CN114018666A - Detection method of soybean isoflavone - Google Patents
Detection method of soybean isoflavone Download PDFInfo
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- CN114018666A CN114018666A CN202111300406.8A CN202111300406A CN114018666A CN 114018666 A CN114018666 A CN 114018666A CN 202111300406 A CN202111300406 A CN 202111300406A CN 114018666 A CN114018666 A CN 114018666A
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- soybean
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- methanol
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
Abstract
The invention discloses a method for detecting soybean isoflavone, which belongs to the technical field of medicines and comprises the following steps: crushing soybean raw materials, mixing the crushed soybean raw materials with a weak base aqueous solution, then carrying out catalytic treatment at a high temperature, adding a dilute hydrochloric acid aqueous solution to adjust the pH value, finally supplementing high-concentration alcohol, refluxing and dissolving, and filtering to obtain a sample solution. The method disclosed by the invention has the characteristics of simple detection steps and stable and accurate result, can greatly improve the detection authenticity of the soybean isoflavone in the raw material soybean, and has practical raw material quality evaluation significance for guiding soybean isoflavone extraction and production enterprises.
Description
Technical Field
The invention belongs to the technical field of medicines, and particularly relates to a method for detecting soybean isoflavone.
Background
The soybean isoflavone mainly exists in soybeans in the form of malonyl glucoside, and is converted into glucoside under the conditions of high temperature and water, the existing analysis methods all use the analysis of glucoside as a target substance, the existing quality analysis methods are based on GB/T23788-2009, the standard is a detection method of the soybean isoflavone in the health care product, the raw material is extracted by methanol or ethanol and then filtered to obtain a sample solution, the product is true and accurate, but the difference of the soybean isoflavone in the soybean raw material is large, and the detection basis of the soybean isoflavone in the raw material is lacked at present.
Disclosure of Invention
The invention aims to provide a method for detecting soybean isoflavone by aiming at the existing problems, and the method adopts an enhanced technology to carry out deep catalysis on malonyl, thereby greatly improving the detection authenticity of the soybean isoflavone in raw material soybeans and having practical raw material quality evaluation significance for guiding soybean isoflavone extraction and production enterprises.
The invention is realized by the following technical scheme:
a method for detecting soybean isoflavone comprises the following steps:
crushing soybean raw materials, mixing the crushed soybean raw materials with a weak base aqueous solution, then carrying out catalytic treatment at a high temperature, adding a dilute hydrochloric acid aqueous solution to adjust the pH value, finally supplementing high-concentration alcohol, refluxing and dissolving, and filtering to obtain a sample solution.
Further, the soybean raw material is at least one of whole soybeans, soybean meal and soybean germs.
Furthermore, the mass concentration of the solute in the weak base aqueous solution is 0.5-5%.
Further, the solute in the weak base aqueous solution is at least one of sodium carbonate, sodium bicarbonate, potassium carbonate and potassium bicarbonate.
Further, the temperature of the high-temperature condition is 80-100 ℃.
Further, the time length of the catalytic treatment is 2-5 hours.
Further, the pH value is 2-6.
Further, the high-concentration alcohol is an aqueous solution of methanol or ethanol.
Furthermore, the volume concentration of the high-concentration alcohol is 80-100%.
Compared with the prior art, the invention has the following advantages:
the method has the characteristics of simple detection steps and stable and accurate result, can greatly improve the detection authenticity of the soybean isoflavone in the raw material soybean, has practical raw material quality evaluation significance for guiding soybean isoflavone extraction and production enterprises, and has great popularization and application values.
Detailed Description
Example 1
Taking 10g of a whole soybean crushed sample, adding 100ml of 0.5% sodium carbonate aqueous solution, carrying out heat preservation and reflux for 2h at 80 ℃ in a water bath, pouring out an extracting solution, carrying out heat preservation and reflux for 1h at 80 ℃ by using 80% methanol aqueous solution, repeatedly extracting for 1 time by using methanol, combining 3 times of extracting solutions, adjusting the pH value to 2 by using dilute hydrochloric acid, filtering, and fixing the volume by using 80% methanol to obtain a sample solution, wherein the comparative detection results are shown in table 1.
Example 2
Taking 10g of a whole soybean crushed sample, adding 100ml of 0.5% sodium carbonate aqueous solution, carrying out heat preservation and reflux for 2h at 80 ℃ in a water bath, pouring out an extracting solution, carrying out heat preservation and reflux for 1h at 80 ℃ by using 80% methanol aqueous solution, repeatedly extracting for 1 time by using methanol, combining 3 times of extracting solutions, adjusting the pH value to 4 by using dilute hydrochloric acid, filtering, and fixing the volume by using 80% methanol to obtain a sample solution, wherein the comparative detection results are shown in table 1.
Example 3
Taking 10g of a whole soybean crushed sample, adding 100ml of 0.5% sodium carbonate aqueous solution, carrying out heat preservation and reflux for 2h at 80 ℃ in a water bath, pouring out an extracting solution, carrying out heat preservation and reflux for 1h at 80 ℃ by using 80% methanol aqueous solution, repeatedly extracting for 1 time by using methanol, combining 3 times of extracting solutions, adjusting the pH value to be 6 by using dilute hydrochloric acid, filtering, and fixing the volume by using 80% methanol to obtain a sample solution, wherein the comparative detection results are shown in table 1.
Example 4
Taking 10g of a whole soybean crushed sample, adding 100ml of 0.5% potassium carbonate aqueous solution, carrying out heat preservation and reflux for 2h at 80 ℃ in a water bath, pouring out an extracting solution, carrying out heat preservation and reflux for 1h at 80 ℃ by using 80% methanol aqueous solution, repeatedly extracting for 1 time by using methanol, combining 3 times of extracting solutions, adjusting the pH value to be 4 by using dilute hydrochloric acid, filtering, and fixing the volume by using 80% methanol to obtain a sample solution, wherein the comparative detection results are shown in table 1.
Example 5
Taking 10g of a whole soybean crushed sample, adding 100ml of 5% sodium carbonate aqueous solution, carrying out heat preservation and reflux for 2h at 80 ℃ in a water bath, pouring out an extracting solution, carrying out heat preservation and reflux for 1h at 80 ℃ by using 80% methanol aqueous solution, repeatedly carrying out methanol extraction for 1 time, combining 3 times of extracting solutions, adjusting the pH value to be 4 by using dilute hydrochloric acid, filtering, and carrying out constant volume by using 80% methanol to obtain a sample solution, wherein the comparative detection results are shown in table 1.
Example 6
Taking 10g of a whole soybean crushed sample, adding 100ml of 5% potassium carbonate aqueous solution, carrying out heat preservation reflux for 2h at 80 ℃ in a water bath, pouring out an extracting solution, carrying out heat preservation reflux for 1h at 80 ℃ by using 80% methanol aqueous solution, repeatedly carrying out methanol extraction for 1 time, combining 3 times of extracting solutions, adjusting the pH value to be 4 by using dilute hydrochloric acid, filtering, and carrying out constant volume by using 80% methanol to obtain a sample solution, wherein the comparative detection results are shown in table 1.
Example 7
Taking 10g of a whole soybean crushed sample, adding 100ml of 0.5% sodium carbonate aqueous solution, carrying out heat preservation and reflux for 2h at 90 ℃ in a water bath, pouring out an extracting solution, carrying out heat preservation and reflux for 1h at 80 ℃ by using 80% methanol aqueous solution, repeatedly extracting for 1 time by using methanol, combining 3 times of extracting solutions, adjusting the pH value to 4 by using dilute hydrochloric acid, filtering, and fixing the volume by using 80% methanol to obtain a sample solution, wherein the comparative detection results are shown in table 1.
Example 8
Taking 10g of a whole soybean crushed sample, adding 100ml of 0.5% sodium carbonate aqueous solution, carrying out heat preservation and reflux for 2h at 100 ℃ of an electric heating sleeve, pouring out an extracting solution, carrying out heat preservation and reflux for 1h at 80 ℃ by using 80% methanol aqueous solution, repeatedly extracting by using methanol for 1 time, combining 3 times of extracting solutions, adjusting the pH value to be 4 by using dilute hydrochloric acid, filtering, and fixing the volume by using 80% methanol to obtain a sample solution, wherein the comparative detection results are shown in table 1.
Example 9
Taking 10g of soybean meal, adding 100ml of 0.5% sodium carbonate aqueous solution, carrying out heat preservation and reflux for 2h at 80 ℃ in a water bath, pouring out an extracting solution, carrying out heat preservation and reflux for 1h at 80 ℃ by using 80% methanol aqueous solution, repeatedly carrying out methanol extraction for 1 time, combining 3 times of extracting solutions, adjusting the pH value to be 4 by using dilute hydrochloric acid, filtering, and carrying out constant volume by using 80% methanol to obtain a sample solution, wherein the comparative detection results are shown in table 1.
Example 10
Adding 10g soybean germ into 100ml 0.5% sodium carbonate aqueous solution, boiling and refluxing for 2h at 100 ℃ of an electric heating jacket, pouring out the extracting solution, preserving heat and refluxing for 1h at 80 ℃ by using 80% methanol aqueous solution, repeatedly extracting for 1 time by using methanol, combining the extracting solutions for 3 times, adjusting the pH value to 4 by using dilute hydrochloric acid, filtering, and fixing the volume by using 80% methanol to obtain a sample solution, wherein the comparative detection results are shown in Table 1.
Example 11
Adding 10g soybean germ into 100ml 0.5% sodium carbonate aqueous solution, boiling and refluxing for 2h at 80 ℃ in an electric heating sleeve, pouring out the extracting solution, preserving heat and refluxing for 1h at 80 ℃ by 100% methanol aqueous solution, repeatedly extracting for 1 time by methanol, combining the extracting solutions for 3 times, adjusting the pH value to 4 by dilute hydrochloric acid, filtering, and fixing the volume by 100% methanol to obtain a sample solution, wherein the comparative detection results are shown in Table 1.
Example 12
Adding 10g soybean germ into 100ml 0.5% sodium carbonate aqueous solution, boiling and refluxing for 2h at 80 ℃ in an electric heating sleeve, pouring out the extracting solution, preserving heat and refluxing for 1h at 80 ℃ by 80% methanol aqueous solution, repeatedly extracting for 1 time by methanol, combining the extracting solutions for 3 times, adjusting the pH value to 4 by dilute hydrochloric acid, filtering, and fixing the volume by 80% ethanol to obtain a sample solution, wherein the comparative detection results are shown in Table 1.
Example 13
Adding 10g soybean germ into 100ml 0.5% sodium carbonate aqueous solution, boiling and refluxing for 2h at 80 ℃ in an electric heating sleeve, pouring out the extracting solution, preserving heat and refluxing for 1h at 80 ℃ by using 100% ethanol aqueous solution, repeatedly extracting for 1 time by using methanol, combining the extracting solutions for 3 times, adjusting the pH value to 4 by using dilute hydrochloric acid, filtering, and fixing the volume by using 80% methanol to obtain a sample solution, wherein the comparative detection results are shown in Table 1.
Example 14
Adding 100ml of 0.5% sodium carbonate aqueous solution into 10g of soybean germ, boiling and refluxing for 5h at 100 ℃ of an electric heating jacket, pouring out an extracting solution, preserving heat and refluxing for 1h at 80 ℃ by using 80% methanol aqueous solution, repeatedly extracting for 1 time by using methanol, combining 3 times of extracting solutions, adjusting the pH value to be 4 by using dilute hydrochloric acid, filtering, fixing the volume by using 80% methanol to obtain a sample solution, and comparing and detecting results shown in table 1.
TABLE 1
As can be seen from the above table 1, the method of the present invention can significantly improve the accuracy of detection.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing description, it will be apparent to one skilled in the art that various changes, modifications, equivalents, and improvements may be made without departing from the spirit and scope of the invention.
Claims (9)
1. A method for detecting soybean isoflavone is characterized by comprising the following steps:
crushing soybean raw materials, mixing the crushed soybean raw materials with a weak base aqueous solution, then carrying out catalytic treatment at a high temperature, adding a dilute hydrochloric acid aqueous solution to adjust the pH value, finally supplementing high-concentration alcohol, refluxing and dissolving, and filtering to obtain a sample solution.
2. The method for detecting soybean isoflavones as claimed in claim 1, wherein the soybean material is at least one of whole soybeans, soybean meal and soybean germs.
3. The method for detecting soybean isoflavone according to claim 1, wherein the mass concentration of solute in the weak alkaline aqueous solution is 0.5-5%.
4. The method for detecting soybean isoflavone according to claim 1, wherein the solute in the weak alkaline aqueous solution is at least one of sodium carbonate, sodium bicarbonate, potassium carbonate and potassium bicarbonate.
5. The method for detecting soybean isoflavone according to claim 1, wherein the temperature of the high temperature condition is 80 to 100 ℃.
6. The method for detecting soybean isoflavones as claimed in claim 1, wherein the time period of the catalytic treatment is 2-5 h.
7. The method for detecting soybean isoflavones as claimed in claim 1, wherein the pH value is 2 to 6.
8. The method for detecting soybean isoflavones as claimed in claim 1, wherein the high-concentration alcohol is an aqueous solution of methanol or ethanol.
9. The method for detecting soybean isoflavone according to claim 8, wherein the volume concentration of the high concentration alcohol is 80-100%.
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| CN202111300406.8A CN114018666A (en) | 2021-11-04 | 2021-11-04 | Detection method of soybean isoflavone |
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Citations (11)
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| CN102977066A (en) * | 2012-12-07 | 2013-03-20 | 山东大学 | Method for extracting and purifying isoflavones in soybean |
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| KR20140069385A (en) * | 2012-11-28 | 2014-06-10 | 한국생명공학연구원 | Method for predicting isoflavone content in leguminous crop using prediction model of isoflavone content in leguminous crop |
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| CN105628845A (en) * | 2016-02-01 | 2016-06-01 | 北京理工大学 | Content measuring method of malonyl-ginsenoside |
| CN105777692A (en) * | 2016-03-18 | 2016-07-20 | 河南省农业科学院芝麻研究中心 | Method for extracting and determining soybean isoflavones |
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| CN101450958A (en) * | 2008-12-29 | 2009-06-10 | 天津理工大学 | Synthetic method of isoflavone 7-O-glucose glycoside |
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