CN114264763A - Method for sampling lysimachia capillipes - Google Patents
Method for sampling lysimachia capillipes Download PDFInfo
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- CN114264763A CN114264763A CN202111576697.3A CN202111576697A CN114264763A CN 114264763 A CN114264763 A CN 114264763A CN 202111576697 A CN202111576697 A CN 202111576697A CN 114264763 A CN114264763 A CN 114264763A
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Abstract
The invention discloses a method for sampling lysimachia capillipes in the technical field of natural medicine preparation, which comprises the following steps: step one, taking fresh lysimachia capillipes from a purchase point; step two, obtaining an extract of the lysimachia capillipes medicinal material; step three, dividing the extract in the step two into a plurality of precisely-weighed equal mass parts; step four, adding 20 times of water and 30-95% ethanol into each part of the divided extract respectively, and extracting for at least 2 hours; and step five, filtering the extract obtained in the step four, scanning and determining the content of the lysimachia capillipes saponin, and dividing the quality difference of the raw materials.
Description
Technical Field
The invention relates to the technical field of natural medicine preparation, in particular to a method for sampling lysimachia capillipes.
Background
Lysimachia capillipes is a plant of the genus Pelargonium of the family Primulaceae. The plant height is 40-60 cm, and the dried plant has strong fragrance. The stem is usually 2 or more bunched, upright, branched above the middle, herbaceous, ridged, and sometimes narrow-winged. Leaf intergrowth, egg-like to egg-like, needle-like, 1.5-7 cm long and 1-3 cm wide. The single flower emerges from the axilla; the flower stalks are fine and filamentous, and the length of the flower stalks is 1.5 to 3.5 centimeters; the length of the calyx is 2-4 mm. The capsule is nearly spherical, white, 3-4 mm in diameter and longer than the reserved calyx. The flowering period is 6-7 months, and the fruit period is 8-10 months.
The Chinese invention CN101507740B discloses a method for preparing a lysimachia capillipes total saponin extract by utilizing macroporous resin and application thereof, which comprises the steps of crushing lysimachia capillipes medicinal materials or directly using lysimachia capillipes decoction pieces, adding water with the mass volume ratio of 6-15 times or ethanol with the volume ratio of 10% -95%, heating, refluxing, extracting, filtering, combining extracting solutions and concentrating; filtering or centrifuging, passing through chromatographic column filled with macroporous resin, washing resin with water, and discarding water eluate; eluting with aqueous ethanol, and collecting ethanol eluate; concentrating the ethanol eluate under reduced pressure, and drying under reduced pressure or by spray drying to obtain total saponins of herba Lysimachiae Foenumgraeci. The macroporous resin adopted by the invention has large adsorption capacity on the total saponin of the lysimachia capillipes and is completely desorbed, and the content of the obtained total saponin is high, so that the extraction rate of the total saponin of the lysimachia capillipes can be obviously improved, and the production cost is reduced. The total saponin extract of the lysimachia capillipes has obvious anti-tumor effect and can be used for preparing medicaments for treating tumors.
However, in the process of implementing the technical solution of the invention in the embodiments of the present application, the inventors of the present application find that the above-mentioned technology has at least the following technical problems:
1. the lysimachia capillipes is extracted blindly when the lysimachia capillipes is selected, so that a large amount of lysimachia capillipes with low saponin content also participates in extraction, and the extraction cost of saponin is improved;
2. when the lysimachia capillipes is selected, due to the influence of factors such as production environment, altitude and the like, the selection result is easily influenced by various saponin content mixing factors;
3. when the saponin extraction is carried out under the condition that the chemical property change before the lysimachia capillipes is not clear, the extraction failure rate is easily improved.
Based on the above, the invention designs a method for sampling lysimachia capillipes to solve the above problems.
Disclosure of Invention
The present invention is directed to a method for sampling lysimachia capillipes, which solves the above mentioned problems of the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for sampling Lysimachia capillipes Hemsl comprises the following steps:
step one, taking fresh lysimachia capillipes from a purchase point;
step two, obtaining an extract of the lysimachia capillipes medicinal material;
step three, dividing the extract in the step two into a plurality of precisely-weighed equal mass parts;
step four, adding 20 times of water and 30-95% ethanol into each part of the divided extract respectively, and extracting for at least 2 hours;
and step five, filtering the extract obtained in the step four, scanning and measuring the content of the lysimachia capillipes hemsl saponin, and dividing the quality difference of the raw materials.
Further, the time range from the picking of the lysimachia capillipes to the using at the purchasing point is 0-8 hours.
Further, the picking of the lysimachia capillipes comprises:
establishing sampling environment classification, grouping different types of altitude units in the same sampling environment, taking boundary staggered points of four adjacent groups of grouping units as a group of sampling points, and collecting lysimachia capillipes of each sampling point.
Further, the sampling environment comprises one or more of a passion fruit shelf, a greenhouse or a shading net.
Furthermore, the ultrafiltration membrane is made of polytetrafluoroethylene.
Further, the scanning assay instrument comprises one of a liquid phase spectrometer or a thin layer scanner.
One or more technical solutions provided in the embodiments of the present invention have at least the following technical effects or advantages:
1. according to the invention, the sampling points are selected according to the gradient four groups of junctions of adjacent altitudes when the lysimachia capillipes is picked and sampled, so that the obtained lysimachia capillipes saponin content is more representative;
2. according to the method, the fresh lysimachia capillipes is screened, so that various stable performances of the lysimachia capillipes tested by assay can be improved, and the accuracy of the saponin content testing is improved;
3. according to the invention, the precision and the accuracy of the saponin content measurement are realized by a single-factor test mode, so that the raw materials are rapidly classified according to different qualities of the raw materials;
in conclusion, the method has the characteristics of accurate determination of the lysimachia capillipes hemsl saponin content, accurate determination of the saponin due to a sampling mode, convenience in raw material classification and the like.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a sampling process of the present invention;
FIG. 2 is a flow chart of the Lysimachia capillipes Hara picking process of the present invention;
FIG. 3 is a layout of picking points according to the present invention;
FIG. 4 is a flow chart of the process for obtaining the Lysimachia capillipes Heim extract of 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.
Example one
As shown in fig. 1, a method for sampling lysimachia capillipes includes the following steps:
step one, taking fresh lysimachia capillipes from a purchase point;
step two, obtaining an extract of the lysimachia capillipes medicinal material;
step three, dividing the extract in the step two into a plurality of precisely-weighed equal mass parts;
step four, adding 20 times of water and 30-95% ethanol into each part of the divided extract respectively, and extracting for at least 2 hours;
and step five, filtering the extract obtained in the step four, scanning and measuring the content of the lysimachia capillipes hemsl saponin, and dividing the quality difference of the raw materials.
Through the steps, before the lysimachia capillipes hemsl extract is extracted, it needs to be noted that the lysimachia capillipes hemsl is fresh, namely, the lysimachia capillipes hemsl can be kept in a fresh state all the time from picking to a purchasing point and waiting for a laboratory to sample, so that during quality detection, component loss or denaturation is minimum, the accuracy of detection data is improved, the lysimachia capillipes hemsl extract is classified according to equal quality, the saponin content is measured through filtration after water and ethanol extraction, and the quality difference of raw materials can be detected quickly by utilizing the uniqueness (only containing saponin B and saponin C) of the lysimachia capillipes hemsl, so that the lysimachia capillipes hemsl extract is stacked according to different qualities.
It is noteworthy that, when the saponin content is measured, it is carried out by a one-way test:
taking 10g of a weighed extract of the lysimachia capillipes, adding 20 times (V/m) of water, extracting for more than 2 hours, filtering, and determining the content of the saponin by a liquid phase spectrometer; collecting 10g of a weighed extract of the lysimachia capillipes hance, adding 30% ethanol, extracting for more than 2 hours, filtering, and measuring the saponin content by a liquid phase spectrometer;
③ taking 10g of a weighed extract of the lysimachia capillipes hance, adding 50 percent ethanol, extracting for more than 2 hours, filtering, and measuring the content of the saponin by a liquid phase spectrometer;
taking 10g of a weighed extract of the lysimachia capillipes hemsl, adding 70% ethanol, extracting for more than 2 hours, filtering, and determining the content of the saponin by a liquid phase spectrometer;
fifthly, taking 10g of the extract of the closely-weighed lysimachia capillipes hemsl, adding 95% ethanol, extracting for more than 2 hours, filtering, and determining the content of the saponin by a liquid phase spectrometer.
More specifically, the time range from the picking of the lysimachia capillipes to the use at the purchase point is 0-8 hours.
In this embodiment, the property of the lysimachia capillipes before the measurement in the fresh state can be effectively ensured by controlling the use of the lysimachia capillipes in the laboratory to the purchase point within 8 hours after the lysimachia capillipes is picked.
As shown in fig. 2-3, the picking of the lysimachia capillipes comprises:
establishing sampling environment classification, grouping different types of altitude units in the same sampling environment, taking boundary staggered points of four adjacent groups of grouping units as a group of sampling points, and collecting lysimachia capillipes of each sampling point.
In the embodiment, when sampling is carried out in the same established environment, by dividing and grouping different altitudes taking mu as a unit and selecting sampling points at four adjacent groups of altitude junctions in each altitude, the periodic variable values of each altitude are confirmed, the data diversity of the saponin content of the picked slender sweetclover samples is improved, sampling is carried out in other environments, and the saponin content determination in other planting environments is realized.
Further, the sampling environment comprises one or more of a passion fruit shelf, a greenhouse or a shading net.
In this embodiment, since the saponin content of the lysimachia capillipes is different under the white vanilla fruit shelf, in the growing environment of a greenhouse or a shading net due to the variation of environmental factors, for example, when the lysimachia capillipes is interplanted under the passion fruit shelf, the lysimachia capillipes is a semi-yin semi-yang plant which can grow under the valley forest with the altitude of 500 plus 1000 meters, in the stream side and in the humid place rich in humus, the obtained saponin content of the lysimachia capillipes can be changed to a certain extent by interplanting under the passion fruit shelf, and the performance of the obtained saponin content of the lysimachia capillipes is different under the conditions of the shading place, the greenhouse and the like, so the saponin content under various growing environments can be compared.
In still further embodiments, the scanning assay instrument comprises one of a liquid phase spectrometer or a thin layer scanner;
in the embodiment, when the liquid phase spectrometer is used for detecting the content of the saponin, the distribution ratio difference of each component in the mixture after extraction and filtration is utilized to firstly separate the extracted mixture, and then the extracted mixture is analyzed and identified; when a thin-layer scanner is used for measuring the saponin content, the extraction mixture is placed on a measuring thin-layer class, and spots on a thin-layer plate can be scanned in situ to obtain an absorption spectrum curve, so that the saponin content can be quickly and accurately qualitatively and quantitatively analyzed.
Example two
As shown in fig. 4, in which the same or corresponding components as in the first embodiment are denoted by the same reference numerals as in the first embodiment, only the points of difference from the first embodiment will be described below for the sake of convenience. The second embodiment is different from the first embodiment in that: the obtaining of the lysimachia capillipes extract comprises the following steps:
crushing lysimachia capillipes hemsl, adding 60-70% of ethanol for cold leaching extraction, carrying out primary filtration, then carrying out fine filtration through a 3000-10000 ultrafiltration membrane, recovering ethanol from permeate, extracting obtained concentrated solution through water saturated n-butyl alcohol, carrying out organic phase medicinal activated carbon decoloration, carrying out reduced pressure concentration, and drying to obtain the extract.
In this example, the obtaining of the lysimachia capillipes extract includes the following embodiments:
a. pulverizing Lysimachia capillipes Hemsl, adding 60% ethanol for cold extraction, filtering with 3000 ultrafiltration membrane, recovering ethanol from the filtrate, extracting with water saturated n-butanol, decolorizing with medicinal active carbon, concentrating under reduced pressure, and drying to obtain extract.
b. Pulverizing Lysimachia capillipes Hemsl, adding 65% ethanol, cold soaking, extracting, filtering with 6500 ultrafiltration membrane, recovering ethanol from the filtrate, extracting with water saturated n-butanol, decolorizing with medicinal active carbon, concentrating under reduced pressure, and drying to obtain extract.
c. Pulverizing Lysimachia capillipes Hemsl, adding 70% ethanol, cold soaking, extracting, filtering with 10000 ultrafiltration membrane, recovering ethanol from the filtrate, extracting with water saturated n-butanol, decolorizing with organic phase and medicinal active carbon, concentrating under reduced pressure, and drying to obtain extract
Preferably, the material used for the ultrafiltration membrane is a polytetrafluoroethylene material.
In the embodiment, because the polytetrafluoroethylene material is a high molecular polymer obtained by polymerizing tetrafluoroethylene as a monomer, is white wax-like, semitransparent, heat-resistant and cold-resistant, and can be used at minus 180-260 ℃ for a long time, the polytetrafluoroethylene material has the characteristics of acid resistance, alkali resistance and various organic solvents resistance, and is almost insoluble in all solvents, so that the stability of the chemical property of the extract can be effectively ensured by using the ultrafiltration membrane made of the polytetrafluoroethylene material during filtration.
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 preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (7)
1. A method for sampling Lysimachia capillipes Hemsl, comprising the steps of:
step one, taking fresh lysimachia capillipes from a purchase point;
step two, obtaining an extract of the lysimachia capillipes medicinal material;
step three, dividing the extract in the step two into a plurality of precisely-weighed equal mass parts;
step four, adding 20 times of water and 30-95% ethanol into each part of the divided extract respectively, and extracting for at least 2 hours;
and step five, filtering the extract obtained in the step four, scanning and measuring the content of the lysimachia capillipes hemsl saponin, and dividing the quality difference of the raw materials.
2. A method for sampling Lysimachia capillipes according to claim 1, characterized in that the time from the picking of the Lysimachia capillipes to the point of purchase for use is in the range of 0 to 8 hours.
3. A method for sampling lysimachia capillipes according to claim 2, wherein the picking of lysimachia capillipes comprises:
establishing sampling environment classification, grouping different types of altitude units in the same sampling environment, taking boundary staggered points of four adjacent groups of grouping units as a group of sampling points, and collecting lysimachia capillipes of each sampling point.
4. The method for sampling Lysimachia capillipes Hemsl according to claim 3, characterized in that the sampling environment comprises one or more of under-shelf passion fruit, greenhouse or shade net.
5. A method for sampling lysimachia capillipes according to claim 1, wherein the obtaining of the lysimachia capillipes extract comprises:
crushing lysimachia capillipes hemsl, adding 60-70% of ethanol for cold leaching extraction, carrying out primary filtration, then carrying out fine filtration through a 3000-10000 ultrafiltration membrane, recovering ethanol from permeate, extracting obtained concentrated solution through water saturated n-butyl alcohol, carrying out organic phase medicinal activated carbon decoloration, carrying out reduced pressure concentration, and drying to obtain the extract.
6. A method for sampling Lysimachia capillipes according to claim 5, characterized in that the ultrafiltration membrane is made of PTFE.
7. A method according to claim 1, wherein the scanning measuring device comprises one of a liquid phase spectrometer or a thin layer scanner.
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