection result in the white spirit body and combining the model. The method for judging the harmful formaldehyde in the wine body is high in speed, is an environment-friendly detection method capable of quickly identifying the harmful formaldehyde, is high in detection efficiency, does not involve toxic reagents in sample treatment, and is beneficial to environmental protection and occupational health safety.
Description
Technical Field
The invention relates to the technical field of white spirit detection, in particular to a method for rapidly judging formaldehyde content in white spirit.
Background
The white spirit is a special traditional product in China, has bright characteristics and has wide consumption groups. Meanwhile, the white spirit has unique cultural connotation and huge commercial value, so that the food safety problem of the white spirit is not ignored, and in recent years, the report of higher formaldehyde content of the commercially available white spirit is brought to the attention of consumers on the white spirit food safety problem, and the report brings negative influence to the white spirit consumer market. The flavor compounds in the white spirit are various in types, and various reactions, such as oxidation-reduction reaction, hydrolysis reaction, esterification reaction and the like, are continuously carried out on the flavor compounds in the ageing process, so that the change condition of formaldehyde indexes in the white spirit body needs to be paid attention to in order to ensure the quality safety of the white spirit product. At present, the detection method for the formaldehyde content in the wine body comprises an ultraviolet spectrophotometry, a gas chromatograph and a liquid chromatograph, a plurality of chemical reagents are needed in the detection process, the detection steps are complicated, the detection time is long, for example, the high-efficiency liquid phase method needs to use 2, 4-dinitrophenylhydrazine to derive formaldehyde in a sample, then the high-efficiency liquid phase method is used for quantitatively detecting the sample, the analysis time is long, and the 2, 4-dinitrophenylhydrazine has toxicity and is easy to cause environmental pollution and experimental damage.
Therefore, there is a need to design a method for rapidly determining formaldehyde content in white spirit, and a sample can be detected through simple treatment, so that the detection timeliness can be improved.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for rapidly judging the formaldehyde content in white spirit, which utilizes high performance liquid chromatography to detect the formaldehyde and formic acid content in white spirit samples with the same flavor in different years, respectively establishes a formaldehyde and formic acid correlation model, and then utilizes the formic acid content measurement result in the wine sample to be detected to rapidly judge the formaldehyde content in the wine sample to be detected.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for rapidly judging formaldehyde content in white spirit comprises the following steps:
(1) Determining the formic acid content in the white spirit product to be tested by utilizing high performance liquid chromatography;
(2) Establishing a relation model of formaldehyde and formic acid with corresponding flavor;
(3) And (3) rapidly calculating the formaldehyde content in the white spirit product to be measured based on the formic acid content in the white spirit product to be measured obtained in the step (1) and the model obtained in the step (2).
Preferably, in the step (2), white spirit products with different concentrations are filtered by a 0.22 mu organic microporous filter membrane to be used as a sample solution, and the sample solution is injected into a high performance liquid chromatograph to detect the content of the formic acid in the spirit sample.
Preferably, in the steps (1) and (2), the analysis conditions of the liquid chromatograph of the formic acid content detection method are as follows: using a C18 chromatographic column as an analytical chromatographic column; gradient eluting with acetonitrile 0.1% phosphoric acid solution for 0-7min and acetonitrile 2%;7-8min, acetonitrile 2-80%;8-13min, acetonitrile 80%;13-28min, acetonitrile 2%, flow rate 1.0mL/min, column temperature 30 ℃, sample injection amount 10 μl, and detection wavelength 210nm.
Preferably, in the step (2), the formaldehyde content in the wine body needs to be detected in the process of establishing the model of the invention. The analysis conditions of the liquid chromatograph used in the formaldehyde content detection method are as follows: using a C18 chromatographic column as an analytical chromatographic column; isocratic elution with methanol: water (68:32); the flow rate is 1.0mL/min, the column temperature is 40 ℃, the sample injection amount is 10 mu L, and the detection wavelength is 360nm.
Preferably, when the model is built in the step (2), the standard substance and the sample solution of the formaldehyde content detection method are firstly subjected to derivatization treatment, and the specific method comprises the following steps: respectively taking 1mL of formaldehyde standard substance series solution and 1.0mL of white spirit sample, placing into a 10mL volumetric flask, adding 2' 4-dinitrophenylhydrazine derivative solution to a scale mark, shaking uniformly, carrying out derivatization at 60 ℃ for 60 minutes, taking out, cooling to room temperature, and filtering by using a 0.22 mu m organic filter membrane to obtain the formaldehyde standard substance series solution.
Preferably, in the step (2), formic acid content data in the sample solution is required to be used as an independent variable, formaldehyde content in the corresponding wine sample is required to be used as a dependent variable, and a data model between the independent variable and the dependent variable is established by utilizing linear regression analysis.
Compared with the prior art, the invention has the following effects:
the method for rapidly judging the formaldehyde content in the wine body is simple, convenient and rapid, has high accuracy, can detect the formaldehyde content by simple treatment of the sample, greatly improves the detection timeliness, does not involve toxic reagents in sample treatment, and is beneficial to environmental protection and occupational health safety.
Drawings
FIG. 1 is a schematic diagram of a formaldehyde-formic acid content relationship model in an embodiment of the invention;
Detailed Description
The following detailed description of embodiments of the present application, taken in conjunction with the accompanying drawings and examples, uses terminology used in the description of the embodiments of the application to explain specific examples of the application only and is not intended to limit the application.
Example 1
And respectively taking strong aromatic Chinese liquor samples with ageing time of 0.5 years, 1 year, 3 years, 5 years, 7 years and 9 years, and developing the content detection of formic acid and formaldehyde to establish a relation model.
1.1 instruments
Liquid chromatograph: high performance liquid chromatograph equipped with ultraviolet detector or diode array detector, purchased from: agilent technologies Co., ltd.) electronic balance: one ten million electronic balance, model AB135-S, available from mertrer-tolidol. And (3) a water purifier: model: option R7-Flex2, available from Weily Water treatment technologies (Shanghai) Inc.
1.2 test drug
1.2.1 control: formaldehyde and formic acid standard substances are used for content determination.
1.2.2 acetonitrile, methanol, acetic acid, 2, 4-dinitrophenylhydrazine, sodium acetate: a chromatographic purity reagent; pure water is primary test water prepared by Option R7-Flex 2.
1.2.3 buffer solution: 2.6g of sodium acetate is weighed and dissolved in pure water, water is added to fix the volume to 500mL, acetic acid 0.5mL is added, and water is added to fix the volume to 500mL for standby.
1.2.4 2, 4-dinitrophenylhydrazine solution: accurately weighing a proper amount of 2, 4-dinitrophenylhydrazine into a volumetric flask, dissolving the 2, 4-dinitrophenylhydrazine in acetonitrile, and fixing the volume to prepare a solution containing 1.5mg of 2, 4-dinitrophenylhydrazine per milliliter for later use.
1.2.5 derivative liquid: mixing the buffer solution (2.3) with 2, 4-dinitrophenylhydrazine solution according to the formula 1:1, and is prepared by mixing according to the proportion.
1.3 preparation of formaldehyde test solution:
precisely sucking 1.0 mL-10 mL volumetric flask, adding derivative solution to scale, shaking, derivatizing at 60deg.C for 30 min, cooling to room temperature, and filtering with 0.22 μm needle filter to obtain sample solution.
1.4 preparation of formaldehyde standard substance solution:
precisely measuring a proper amount of formaldehyde standard substance, adding a buffer solution to dilute the formaldehyde standard substance to a certain concentration, precisely sucking the diluted formaldehyde standard substance solution into a 10mL volumetric flask, adding a derivative solution to a scale mark, shaking the flask uniformly, carrying out derivative at 60 ℃ for 30 minutes, cooling the flask to room temperature, and filtering the flask by a 0.22 mu m needle filter to obtain a sample solution.
1.5 Formaldehyde chromatography conditions:
chromatographic analysis was performed with a C18 column, eluting with methanol/water (60:40) isocratically at a flow rate of 1.0mL/min, a sample injection amount of 10. Mu.L, a column temperature of 35℃and a detection wavelength of 360nm.
1.6 determination of Formaldehyde content
And (3) the sample injection volumes of the standard substance solution and the sample solution are 10 mu L, and the standard substance solution and the sample solution are injected into a liquid chromatograph to respectively obtain the formaldehyde peak area in the standard substance solution and the formaldehyde peak area in the sample solution, the quality is improved according to the retention time, and the linear relation is established according to the peak area and the concentration of the standard substance solution, so that the formaldehyde in the sample solution is quantified.
1.7 preparation of formic acid sample solution
And filtering a proper amount of white spirit sample by using a 0.22 mu m needle filter to obtain the white spirit.
1.8 formic acid chromatographic conditions:
using a C18 chromatographic column as an analytical chromatographic column; gradient eluting with acetonitrile 0.1% phosphoric acid solution for 0-7min and acetonitrile 2%;7-8min, acetonitrile 2-80%;8-13min, acetonitrile 80%;13-28min and acetonitrile 2%. The flow rate is 1.0mL/min, the column temperature is 30 ℃, the sample injection amount of the test sample and the standard solution is 10 mu L, and the detection wavelength is 210nm.
1.9 determination of formic acid content
And (3) the sample injection volumes of the standard substance solution and the sample solution are 10 mu L, the standard substance solution and the sample solution are injected into a liquid chromatograph to respectively obtain the formic acid peak area in the standard substance solution and the formic acid peak area in the sample solution, the quality is improved according to the retention time, the linear relation is established according to the peak area and the concentration of the standard substance solution, and the formic acid in the sample solution is quantified.
The formaldehyde and formic acid content of the sample was determined as follows:
table 1: detection data in strong aromatic Chinese spirits
And establishing a correlation model of formic acid and formaldehyde in the Luzhou-flavor liquor by taking the formic acid content as an independent variable and the formaldehyde content as an independent variable, as shown in figure 1.
Detecting the formic acid content in the strong aromatic Chinese spirits to be detected, and then bringing the detected value into a model to calculate the formaldehyde content, wherein the detection result and the formaldehyde content measured by a liquid phase method are as shown in Table 2:
table 2: judgment of formaldehyde content in strong aromatic Chinese spirits
The method has the advantages that the relative deviation between the formaldehyde content in the wine body and the measured value of the liquid chromatography is less than 10% by using the model, the result shows that the established formaldehyde and formic acid content relation model is good in applicability for judging the formaldehyde content in the wine body, the detection of the formic acid content in the wine body is simple and easy, the use of derivative reagents polluting the environment is not needed, the detection time is greatly shortened, and the method is simple, practical, quick and accurate and is suitable for popularization and use.
Claims (1)
1. A method for rapidly judging formaldehyde content in white spirit is characterized by comprising the following steps:
(1) Filtering the distilled spirit products with different concentrations with 0.22 mu organic microporous filter membrane to obtain a sample solution, and injecting the sample solution into a high performance liquid chromatograph to detect the content of the formic acid in the distilled spirit sample; the analysis conditions of the liquid chromatograph of the formic acid content detection method are as follows: using a C18 chromatographic column as an analytical chromatographic column; gradient eluting with acetonitrile 0.1% phosphoric acid solution for 0-7min and acetonitrile 2%;7-8min, acetonitrile 2-80%;8-13min, acetonitrile 80%;13-28min, acetonitrile 2%, flow rate 1.0mL/min, column temperature 30 ℃, sample injection amount 10 μL, and detection wavelength 210nm;
detecting formaldehyde content in formaldehyde standard substances and test sample solutions, wherein the formaldehyde content detection method comprises the following steps of: using a C18 chromatographic column as an analytical chromatographic column; isocratic elution is carried out by methanol and water according to the proportion of 68:32, the flow rate is 1.0mL/min, the column temperature is 40 ℃, the sample injection amount is 10 mu L, and the detection wavelength is 360nm;
when a model is built, the formaldehyde standard substance and the sample solution are firstly subjected to derivatization treatment, and the specific method comprises the following steps: respectively taking 1mL of formaldehyde standard substance series solution and 1.0mL of white spirit sample, placing into a 10mL volumetric flask, adding 2' 4-dinitrophenylhydrazine derivative solution to a scale mark, shaking uniformly, carrying out derivative at 60 ℃ for 60 minutes, taking out, cooling to room temperature, and filtering with a 0.22 mu m organic filter membrane to obtain the formaldehyde standard substance series solution;
(2) Establishing a relation model of formaldehyde and formic acid with corresponding flavor: taking formic acid content data in the sample solution as independent variables, taking formaldehyde content in the sample solution as dependent variables, and establishing a data model between the independent variables and the dependent variables by utilizing linear regression analysis;
(3) And (3) rapidly calculating the formaldehyde content in the white spirit product to be measured based on the formic acid content in the white spirit product to be measured obtained in the step (1) and the model obtained in the step (2).
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| CN202211095261.7A CN115453022B (en) | 2022-09-06 | 2022-09-06 | Method for rapidly judging formaldehyde content in white spirit |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101762660A (en) * | 2010-01-08 | 2010-06-30 | 浙江出入境检验检疫局检验检疫技术中心 | Method for testing formaldehyde in food by means of derivation extraction |
| CN108088889A (en) * | 2016-11-21 | 2018-05-29 | 中国科学院大连化学物理研究所 | The device and method of negative ion mode ion mobility spectrometry on-line checking formaldehyde |
| CN110007039A (en) * | 2019-05-13 | 2019-07-12 | 四川轻化工大学 | Qualitative determination method and content determination method for formic acid in edible wine |
| CN113933406A (en) * | 2021-09-03 | 2022-01-14 | 贵州茅台酒厂（集团）习酒有限责任公司 | Method for detecting content of formaldehyde in white spirit sample |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200900689A (en) * | 2007-06-20 | 2009-01-01 | Dev Center Biotechnology | A device for detecting methanol concentration and the method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101762660A (en) * | 2010-01-08 | 2010-06-30 | 浙江出入境检验检疫局检验检疫技术中心 | Method for testing formaldehyde in food by means of derivation extraction |
| CN108088889A (en) * | 2016-11-21 | 2018-05-29 | 中国科学院大连化学物理研究所 | The device and method of negative ion mode ion mobility spectrometry on-line checking formaldehyde |
| CN110007039A (en) * | 2019-05-13 | 2019-07-12 | 四川轻化工大学 | Qualitative determination method and content determination method for formic acid in edible wine |
| CN113933406A (en) * | 2021-09-03 | 2022-01-14 | 贵州茅台酒厂（集团）习酒有限责任公司 | Method for detecting content of formaldehyde in white spirit sample |
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| Title |
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| HPLC法测定市售白酒中的甲醛含量;胡杨等;酿酒科技;第8卷;114-117 * |
| Use of Mass Spectrometry for the Determination of Formaldehyde in Samples Potentially Toxic to Humans: A Brief Review;Aline de Souza等;INTECH;253-272 * |
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