CN107607669B - Quality detection method for safflower and safflower formula granules - Google Patents
Quality detection method for safflower and safflower formula granules Download PDFInfo
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Abstract
The invention relates to a quality detection method of types of safflower and safflower formula particles, which belongs to the technical field of traditional Chinese medicine quality detection, and types of safflower quality detection comprises the following steps of (1) preparing a test solution (2) preparing a reference solution (3) preparing a reference medicinal material solution (4) performing thin-layer chromatography detection, and also discloses a quality detection method of types of safflower formula particles.
Description
Technical Field
The invention belongs to the field of quality detection of traditional Chinese medicines, and particularly relates to a quality detection method for safflower and safflower formula granules.
Background
Safflower is the dry flower of Carthamus tinctorius L of Carthamus of Compositae, also called the safflower, also called as grass safflower, red thorn safflower, safflower vegetable, etc. safflower is a traditional Chinese medicinal material commonly used in China, has good medicinal value, has the efficacies of activating blood circulation to dissipate blood stasis, dissipating blood stasis to relieve pain, reducing blood pressure and reducing blood fat, etc., has definite curative effect in treating coronary heart disease, hypertension and cerebral hemorrhage diseases, and is collected in 2015 edition Chinese pharmacopoeia.
However, the safflower is identified according to a safflower thin layer identification method recorded in the current pharmacopoeia, acetone is used as a solvent, a mixed solution of ethyl acetate-formic acid-water-methanol is used as a developing agent, and a silica gel plate H thin layer plate is used, so that the displayed color spots are fuzzy, the definition is not high, the separation effect is not good, the reproducibility is not good, and the identification effect is not good.
However, the traditional Chinese medicine formula particle loses the appearance characteristics of the original medicinal materials after being processed by series procedures, and the character identification is not suitable for the traditional Chinese medicine formula particle, so new quality detection methods are selected.
In view of the above, it is necessary to provide new methods for detecting the quality of safflower and safflower-containing granules.
Disclosure of Invention
The invention aims to provide a quality detection method for carthamus tinctorius, which has the advantages of high definition, good separation effect, obvious spots and good reproducibility, can better control the quality of the carthamus tinctorius, and ensures the curative effect of clinical medication.
In order to realize the purpose, the adopted technical scheme is as follows:
the quality detection method of safflower comprises the following steps:
(1) preparing a test solution: adding methanol into the safflower medicinal material powder, carrying out ultrasonic extraction for 35-45 minutes, and taking supernatant as a test solution; wherein the mass ratio of the safflower medicinal material powder to the methanol is 1 g: 45-55 ml;
(2) preparation of control solutions: adding methanol into hydroxysafflor yellow A to obtain reference solution; wherein the volume ratio of the mass of the hydroxysafflor yellow A to the methanol is 0.120-0.124 mg: 1 ml;
(3) preparing a reference medicinal material solution: adding methanol into control powder of Carthami flos, ultrasonic extracting for 35-45 min, and collecting supernatant as control solution; wherein the mass ratio of the safflower reference medicinal material powder to the methanol is 1 g: 120-;
(4) sucking 4 μ L of the sample solution, 2 μ L of the reference solution and 5 μ L of the reference material, respectively dropping on polyamide thin layer plates, developing, taking out, air drying, and inspecting under ultraviolet light and white light.
And , the developing solvent is a mixed solution of 3.6% hydrochloric acid solution, methanol and ethyl acetate by mass fraction.
And , wherein the volume ratio of the components in the developing solvent is hydrochloric acid solution, methanol and ethyl acetate is 7:3: 1.
, in the step (1), the mass-to-methanol volume ratio of the safflower medicinal powder is 1g to 50ml, the ultrasonic extraction time is 40 minutes, and the safflower medicinal powder is sieved by a third sieve;
in the step (2), the ratio of the mass of the hydroxysafflor yellow A to the volume of the methanol is 0.122 mg: 1 ml;
in the step (3), the mass ratio of the safflower reference medicinal material powder to the methanol is 1 g: 125 ml;
in the step (4), the wavelength observed under the ultraviolet lamp is 366 nm.
, wherein in the step (1), the ultrasonic treatment frequency is 50k Hz, and the temperature is 25 ℃;
in the step (3), the ultrasonic treatment frequency is 50k Hz, and the temperature is 25 ℃.
Another aims at providing a quality detection method for safflower formula granules, which has the advantages of high definition, good separation effect, obvious spots and good reproducibility, can better control the quality of the safflower formula granules and ensure the curative effect of clinical medication.
In order to realize the purpose, the adopted technical scheme is as follows:
the quality detection method of safflower formula granules comprises the following steps:
(1) preparing a test solution: adding methanol into the safflower formula particle powder, carrying out ultrasonic extraction for 35-45 minutes, and taking supernatant as a test solution; wherein the mass of the safflower formula particle powder and the volume ratio of the methanol are respectively 0.6 g: 45-55 ml;
(2) preparation of control solutions: adding methanol into hydroxysafflor yellow A to obtain reference solution; wherein the volume ratio of the mass of the hydroxysafflor yellow A to the methanol is 0.120-0.124 mg: 1 ml;
(3) preparing a reference medicinal material solution: adding methanol into control powder of Carthami flos, ultrasonic extracting for 35-45 min, and collecting supernatant as control solution; wherein the mass ratio of the safflower reference medicinal material powder to the methanol is 1 g: 120-;
(4) sucking 4 μ L of the sample solution, 2 μ L of the reference solution and 5 μ L of the reference material, respectively dropping on polyamide thin layer plates, developing, taking out, air drying, and inspecting under ultraviolet light and white light.
And , the developing solvent is a mixed solution of 3.6% hydrochloric acid solution, methanol and ethyl acetate by mass fraction.
And , wherein the volume ratio of the components in the developing solvent is hydrochloric acid solution, methanol and ethyl acetate is 7:3: 1.
, in the step (1), the mass-to-methanol volume ratio of the safflower formula particle powder is 0.6 g: 50ml, the ultrasonic extraction time is 40 minutes, and the safflower formula particle powder is sieved by a third sieve;
in the step (2), the ratio of the mass of the hydroxysafflor yellow A to the volume of the methanol is 0.122 mg: 1 ml;
in the step (3), the mass ratio of the safflower reference medicinal material powder to the methanol is 1 g: 125 ml;
in the step (4), the wavelength observed under the ultraviolet lamp is 366 nm.
, wherein in the step (1), the ultrasonic treatment frequency is 50k Hz, and the temperature is 25 ℃;
in the step (3), the ultrasonic treatment frequency is 50k Hz, and the temperature is 25 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention relates to a quality detection method of safflower and safflower formula particles, which is characterized in that based on physicochemical properties of safflower, research and improvement are carried out on the basis of a safflower thin-layer chromatography identification method of the existing Chinese pharmacopoeia, thin-layer chromatography methods of safflower and safflower formula particles with high definition, good separation effect, obvious spots and good reproducibility are provided, the quality control of the safflower and safflower formula particles is improved, an active ingredient HSYA in the safflower is a compound with a single chalcone glycoside structure, is a water-soluble flavonoid compound, is extracted by methanol, is more favorable for dissolving and can be better developed on a polyamide plate, compared with the existing silica gel H plate, the polyamide plate has better separation effect on the HSYA, other unknown ingredients can be correspondingly separated under the condition, the separation effect of the silica gel H plate is not good, other unknown ingredients are not separated into a tailing strip shape, and a developing agent with stronger development ability, namely 3.6% hydrochloric acid solution-methanol-ethyl acetate is adopted, so that the quality of the safflower and safflower formula particles and the clinical medication effect can be better controlled.
2. The quality detection method of safflower formula granules makes up the blank of thin-layer identification of the safflower formula granules, has great significance for improving the quality control of the safflower formula granules and ensuring the product quality, and simultaneously has important guiding significance for the effectiveness and the safety of clinical medication.
Drawings
FIG. 1 is a thin layer chromatogram of safflower under ultraviolet in example 1; wherein S is a reference substance, S0 is a safflower reference medicinal material, and S1-S7 are safflower test samples of different batches;
FIG. 2 is a thin layer chromatogram under a white light lamp of safflower in example 1; wherein S is a reference substance, S0 is a safflower reference medicinal material, and S1-S7 are safflower test samples of different batches;
FIG. 3 is a thin layer chromatogram of the safflower granules of example 4 under UV light; wherein S is a reference substance, A1-A7 is safflower formula granules from different manufacturers, and 8 is a negative reference substance;
FIG. 4 is a thin layer chromatogram under a white light lamp of the thin layer chromatogram of the safflower formula granules in example 4; wherein S is HSYA reference substance, A1-A7 safflower formula granule of different manufacturers, and 8 is negative reference;
FIG. 5 is a thin layer chromatogram measured by No. 1 developer in experimental test 1 for investigating the influence of different developers and different proportions on thin layer chromatography; wherein, the left picture is under ultraviolet light, the right picture is under white light, 1 is a reference substance, 2 is a safflower reference medicinal material, and 3 and 4 are safflower test samples;
FIG. 6 is a thin layer chromatogram measured by No. 2 developer in experimental test 1 for investigating the influence of different developers and different proportions on thin layer chromatography; wherein, the left picture is under ultraviolet light, the right picture is under white light, 1 is a reference substance, 2 is a safflower reference medicinal material, and 3 and 4 are safflower test samples;
FIG. 7 is a thin layer chromatogram measured by the No. 3 developing agent in the experimental test 1 for investigating the influence of different developing agents and different proportions on thin layer chromatography; wherein, the left picture is under ultraviolet light, the right picture is under white light, 1 is a reference substance, 2 is a safflower reference medicinal material, and 3 and 4 are safflower test samples;
FIG. 8 is a thin layer chromatogram measured by developer No. 4 in an experimental test 1 for investigating the influence of different developers and different proportions on thin layer chromatography; wherein, the left picture is under ultraviolet light, the right picture is under white light, 1 is a reference substance, 2 is a safflower reference medicinal material, and 3 and 4 are safflower test samples;
FIG. 9 is a thin layer chromatogram measured by developer No. 5 in experimental test 1 for investigating the influence of different developers and different proportions on thin layer chromatography; wherein, the left picture is under ultraviolet light, the right picture is under white light, 1 is a reference substance, 2 is a safflower reference medicinal material, and 3 and 4 are safflower test samples;
FIG. 10 is a thin layer chromatogram measured by No. 6 developer in experimental test 1 to investigate the effects of different developers and different ratios on thin layer chromatography; wherein, the left picture is under ultraviolet light, the right picture is under white light, 1 is a reference substance, 2 is a safflower reference medicinal material, and 3 and 4 are safflower test samples;
FIG. 11 is a thin layer chromatogram obtained from No. 7 developer in experimental test 1 for examining the effects of different developers and different ratios on thin layer chromatography; wherein, the left picture is under ultraviolet light, the right picture is under white light, 1 is a reference substance, 2 is a safflower reference medicinal material, and 3 and 4 are safflower test samples;
FIG. 12 is a thin layer chromatogram measured by No. 8 developer in experimental test 1 for examining the effects of different developers and different ratios on thin layer chromatography; wherein, the left picture is under ultraviolet light, the right picture is under white light, 1 is a reference substance, 2 is a safflower reference medicinal material, and 3 and 4 are safflower test samples;
FIG. 13 is a thin layer chromatogram measured with developer No. 9 in an experimental test 1 for investigating the effect of different developers and different proportions on thin layer chromatography; wherein, the left picture is under ultraviolet light, the right picture is under white light, 1 is a reference substance, 2 is a safflower reference medicinal material, and 3 and 4 are safflower test samples;
FIG. 14 is a thin layer chromatogram of method 1 safflower under white light in Experimental test 2.
Detailed Description
In order to further illustrate the method for testing the quality of kinds of safflower and safflower formula granules of the present invention and achieve the intended purpose of the invention, the following detailed description will be made on the method for testing the quality of kinds of safflower and safflower formula granules according to the present invention with reference to the preferred embodiments, and the detailed description will be given later on, in the following description, different " embodiment" or "embodiment" refers to different embodiments which are the same as embodiment, and in addition, specific features, structures or characteristics in or more embodiments can be combined in any suitable form.
Before describing the quality detection method of safflower and safflower formula granules in detail, it is necessary to explain the raw materials and methods mentioned in the invention by steps to achieve better effect.
The principle of the invention is as follows: factors such as different thin-layer plates with different extracting conditions and different spreading agents can influence the result. The silica gel thin-layer chromatography is mainly used for separating and detecting flavonoid compounds with lower polarity, and the silica gel plate only has adsorption capacity; the polyamide thin-layer chromatography is suitable for separating and identifying various types of flavones containing free phenolic hydroxyl, and the polyamide has strong adsorption capacity on flavonoid compounds, because the polyamide not only has adsorption capacity on the flavonoid compounds, but also can be combined with the flavonoid compounds containing free phenolic hydroxyl to form hydrogen bonds, so that the polyamide plate has better unfolding separation effect. HSYA is a compound with a single chalcone glycoside structure, belongs to flavonoid, is extracted by acetone, and cannot be separated under a polyamide plate; and the methanol extraction is adopted, because the HSYA is a water-soluble flavonoid compound, the dissolution is more favorable under the methanol extraction, the HSYA can be well developed, and the separation effect is good. The developing agent with stronger developing capability mostly contains alcohol, acid or water, so 3.6% hydrochloric acid solution-methanol-ethyl acetate is adopted.
The examples, which do not indicate specific techniques or conditions, are carried out according to techniques or conditions described in literature in the art. The raw materials and equipment used in the examples are not indicated by manufacturers, and are all conventional products commercially available.
Hydroxysafflor yellow A (HSYA), the most effective water-soluble part of the pharmacological effect of safflower, is a compound with a single chalcone glycoside structure, can inhibit platelet aggregation and release induced by platelet activating factor, can competitively inhibit the combination of the platelet activating factor and platelet receptors, and is an effective component of safflower yellow for promoting blood circulation and removing blood stasis. The HSYA reference substance adopted in the embodiment of the invention is produced by the China pharmaceutical and biological product institute (111637-200905).
Other main materials adopted in the embodiment of the invention:
safflower control drug (S0, 120907-.
Safflower (S1, Sinkiang JimuSaer county, 20150803, Sinkiang Qikangabovit GmbH, S2, Sinkiang Tacheng county, 20150822, Sinkiang Qikangabovit GmbH, S3, Sinkiang Hocheng county, 20160507, Anhui Shunshun Chinese herbal pieces GmbH, S4, Sinkiang JimuSaer county, 20160805, Sinkiang Xinjiang Xinte Kazay GmbH, S5, Sinkiang Tacheng county, 20160805, Sinkiang Xintamayu Gnjin, S6, Sinkiang Hepianyu, 20160815, self-purchased from Xinjiang Hepianyu, S7, Sinkiang Yining county, 20160908, and Xinpianying county) is identified as genuine pharmacopoeia according to the national pharmacopoeia of the classification of safflower.
Safflower dispensing granule (A1, 1607143, Jiangyin Tianjiang medicine, Inc.; A2, 1612001w, Sanjiu medicine; A3, 1512004, Sichuan New Green medicine, science and technology development, Inc.; A4, 6082331, east prescription pharmaceutical, Inc.; A5, 1512036, Sichuan New Green medicine, science and technology development, Inc.; A6, 1610001w, Sanjiu medicine; A7, 1701001, Jiangyin Tianjiang medicine, Inc.).
Polyamide thin-layer plates (four-methyl biochemical plastics factory, road and bridge, Taizhou, Zhejiang) and silica gel H thin-layer plates (silicon source materials, Inc., of Anhui Liang).
The screen size is numbers, the number of parallel wires (screen hole number) in each inch of linear length on the screen is screen size, the inner diameter of screen hole is 355 + -13 microns, the number is 50 meshes.
After understanding the above raw materials and methods, the following will describe the quality testing method for kinds of safflower and safflower formula granules in the invention in more detail in step :
example
Example 1.
The quality detection method of safflower plants comprises the following steps:
(1) preparing a test solution: adding 25ml methanol into 0.5g Carthami flos powder (sieved with a third sieve), ultrasonic extracting for 40 min at ultrasonic treatment power of 100w and frequency of 50kHz and temperature of 25 deg.C, and collecting supernatant as sample solution. According to the steps, 7 different batches of safflower test solution are respectively prepared.
(2) Preparation of control solutions: adding 1ml methanol into 0.122mg hydroxysafflor yellow A, and mixing well to obtain control solution.
(3) Preparing a reference medicinal material solution: adding 25ml methanol into 0.2g Carthami flos reference medicinal material powder, ultrasonic extracting for 40 min at 50kHz and 25 deg.C with ultrasonic treatment power of 100w, and collecting supernatant as reference medicinal material solution.
(4) According to the thin layer chromatography test, sucking 4 μ L of the sample solution, 2 μ L of the reference solution and 5 μ L of the reference material, respectively dropping on polyamide thin layer plates, developing with 3.6% hydrochloric acid solution-methanol-ethyl acetate (volume ratio of hydrochloric acid solution: methanol: ethyl acetate: 7:3:1) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp and white lamp with wavelength of 366 nm.
(5) As shown in FIG. 1 and FIG. 2, the chromatogram of the sample shows spots of the same color at the corresponding positions of the chromatograms of the reference substance and the reference drug, and the spots have clear bands and good separation effect.
The method for detecting the quality of carthamus tinctorius provided by the embodiment of the invention is characterized in that according to the physicochemical properties of the carthamus tinctorius, the research and improvement of a thin-layer chromatography method are carried out on the basis of a thin-layer identification method recorded in pharmacopoeia, active ingredients HSYA in the carthamus tinctorius are extracted by methanol, a 3.6% hydrochloric acid solution with strong developing capacity-methanol-ethyl acetate is adopted, and the active ingredients are developed on a polyamide plate.
Example 2.
The quality detection method of safflower plants comprises the following steps:
(1) preparing a test solution: adding 45ml of methanol into 1g of safflower medicinal material powder (sieved by a third sieve), and carrying out ultrasonic extraction for 35 minutes at the ultrasonic treatment power of 100w, the frequency of 50kHz and the temperature of 25 ℃, and taking supernatant as a test solution;
(2) preparation of control solutions: adding 1ml methanol into 0.120mg hydroxysafflor yellow A, and mixing well to obtain reference solution;
(3) preparing a reference medicinal material solution: adding 24ml of methanol into 0.2g of safflower control medicinal material powder, carrying out ultrasonic extraction for 35 minutes, wherein the ultrasonic treatment power is 100w, the frequency is 50kHz, the temperature is 25 ℃, and taking supernate as a control medicinal material solution;
(4) according to the thin layer chromatography test, sucking 4 μ L of the sample solution, 2 μ L of the reference solution and 5 μ L of the reference material, respectively dropping on polyamide thin layer plates, developing with 3.6% hydrochloric acid solution-methanol-ethyl acetate (volume ratio of hydrochloric acid solution: methanol: ethyl acetate: 7:3:1) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp and white lamp with wavelength of 366 nm.
(5) Spots of the same color are displayed on the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution and the reference medicinal material.
The method for detecting the quality of carthamus tinctorius provided by the embodiment of the invention is characterized in that according to the physicochemical properties of the carthamus tinctorius, the research and improvement of a thin-layer chromatography method are carried out on the basis of a thin-layer identification method recorded in pharmacopoeia, active ingredients HSYA in the carthamus tinctorius are extracted by methanol, a 3.6% hydrochloric acid solution with strong developing capacity-methanol-ethyl acetate is adopted, and the active ingredients are developed on a polyamide plate.
Example 3.
The quality detection method of safflower plants comprises the following steps:
(1) preparing a test solution: adding 55ml of methanol into 1g of safflower medicinal material powder (sieved by a third sieve), and performing ultrasonic extraction for 45 minutes at the ultrasonic treatment power of 100w, the frequency of 50kHz and the temperature of 25 ℃, and taking supernatant as a test solution;
(2) preparation of control solutions: adding 1ml methanol into 0.124mg hydroxysafflor yellow A, and mixing well to obtain reference solution;
(3) preparing a reference medicinal material solution: adding 26ml of methanol into 0.2g of safflower control medicinal material powder, carrying out ultrasonic extraction for 45 minutes, wherein the ultrasonic treatment power is 100w, the frequency is 50kHz, and the temperature is 25 ℃, and taking supernate as a control medicinal material solution;
(4) according to the thin layer chromatography test, sucking 4 μ L of the sample solution, 2 μ L of the reference solution and 5 μ L of the reference material, respectively dropping on polyamide thin layer plates, developing with 3.6% hydrochloric acid solution-methanol-ethyl acetate (volume ratio of hydrochloric acid solution: methanol: ethyl acetate: 7:3:1) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp and white lamp with wavelength of 366 nm.
(5) Spots of the same color are displayed on the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution and the reference medicinal material.
The method for detecting the quality of carthamus tinctorius provided by the embodiment of the invention is characterized in that according to the physicochemical properties of the carthamus tinctorius, the research and improvement of a thin-layer chromatography method are carried out on the basis of a thin-layer identification method recorded in pharmacopoeia, active ingredients HSYA in the carthamus tinctorius are extracted by methanol, a 3.6% hydrochloric acid solution with strong developing capacity-methanol-ethyl acetate is adopted, and the active ingredients are developed on a polyamide plate.
Example 4.
The quality detection method of safflower formula granules comprises the following specific operation steps:
(1) preparing a test solution: adding 25ml methanol into 0.3g Carthami flos formula granule powder (sieved with a third sieve), ultrasonic extracting for 40 min at ultrasonic treatment power of 100w and frequency of 50kHz and temperature of 25 deg.C, and collecting supernatant as sample solution. According to the steps, test solutions of safflower formula granules of 7 different manufacturers are respectively prepared.
(2) Preparation of control solutions: adding 1ml methanol into 0.122mg hydroxysafflor yellow A, and mixing well to obtain control solution.
(3) Preparing a reference medicinal material solution: adding 25ml methanol into 0.2g Carthami flos reference medicinal material powder, ultrasonic extracting for 40 min at 50kHz and 25 deg.C with ultrasonic treatment power of 100w, and collecting supernatant as reference medicinal material solution.
(4) According to the thin layer chromatography test, sucking 4 μ L of the sample solution, 2 μ L of the reference solution and 5 μ L of the reference material, respectively dropping on polyamide thin layer plates, developing with 3.6% hydrochloric acid solution-methanol-ethyl acetate (volume ratio of hydrochloric acid solution: methanol: ethyl acetate: 7:3:1) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp and white lamp with wavelength of 366 nm.
(5) As shown in FIGS. 3 and 4, the test chromatogram showed spots of the same color at positions corresponding to those of the control chromatogram, while the negative control showed no spots.
The quality detection method of safflower formula particles, disclosed by the embodiment of the invention, makes up the blank of thin-layer identification of the safflower formula particles, extracts the active ingredient HSYA in flowers by using methanol according to the physicochemical properties of safflower, adopts a 3.6% hydrochloric acid solution-methanol-ethyl acetate which has stronger unfolding capacity, and then unfolds on a polyamide plate.
Example 5.
The quality detection method of safflower formula granules comprises the following specific operation steps:
(1) preparing a test solution: adding 45ml methanol into 0.6g Carthami flos formula granule powder (sieved with a third sieve), ultrasonic extracting for 35 min at ultrasonic treatment power of 100w and frequency of 50kHz and temperature of 25 deg.C, and collecting supernatant as sample solution.
(2) Preparation of control solutions: adding 1ml methanol into 0.120mg hydroxysafflor yellow A, and mixing well to obtain control solution.
(3) Preparing a reference medicinal material solution: adding 24ml methanol into 0.2g Carthami flos reference medicinal material powder, ultrasonic extracting for 35 min at 50kHz and 25 deg.C with ultrasonic treatment power of 100w, and collecting supernatant as reference medicinal material solution.
(4) According to the thin layer chromatography test, sucking 4 μ L of the sample solution, 2 μ L of the reference solution and 5 μ L of the reference material, respectively dropping on polyamide thin layer plates, developing with 3.6% hydrochloric acid solution-methanol-ethyl acetate (volume ratio of hydrochloric acid solution: methanol: ethyl acetate: 7:3:1) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp and white lamp with wavelength of 366 nm.
(5) In the chromatogram of the test solution, spots of the same color were shown at the positions corresponding to those of the control solution, while the negative control solution was absent.
The quality detection method of safflower formula particles, disclosed by the embodiment of the invention, makes up the blank of thin-layer identification of the safflower formula particles, extracts the active ingredient HSYA in flowers by using methanol according to the physicochemical properties of safflower, adopts a 3.6% hydrochloric acid solution-methanol-ethyl acetate which has stronger unfolding capacity, and then unfolds on a polyamide plate.
Example 6.
The quality detection method of safflower formula granules comprises the following specific operation steps:
(1) preparing a test solution: adding 55ml methanol into 0.6g Carthami flos formula granule powder (sieved with a third sieve), ultrasonic extracting for 45 min at ultrasonic treatment power of 100w and frequency of 50kHz and temperature of 25 deg.C, and collecting supernatant as sample solution.
(2) Preparation of control solutions: adding 1ml methanol into 0.124mg hydroxysafflor yellow A, and mixing well to obtain control solution.
(3) Preparing a reference medicinal material solution: adding 26ml methanol into 0.2g Carthami flos reference medicinal material powder, ultrasonic extracting for 45 min at 50kHz and 25 deg.C under 100w ultrasonic treatment power, and collecting supernatant as reference medicinal material solution.
(4) According to the thin layer chromatography test, sucking 4 μ L of the sample solution, 2 μ L of the reference solution and 5 μ L of the reference material, respectively dropping on polyamide thin layer plates, developing with 3.6% hydrochloric acid solution-methanol-ethyl acetate (volume ratio of hydrochloric acid solution: methanol: ethyl acetate: 7:3:1) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp and white lamp with wavelength of 366 nm.
(5) In the chromatogram of the test solution, spots of the same color were shown at the positions corresponding to those of the control solution, while the negative control solution was absent.
The quality detection method of safflower formula particles, disclosed by the embodiment of the invention, makes up the blank of thin-layer identification of the safflower formula particles, extracts the active ingredient HSYA in flowers by using methanol according to the physicochemical properties of safflower, adopts a 3.6% hydrochloric acid solution-methanol-ethyl acetate which has stronger unfolding capacity, and then unfolds on a polyamide plate.
Two experimental tests
1. Effect of different developing Agents and different ratios on thin layer chromatography
(1) Developing agent: different volume ratios (v/v) of developing agent were selected:
note: the 3.6% hydrochloric acid solution refers to 3.6% hydrochloric acid solution
(2) The experimental steps are as follows: selecting No. 1-9 developing agent, preparing 2 different batches of safflower test solution, and other steps are the same as example 1.
(3) As a result: the test results are shown in fig. 5 to 13. As shown in the figure, compared with other developing agents, the developing agent of 3.6% hydrochloric acid solution-methanol-ethyl acetate (7:3:1) can be used for developing to well separate the components in the sample, so that the developing agent of 3.6% hydrochloric acid solution-methanol-ethyl acetate (7:3:1) is selected.
2. Compared with the prior art
(1) Identifying Carthami flos by thin layer chromatography method specified in 2015 edition Chinese pharmacopoeia part
(2) The experimental steps are as follows:
the method comprises the following steps:
according to the identification item of the safflower thin layer of the th part of the 2015 version Chinese pharmacopoeia, 0.5g of the powder (screened by a third sieve) is taken, 5mL of an acetone solution with the mass fraction of 80% is added, the mixture is tightly packed, shaken for 15 minutes and kept stand, the supernatant is taken as a test solution, 0.5g of the safflower control drug is taken, a control drug solution is prepared by the same method, an appropriate amount of an HSYA control is taken, a control drug solution is prepared by the same method, a thin layer chromatography (general rule 0502) test is carried out, 5 mu L of the control drug solution, 5 mu L of the safflower control drug solution and 5 mu L of the safflower test solution are respectively spotted on the same silica gel H thin layer plate, ethyl acetate-formic acid-water-methanol (the volume ratio of the ethyl acetate-formic acid-water-methanol is 7:2:3:0.4) is taken as a developing agent, the developing agent is taken out, and.
The method 2 comprises the following steps: example 2.
(3) As a result, in comparison with FIG. 2, in the chromatogram of the test sample, spots of the same color were observed at the positions corresponding to those of the control material and the control chromatogram, but the spots were blurred, so that the quality detection method for carthamus tinctorius provided by the invention was better.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (6)
1, quality detection method of safflower, characterized by, including the following steps:
(1) preparing a test solution: adding methanol into the safflower medicinal material powder, carrying out ultrasonic extraction for 35-45 minutes, and taking supernatant as a test solution; wherein the mass ratio of the safflower medicinal material powder to the methanol is 1 g: 45-55 ml;
(2) preparation of control solutions: adding methanol into hydroxysafflor yellow A to obtain reference solution; wherein the volume ratio of the mass of the hydroxysafflor yellow A to the methanol is 0.120-0.124 mg: 1 ml;
(3) preparing a reference medicinal material solution: adding methanol into control powder of Carthami flos, ultrasonic extracting for 35-45 min, and collecting supernatant as control solution; wherein the mass ratio of the safflower reference medicinal material powder to the methanol is 1 g: 120-;
(4) sucking 4 μ L of the test solution, 2 μ L of the reference solution and 5 μ L of the reference material, respectively dropping on polyamide thin layer plates, developing with 3.6% hydrochloric acid solution, methanol and ethyl acetate at a volume ratio of 7:3:1, taking out, air drying, and inspecting under ultraviolet light and white light.
2. The quality inspection method according to claim 1, wherein,
in the step (1), the mass-to-methanol volume ratio of the safflower medicinal powder is 1 g: 50 ml; the ultrasonic extraction time is 40 minutes; the safflower medicinal powder is sieved by a third sieve;
in the step (2), the ratio of the mass of the hydroxysafflor yellow A to the volume of the methanol is 0.122 mg: 1 ml;
in the step (3), the mass ratio of the safflower reference medicinal material powder to the methanol is 1 g: 125 ml;
in the step (4), the wavelength observed under the ultraviolet lamp is 366 nm.
3. The quality inspection method according to claim 2, wherein,
in the step (1), the ultrasonic treatment frequency is 50k Hz, and the temperature is 25 ℃;
in the step (3), the ultrasonic treatment frequency is 50k Hz, and the temperature is 25 ℃.
The quality detection method of the safflower formula granules of 4 and is characterized by comprising the following steps:
(1) preparing a test solution: adding methanol into the safflower formula particle powder, carrying out ultrasonic extraction for 35-45 minutes, and taking supernatant as a test solution; wherein the mass of the safflower formula particle powder and the volume ratio of the methanol are respectively 0.6 g: 45-55 ml;
(2) preparation of control solutions: adding methanol into hydroxysafflor yellow A to obtain reference solution; wherein the volume ratio of the mass of the hydroxysafflor yellow A to the methanol is 0.120-0.124 mg: 1 ml;
(3) preparing a reference medicinal material solution: adding methanol into control powder of Carthami flos, ultrasonic extracting for 35-45 min, and collecting supernatant as control solution; wherein the mass ratio of the safflower reference medicinal material powder to the methanol is 1 g: 120-;
(4) sucking 4 μ L of the test solution, 2 μ L of the reference solution and 5 μ L of the reference material, respectively dropping on a polyamide thin layer plate of , developing with a developing agent containing 3.6% hydrochloric acid solution, methanol and ethyl acetate at a volume ratio of 7:3:1, taking out, air drying, and inspecting under ultraviolet light and white light.
5. The quality inspection method according to claim 4, wherein,
in the step (1), the mass-to-methanol volume ratio of the safflower formula particle powder is 0.6 g: 50 ml; the ultrasonic extraction time is 40 minutes; the safflower formula particle powder is sieved by a third sieve;
in the step (2), the ratio of the mass of the hydroxysafflor yellow A to the volume of the methanol is 0.122 mg: 1 ml;
in the step (3), the mass ratio of the safflower reference medicinal material powder to the methanol is 1 g: 125 ml;
in the step (4), the wavelength observed under the ultraviolet lamp is 366 nm.
6. The quality inspection method according to claim 5, wherein,
in the step (1), the ultrasonic treatment frequency is 50kHz, and the temperature is 25 ℃;
in the step (3), the ultrasonic treatment frequency is 50kHz, and the temperature is 25 ℃.
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