CN112834651A - Method for extracting phillyrin from forsythia suspense leaves - Google Patents
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Abstract
The invention discloses a method for extracting phillyrin from forsythia suspense leaves, which comprises the following steps: extracting folium forsythiae with water, respectively examining the influence of water addition, extraction temperature, extraction frequency and extraction time on phillyrin yield by single factor test, and extracting with L9(34) Determining the optimal extraction process of phillyrin in forsythia suspense leaves by an orthogonal experimental method; the best extraction process is as follows: extracting with 20 times of water at 90 deg.C for 2 times, each time for 60min, and the yield of phillyrin in folium forsythiae can reach 5.45%. The method for extracting the phillyrin adopts water as an extraction solvent, has the advantages of low production cost, no pollution to the environment, convenient extraction operation, safety and high efficiency, high phillyrin extraction rate and good quality, and provides a reference basis for the development and utilization of phillyrin leaf resources.
Description
Technical Field
The invention relates to an extraction method, in particular to a method for extracting phillyrin from forsythia suspense leaves.
Background
Phillyrin is used as an effective component in forsythia suspense leaves, has the effects of resisting bacteria, viruses, oxidation, lipid and liver, and the like, in recent years, the development of forsythia suspense fruit resources is relatively wide, but forsythia suspense leaf resources are wasted greatly, but researches prove that the content of phillyrin in forsythia suspense leaves is 40 times higher than that of old forsythia suspense and 2-4 times higher than that of green forsythia suspense, the forsythia suspense leaves have eating habits and history records in folk, and the results of six toxicity studies such as acute oral toxicity tests and 90d oral toxicity tests of forsythia suspense leaves carried out by Shanxi province disease prevention and control centers show that the forsythia suspense leaves have edible safety. Therefore, the original national health and family planning committee of 2017 approved the new food raw materials of forsythia suspense leaves to be stopped from examination, meanwhile, the Shanxi province issued "food safety local standard forsythia suspense leaves" DBS14-001-2017, and forsythia suspense leaves are listed as food category firstly in the whole country for management. In recent years, there are many extraction processes related to phillyrin, such as alcoholic solvent extraction, ultrasonic-assisted extraction, microwave-assisted extraction and the like, and in view of high production cost of alcoholic solvent extraction and ultrasonic-assisted extraction and environmental pollution, microwave-assisted extraction is not suitable for industrial mass production.
Disclosure of Invention
The invention aims to provide a method for extracting phillyrin from forsythia suspense leaves, wherein the forsythia suspense leaves are extracted by water, the influence of water addition, extraction temperature, extraction times and extraction time on the yield of phillyrin is respectively inspected by adopting a single-factor test, and L is adopted9(34) Determining the optimal extraction process of phillyrin in forsythia suspense leaves by an orthogonal experimental method; the method for extracting the phillyrin adopts water as an extraction solvent, has the advantages of low production cost, no environmental pollution, convenient extraction operation, safety, high efficiency, high phillyrin extraction rate and good quality, and provides a reference basis for the development and utilization of phillyrin leaf resources.
The purpose of the invention can be realized by the following technical scheme:
a method for extracting phillyrin from folium forsythiae comprises extracting folium forsythiae with water, respectively examining the influence of water addition, extraction temperature, extraction frequency and extraction time on phillyrin yield by single factor test, and adopting L9(34) The optimal extraction process of phillyrin in forsythia suspense leaves is determined by an orthogonal experimental method, and the extraction method comprises the following steps:
s1, determining chromatographic conditions;
s2 drawing standard curve of reference solution
S2S1, weighing 5.00mg of phillyrin reference substance which is dried to constant weight, and placing the phillyrin reference substance in a 50mL volumetric flask;
S2S2, adding 50mL of methanol to dissolve to a constant volume, shaking up, and filtering before sample injection;
S2S3, sucking a reference substance solution by 0.2mL, 0.4mL, 0.5mL, 0.8mL, 1mL, 2mL, 5mL and 10mL, putting the reference substance solution in a 10mL volumetric flask, fixing the volume and shaking up;
S2S4, drawing a standard curve according to the concentration and peak area of the phillyrin reference substance to obtain the concentration range of the reference substance solution;
s3 sample solution preparation by single factor test
S3S1, crushing the weeping forsythia leaves, and sieving the weeping forsythia leaves by a sieve;
S3S2, weighing 10g of forsythia suspense leaf powder, adding 20-volume-of-water, boiling at 80 ℃ for 40min, and filtering;
S3S3, mixing and concentrating the filtrate to 100mL, putting 10mL of extracting solution into a 50mL volumetric flask, metering the volume to a scale mark with methanol, and shaking up to be used as a sample solution for later use;
S3S4, respectively selecting 4 factors of water addition amount, extraction temperature, extraction times and extraction time to perform single-factor test when other conditions are the same;
s4, selecting 4 factors of water addition, extraction temperature, extraction times and extraction time as investigation factors on the basis of single factor test, setting 3 levels for each factor, and using L9(34) The orthogonal table is tested to determine the optimal process conditions;
s5, accurately weighing 9 parts of 10g of forsythia suspense leaf powder, extracting according to the conditions of an orthogonal table, comparing by taking the content of phillyrin as an investigation index, and determining the optimal extraction conditions.
Further, the mass volume of mobile phase acetonitrile and water in the chromatographic conditions is 21: 79; the flow rate was 0.8 mL/min-1The detection wavelength is 277nm, the column temperature is room temperature, the sample injection amount is 10 mu L, and the average value is obtained by three times of sample injection.
Further, in the step S2S2, a 0.22 μm organic filter membrane is used for filtration.
Further, the filtering in the step S3S2 adopts three layers of gauze and filters twice.
Further, the extraction test steps of different water adding amounts in the step S3S4 are as follows:
(1) weighing folium forsythiae powder, setting water addition gradient, and extracting at 80 deg.C for 60min for 2 times;
(2) evaporating and concentrating the sample solution to 50mL, taking 10mL of sample solution, metering the volume of the sample solution to a 50mL volumetric flask by using methanol, and shaking up;
(3) the peak area thereof was detected under the chromatographic conditions of step S1, and the concentration thereof was calculated.
Further, the different temperature extraction test step in the step S3S4 is as follows:
(1) precisely weighing 5 parts of 10g of forsythia suspense leaf powder, respectively adding 150mL of water, and extracting for 2 times at 60, 70, 80, 90 and 100 ℃ for 60min each time;
(2) evaporating and concentrating 5 parts of sample solution to 50mL, taking 10mL of sample solution, diluting with methanol to a constant volume in a 50mL volumetric flask, and shaking up;
(3) the peak area thereof was detected under the chromatographic conditions of step S1, and the concentration thereof was calculated.
Further, the step S3S4 includes the following steps:
(1) precisely weighing 5 parts of 10g of forsythia suspense leaf powder, respectively adding 150mL of water, and respectively extracting for 1, 2, 3, 4 and 5 times at 80 ℃ for 60min each time;
(2) evaporating and concentrating 5 parts of sample solution to 50mL, taking 10mL of sample solution, diluting with methanol to a constant volume in a 50mL volumetric flask, and shaking up;
(3) the peak area thereof was detected under the chromatographic conditions of step S1, and the concentration thereof was calculated.
Further, the step S3S4 includes, at different times, the step of extracting a test:
(1) precisely weighing 5 parts of 10g of forsythia suspense leaf powder, respectively adding 150mL of water, and extracting for 2 times at 80 ℃ for 20 min, 30 min, 40min, 50 min and 60 min;
(2) evaporating and concentrating 5 parts of sample solution to 50mL, taking 10mL of sample solution, diluting with methanol to a constant volume in a 50mL volumetric flask, and shaking up;
(3) the peak area thereof was detected under the chromatographic conditions in step S1, and the concentration thereof was calculated.
The invention has the beneficial effects that:
the method for extracting the phillyrin adopts water as an extraction solvent, has the advantages of low production cost, no pollution to the environment, convenient extraction operation, safety and high efficiency, high phillyrin extraction rate and good quality, and provides a reference basis for the development and utilization of phillyrin leaf resources.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a schematic diagram showing the relationship between the amount of water added and the concentration of phillyrin in the present invention;
FIG. 2 is a schematic diagram showing the relationship between the extraction temperature and the forsythin concentration according to the present invention;
FIG. 3 is a schematic diagram showing the relationship between the extraction frequency and the forsythin concentration;
FIG. 4 is a schematic diagram showing the relationship between the extraction time and the forsythin concentration in the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for extracting phillyrin from folium forsythiae comprises:
s1, chromatographic conditions: thermo chromatography column (4.6mm 250mm,5 μm); the mobile phase is acetonitrile: water 21: 79; the flow rate was 0.8 mL/min-1(ii) a The detection wavelength is 277 nm; the column temperature is room temperature; sampling 10 mu L, sampling three times and taking an average value;
s2, drawing a standard curve: preparation method of reference substance solution
S2S1, precisely weighing 5.00mg of phillyrin reference sample which is dried to constant weight, and placing the phillyrin reference sample in a 50mL volumetric flask;
S2S2, adding 50mL of methanol to dissolve to a constant volume, and shaking up to obtain a mass concentration of 0.100 mg/mL-1The phillyrin reference substance solution is filtered by a 0.22 mu m organic filter membrane before sample injection;
S2S3, precisely sucking a reference substance solution by 0.2mL, 0.4mL, 0.5mL, 0.8mL, 1mL, 2mL, 5mL and 10mL, namely diluting by 50, 25, 12.5, 10, 5, 2 and 1 times, putting the solution into a 10mL volumetric flask, fixing the volume and shaking up;
S2S4, obtaining a regression equation by taking the concentration (X) of the phillyrin reference substance as a horizontal coordinate and taking the peak area (Y) as a vertical coordinate: 14868X +27.465, R2＝0.9987，(R2Representing the degree of coincidence between the data and the function) shows that the forsythin reference substance is 0.002-0.1 mg/mL-1Within the range, the linear relationship is good;
s3, single factor test: method for preparing sample solution
S3S1, crushing the weeping forsythia leaves, and sieving the weeping forsythia leaves with a forty-mesh sieve;
S3S2, accurately weighing 10g of forsythia suspense leaf powder, adding 20-fold water, boiling for 40min at 80 ℃, and filtering twice by using three layers of gauze;
S3S3, mixing and concentrating the filtrate to 100mL, putting 10mL of extracting solution into a 50mL volumetric flask, metering the volume to a scale mark with methanol, and shaking up to be used as a sample solution for later use;
S3S4, when other conditions are the same, selecting 4 factors of water addition amount, extraction temperature, extraction times and extraction time respectively, and performing single-factor test to provide reference for setting the factor level in the orthogonal test;
S3S4S1, and extraction test steps of different water adding amounts:
(1) precisely weighing 5 parts of 10g of forsythia suspense leaf powder, respectively setting the water adding amount to be 10, 15, 20, 25 and 30 times, namely 100, 150, 200, 250 and 300mL, and extracting for 2 times at 80 ℃ for 60min each time;
(2) evaporating and concentrating 5 parts of sample solution to 50mL, taking 10mL of sample solution, diluting with methanol to a constant volume in a 50mL volumetric flask, and shaking up;
(3) the peak area was measured under chromatographic conditions in step S1, and the concentration was calculated, as shown in fig. 1, indicating that: the phillyrin concentration obtained by adding 15 times of water is highest.
S3S4S2, and different-temperature extraction test steps:
(1) precisely weighing 5 parts of 10g of forsythia suspense leaf powder, respectively adding 150mL of water, and extracting for 2 times at 60, 70, 80, 90 and 100 ℃ for 60min each time;
(2) evaporating and concentrating 5 parts of sample solution to 50mL, taking 10mL of sample solution, diluting with methanol to a constant volume in a 50mL volumetric flask, and shaking up;
(3) the peak area was measured under the chromatographic conditions of step S1, and the concentration was calculated, as shown in FIG. 2, whereby the forsythin concentration was the highest at 80 ℃.
S3S4S3, and different times of extraction test steps:
(1) precisely weighing 5 parts of 10g of forsythia suspense leaf powder, respectively adding 150mL of water, and respectively extracting for 1, 2, 3, 4 and 5 times at 80 ℃ for 60min each time;
(2) evaporating and concentrating 5 parts of sample solution to 50mL, taking 10mL of sample solution, diluting with methanol to a constant volume in a 50mL volumetric flask, and shaking up;
(3) the peak area was measured under the chromatographic conditions of step S1, and the concentration was calculated, as shown in fig. 3, resulting in the highest forsythin concentration obtained by 4 extractions.
S3S4S4, and extracting and testing at different time:
(1) precisely weighing 5 parts of 10g of forsythia suspense leaf powder, respectively adding 150mL of water, and extracting for 2 times at 80 ℃ for 20 min, 30 min, 40min, 50 min and 60 min;
(2) evaporating and concentrating 5 parts of sample solution to 50mL, taking 10mL of sample solution, diluting with methanol to a constant volume in a 50mL volumetric flask, and shaking up;
(3) the peak area was detected under the chromatographic conditions in step S1, and the concentration was calculated, as shown in FIG. 4, with the result that the forsythin concentration was the highest at an extraction time of 40 min.
S4, selecting four factors of water addition amount (A), extraction temperature (B), extraction times (C) and extraction time (D) as investigation factors on the basis of single-factor test, setting 3 levels for each factor, and using L9(34) The orthogonal table was tested to determine the optimum process conditions.
TABLE 1 orthogonal test factor horizon
S5, accurately weighing 9 parts of 10g forsythia suspense leaf powder, extracting according to the conditions of an orthogonal table, comparing by taking the content of phillyrin as an investigation index, determining the optimal extraction conditions, wherein the test results are shown in a table 2, and the anova results are shown in a table 3.
TABLE 2 orthogonal experimental design and results
TABLE 3 analysis of variance
As can be seen from Table 2, the major and minor factors affecting the forsythin content are: b is more than A and more than C is more than D, the most obvious influence factor is extraction temperature, extraction time has the smallest influence on the extraction of the phillyrin, so the phillyrin is analyzed as an error term in the table 3, 2 times of extraction and 20 times of water addition are selected from the consideration of saving cost, therefore, the optimal extraction condition is 20 times of water addition, the phillyrin is extracted for 2 times at 90 ℃, and the content of the phillyrin can reach 5.45 percent each time for 60 min.
Example 1: crushing forsythia suspense leaves into tea powder by using a high-speed grinder, weighing 10g of tea powder, adding 15 times of water, extracting for 4 times at 90 ℃ for 80min each time, filtering out filtrate by using gauze, combining the filtrate for 2 times, concentrating to 50mL by using a rotary evaporator, taking 10mL of sample solution, metering volume to a 50mL volumetric flask by using methanol, shaking up, and detecting the content of phillyrin to be 5.18% by using a high-performance liquid phase.
Example 2: crushing forsythia suspense leaves into tea powder by using a high-speed grinder, weighing 10g of the tea powder, adding 20 times of water, extracting for 2 times at 90 ℃ for 60min each time, filtering out filtrate by using gauze, combining the filtrate obtained for 2 times, concentrating the filtrate to 50mL by using a rotary evaporator, taking 10mL of sample solution, metering the volume of the sample solution to a 50mL volumetric flask by using methanol, shaking up the sample solution, and detecting the content of phillyrin in the sample solution to be 5.45% by using a high-performance liquid phase.
The result shows that the phillyrin is extracted for 2 times at 90 ℃ by adding 20 times of water, and the content of the phillyrin obtained is the highest after 60min each time, which is superior to other conditions.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (8)
1. A method for extracting phillyrin from forsythia suspense leaves is characterized in that the forsythia suspense leaves are extracted by water, the influence of water addition, extraction temperature, extraction times and extraction time on the yield of phillyrin is respectively inspected by adopting a single-factor test, and L is adopted9(34) The optimal extraction process of phillyrin in forsythia suspense leaves is determined by an orthogonal experimental method, and the extraction method comprises the following steps:
s1, determining chromatographic conditions;
s2 drawing standard curve of reference solution
S2S1, weighing 5.00mg of phillyrin reference substance which is dried to constant weight, and placing the phillyrin reference substance in a 50mL volumetric flask;
S2S2, adding 50mL of methanol to dissolve to a constant volume, shaking up, and filtering before sample injection;
S2S3, sucking a reference substance solution by 0.2mL, 0.4mL, 0.5mL, 0.8mL, 1mL, 2mL, 5mL and 10mL, putting the reference substance solution in a 10mL volumetric flask, fixing the volume and shaking up;
S2S4, drawing a standard curve according to the concentration and peak area of the phillyrin reference substance to obtain the concentration range of the reference substance solution;
s3 sample solution preparation by single factor test
S3S1, crushing the weeping forsythia leaves, and sieving the weeping forsythia leaves by a sieve;
S3S2, weighing 10g of forsythia suspense leaf powder, adding 20-volume-of-water, boiling at 80 ℃ for 40min, and filtering;
S3S3, mixing and concentrating the filtrate to 100mL, putting 10mL of extracting solution into a 50mL volumetric flask, metering the volume to a scale mark with methanol, and shaking up to be used as a sample solution for later use;
S3S4, respectively selecting 4 factors of water addition amount, extraction temperature, extraction times and extraction time to perform single-factor test when other conditions are the same;
s4, selecting 4 factors of water addition, extraction temperature, extraction times and extraction time as investigation factors on the basis of single factor test, setting 3 levels for each factor, and using L9(34) The orthogonal table is tested to determine the optimal process conditions;
s5, accurately weighing 9 parts of 10g of forsythia suspense leaf powder, extracting according to the conditions of an orthogonal table, comparing by taking the content of phillyrin as an investigation index, and determining the optimal extraction conditions.
2. The method for extracting phillyrin from forsythia suspense leaves according to claim 1, wherein the volume ratio of mobile phase acetonitrile to water in the chromatographic condition is 21: 79; 20.8 mL min-1The detection wavelength is 277nm, the column temperature is room temperature, the sample injection amount is 10 mu L, and the average value is obtained by three times of sample injection.
3. The method for extracting forsythin from forsythia suspense leaves as claimed in claim 1, wherein a 0.22 μm organic filter membrane is used for filtration in the step S2S 2.
4. The method for extracting forsythin from forsythia suspense leaves as claimed in claim 1, wherein the filtering in the step S3S2 adopts three layers of gauze and filtering twice.
5. The method for extracting forsythin from forsythia suspense leaves as claimed in claim 1, wherein the extraction test steps of different water addition amounts in the step S3S4 are as follows:
(1) weighing folium forsythiae powder, setting water addition gradient, and extracting at 80 deg.C for 60min for 2 times;
(2) evaporating and concentrating the sample solution to 50mL, taking 10mL of sample solution, metering the volume of the sample solution to a 50mL volumetric flask by using methanol, and shaking up;
(3) the peak area thereof was detected under the chromatographic conditions of step S1, and the concentration thereof was calculated.
6. The method for extracting forsythin from forsythia suspense leaves as claimed in claim 1, wherein the different temperature extraction test steps in the step S3S4 are as follows:
(1) precisely weighing 5 parts of 10g of forsythia suspense leaf powder, respectively adding 150mL of water, and extracting for 2 times at 60, 70, 80, 90 and 100 ℃ for 60min each time;
(2) evaporating and concentrating 5 parts of sample solution to 50mL, taking 10mL of sample solution, diluting with methanol to a constant volume in a 50mL volumetric flask, and shaking up;
(3) the peak area thereof was detected under the chromatographic conditions of step S1, and the concentration thereof was calculated.
7. The method for extracting forsythin from forsythia suspense leaves as claimed in claim 1, wherein the different times of extraction test steps in the step S3S4 are as follows:
(1) precisely weighing 5 parts of 10g of forsythia suspense leaf powder, respectively adding 150mL of water, and respectively extracting for 1, 2, 3, 4 and 5 times at 80 ℃ for 60min each time;
(2) evaporating and concentrating 5 parts of sample solution to 50mL, taking 10mL of sample solution, diluting with methanol to a constant volume in a 50mL volumetric flask, and shaking up;
(3) the peak area thereof was detected under the chromatographic conditions of step S1, and the concentration thereof was calculated.
8. The method for extracting forsythin from forsythia suspense leaves as claimed in claim 1, wherein the extraction test steps at different times in the step S3S4 are as follows:
(1) precisely weighing 5 parts of 10g of forsythia suspense leaf powder, respectively adding 150mL of water, and extracting for 2 times at 80 ℃ for 20 min, 30 min, 40min, 50 min and 60 min;
(2) evaporating and concentrating 5 parts of sample solution to 50mL, taking 10mL of sample solution, diluting with methanol to a constant volume in a 50mL volumetric flask, and shaking up;
(3) the peak area thereof was detected under the chromatographic conditions in step S1, and the concentration thereof was calculated.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101085043A (en) * | 2006-06-06 | 2007-12-12 | 上海凯宝药业有限公司 | Method for preparing forsythia suspense extraction |
| CN102219813A (en) * | 2011-07-26 | 2011-10-19 | 河南省科高植物天然产物开发工程技术有限公司 | Method for extracting forsythin and forsythoside from forsythia leaves |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101085043A (en) * | 2006-06-06 | 2007-12-12 | 上海凯宝药业有限公司 | Method for preparing forsythia suspense extraction |
| CN102219813A (en) * | 2011-07-26 | 2011-10-19 | 河南省科高植物天然产物开发工程技术有限公司 | Method for extracting forsythin and forsythoside from forsythia leaves |
Non-Patent Citations (3)
| Title |
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| 李晓等: "连翘叶中连翘苷的提取工艺", 《时珍国医国药》 * |
| 闫久江: "连翘中连翘苷的提取方法研究", 《科学与财富》 * |
| 齐建红: "HPLC测定连翘叶不同提取物中连翘苷的含量比较", 《陕西农业科学》 * |
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