CN115166066B - Quality evaluation method of Qizhu oral liquid for improving white blood cells - Google Patents
Quality evaluation method of Qizhu oral liquid for improving white blood cells Download PDFInfo
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- CN115166066B CN115166066B CN202210586599.6A CN202210586599A CN115166066B CN 115166066 B CN115166066 B CN 115166066B CN 202210586599 A CN202210586599 A CN 202210586599A CN 115166066 B CN115166066 B CN 115166066B
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- solution
- oral liquid
- astragalus membranaceus
- methanol
- ethanol
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- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
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Abstract
The invention belongs to the field of medicine quality control, and relates to a quality evaluation method of astragalus membranaceus oral liquid for improving whiteness, which comprises the following steps: 1) Qualitative identification of the raw materials in QIZHUQISHENGBAI oral liquid by thin layer chromatography; 2) Quantitatively analyzing the active ingredients in the raw materials according to a high performance liquid chromatography; 3) And (3) evaluating the quality of the astragalus membranaceus oral liquid by combining the relative density, the pH value and the qualitative identification result obtained in the step (1) with the quantitative analysis result obtained in the step (2). The method is stable and feasible, and can be used for quality evaluation of Qizhu oral liquid. The quality evaluation method of the astragalus membranaceus oral liquid for increasing white blood cells, which is established by the invention, can be used for quality evaluation and control of the astragalus membranaceus oral liquid for increasing white blood cells, and can also provide reference for the content determination and extraction method of the compound preparation containing the medicinal materials.
Description
Technical Field
The invention belongs to the field of medicine quality control, relates to a medicine quality evaluation method, and in particular relates to a quality evaluation method of astragalus membranaceus oral liquid capable of improving whiteness.
Background
Leukopenia is a group of syndromes usually caused by infection, toxic and side effects of drugs and the like, and clinical diagnosis is based on the fact that the total number of white blood cells per liter in peripheral blood is continuously lower than 4.0X10 9 The traditional Chinese medicine composition is a common disease in clinical internal medicine so far, secondary and cause unknown are two common clinical pathogenesis causes, and the physical treatment by radiation irradiation and the toxic and side effects of anti-tumor medicines are most common in leucopenia after tumor chemotherapy and radiotherapy, and can cause the body resistance of a patient to be reduced, increase the risk of infection and further endanger life; and is a major obstacle to the end of the patient's course of disease at a later time due to medication that may affect the normal chemotherapy cycle. Thus increasing white blood cells, improving body functions,Improving the disease resistance of patients, and becoming an important treatment means and method for tumor radiotherapy and chemotherapy.
The astragalus oral liquid for treating leukopenia by radiotherapy and chemotherapy is a novel compound Chinese medicinal preparation which is researched by combining folk use experience on the basis of long-term clinical practice and is composed of regional special Chinese medicinal resources as main medicaments. The preparation is composed of the rhizome of rehmannia, astragalus root, glossy privet fruit, angelica, lucid ganoderma and liquorice, adopts the water decoction method, the centrifugation method and the like for extraction and purification technology, has the characteristics of small dosage, stable quality and the like, and has the effects of increasing white blood cells, improving the immunity of organisms, enhancing the cell sensitivity of chemotherapeutics, reducing adverse reactions caused by tumor radiotherapy and chemotherapy and the like, and has small toxic and side effects.
The prescription proportion and the preparation process of the astragalus root and pearl oral liquid for improving the whiteness are as follows: 15g of astragalus membranaceus, 6g of ginseng, 9g of glossy privet fruit, 6g of liquorice, 10g of lucid ganoderma and 6g of angelica, and extracting for 3 times by decoction with 16 times of water for 1.5 hours each time, filtering, combining filtrate, concentrating the liquid medicine at 60 ℃ under reduced pressure to 3 times of the medicinal materials, centrifuging at a high rotating speed (6000-25000 r/min) for 20 minutes, taking supernatant, concentrating the liquid medicine, calculating the raw medicine amount to be 0.312g/mL, adding sucrose with 15% of flavoring agent and sodium sorbate with 0.15% of bacteriostat, mixing uniformly, and subpackaging according to the specification.
At present, the main pharmacodynamics of the astragalus membranaceus oral liquid for increasing white blood cells and improving immune function are studied primarily, chemical components contained in the astragalus membranaceus oral liquid for increasing white blood cells are not qualitatively identified and quantitatively analyzed by a thin layer chromatography, and the quality of medicines is difficult to control accurately.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides a quality evaluation method of astragalus membranaceus oral liquid for improving whiteness.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a quality evaluation method of astragalus membranaceus oral liquid for whitening is characterized by comprising the following steps of: the quality evaluation method of the astragalus membranaceus oral liquid for improving the whiteness comprises the following steps of:
1) Qualitative identification of the raw materials in QIZHUQISHENGBAI oral liquid by thin layer chromatography;
2) Quantitatively analyzing the active ingredients in the raw materials according to a high performance liquid chromatography;
3) And (3) evaluating the quality of the astragalus membranaceus oral liquid by combining the relative density, the pH value and the qualitative identification result obtained in the step (1) with the quantitative analysis result obtained in the step (2).
The raw materials in the step 1) comprise astragalus root, ginseng and angelica.
When the raw material in the step 1) is astragalus, the specific implementation manner of the step 1) is as follows:
taking 20mL of astragalus membranaceus oral liquid for whitening, adding water saturated n-butanol for extraction for 2 times, each time of 20mL, discarding water solution, combining n-butanol solution, washing for 2 times with ammonia test solution, each time of 20mL, and discarding washing solution; evaporating n-butanol solution in water bath, dissolving residue with methanol 4ml, and making into test solution; according to the preparation method of the sample solution, 5g of each negative pair is prepared into a negative control solution, wherein the negative control is prepared from rhizoma panacis majoris, angelica sinensis, glossy privet fruit, lucid ganoderma and liquorice; adding methanol into astragaloside IV reference substance to obtain reference substance solution containing 1mg per 1 mL; respectively sucking 5 mu L of the sample solution, the negative control solution and the control solution, respectively spotting on the same silica gel G thin layer plate, spreading with a lower layer solution placed below 10 ℃ of chloroform-methanol-water as a developing agent, taking out, airing, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color of spots is clear, and respectively inspecting under sunlight and ultraviolet light; in the chromatogram of the test sample, the same brown spots appear in the sunlight at the positions corresponding to the chromatogram of the reference sample; orange-yellow fluorescent spots with the same color appear under ultraviolet light; the volume ratio of chloroform-methanol-water is 15:7:2; the wavelength of the ultraviolet light is 365nm.
When the raw material in the step 1) is the ginseng, the specific implementation manner of the step 1) is as follows:
taking 5mL of astragalus membranaceus oral liquid for whitening, adding water saturated n-butanol for extraction for 2 times, 10mL each time, discarding water solution, and combining n-butanol solution. Evaporating n-butanol solution in water bath, dissolving residue with methanol 2ml, and making into test solution; taking 1g of a reference medicinal material of the rhizoma panacis majoris to prepare a reference medicinal material solution; according to the preparation method of the sample solution, 5g of each negative control substance is prepared into a negative control solution, wherein the negative control substances are astragalus, angelica, glossy privet fruit, lucid ganoderma and liquorice; adding methanol into ginsenoside Ro reference substance to obtain reference substance solution containing 2mg per 1 mL; respectively sucking 5 mu L of the sample solution, the control medicinal material solution, the negative control solution and the control solution, respectively spotting on the same silica gel G thin layer plate, spreading with the upper layer solution of n-butanol-ethyl acetate-methanol-formic acid-water as a developing agent, taking out, air drying, spraying 10% sulfuric acid ethanol solution, heating at 105deg.C until the spot color is clear, and inspecting under ultraviolet light; fluorescent spots with the same color are displayed on the positions corresponding to the chromatogram of the reference substance under ultraviolet light; the volume ratio of n-butanol-ethyl acetate-methanol-formic acid-water is 15:10:0.5:0.3:2; the wavelength of the ultraviolet light is 365nm.
When the raw material in the step 1) is angelica, the specific implementation manner of the step 1) is as follows:
extracting radix astragali oral liquid with diethyl ether 10mL for 2 times, 15mL each time, discarding water solution, and mixing diethyl ether solutions; evaporating the diethyl ether solution in water bath, dissolving the residue with 2ml ethanol, and preparing into test solution; preparing 1g of radix Angelicae sinensis control medicinal material into control medicinal material solution; according to the preparation method of the sample solution, 5g of each negative control substance is prepared into a negative control solution, wherein the negative control substances are astragalus mongholicus, rhizoma panacis majoris, glossy privet fruit, ganoderma lucidum and liquorice; sucking 10 mu L of each of the sample solution, the control medicinal material solution and the negative control solution, respectively spotting on the same silica gel G thin layer plate, developing with n-hexane-ethyl acetate as developing agent, taking out, airing, and inspecting under ultraviolet light; in the chromatogram of the sample, fluorescent spots with the same color appear in the ultraviolet light at the positions corresponding to the chromatogram of the reference sample, and the negative is not interfered; the volume ratio of the n-hexane to the ethyl acetate is 2:1, a step of; the wavelength of the ultraviolet light is 365nm.
The step 2) is to quantitatively analyze the active ingredients of glossy privet fruit, the active ingredients of the rhizoma panacis majoris and the active ingredients of liquorice in the raw materials according to a high performance liquid chromatography.
The step 2) is to quantitatively analyze the active ingredients of ligustrin, ginsenoside Ro and ginsenoside IVa and ammonium glycyrrhizae in the raw materials according to high performance liquid chromatography.
The specific implementation mode of the quantitative analysis is as follows:
2.1 Preparing a mixed reference solution, a test solution and a negative sample solution;
2.2 The mixed reference substance solution, the test substance solution and the negative sample solution prepared in the step 2.1) are quantitatively analyzed by adopting the same chromatographic conditions.
The specific preparation method of the mixed reference substance solution in the step 2.1) is as follows: accurately weighing 17.08mg of terprivet glycoside, 10.00mg of ginsenoside Ro, 8.56mg of panax japonicus saponin IVa and 8.56mg of ammonium glycyrrhizinate reference substance, placing into a brown volumetric flask, adding 10mL of methanol into the volumetric flask, and preparing into 1.708 mg.mL of terprivet glycoside -1 Ginsenoside Ro 1.00 mg.mL -1 Panax japonicus saponin IVa 0.856 mg/mL -1 Ammonium glycyrrhizate 0.856 mg/mL -1 Is prepared from the mixed reference substance solution;
the specific preparation mode of the sample solution is as follows: taking 2mL of astragalus membranaceus oral liquid for whitening, weighing 5g of D101 macroporous resin, passing through a D101 macroporous resin column, eluting with 2BV water, 3BV 20% ethanol and 5BV 60% ethanol in sequence, collecting 60% ethanol eluent, evaporating to dryness, dissolving residues in a 5mL measuring flask with methanol, diluting to a scale with methanol, and shaking uniformly to obtain a sample solution;
the negative sample solution comprises a astragalus membranaceus oral liquid negative sample solution without glossy privet fruits, a astragalus membranaceus oral liquid negative sample solution without bead ginseng, and a astragalus membranaceus oral liquid negative sample solution without liquorice;
the specific preparation method of the astragalus membranaceus whitening oral liquid negative sample solution without glossy privet fruits comprises the following steps: preparing 2mL of astragalus membranaceus oral liquid without glossy privet fruits according to a conventional process, weighing 5g of D101 macroporous resin, passing through a D101 macroporous resin column, eluting with 2BV water, 3BV 20% ethanol and 5BV 60% ethanol in sequence, collecting 60% ethanol eluent, evaporating to dryness, dissolving residues in a 5mL measuring flask with methanol, diluting to a scale with methanol, shaking uniformly, and taking the residues as a negative sample solution of the astragalus membranaceus oral liquid without glossy privet fruits;
the specific preparation method of the astragalus membranaceus whitening oral liquid negative sample solution without the pearl ginseng comprises the following steps: preparing 2mL of astragalus membranaceus white-ascending oral liquid without the pearl ginseng according to a conventional process, weighing 5g of D101 macroporous resin, passing through a D101 macroporous resin column, eluting with 2BV water, 3BV 20% ethanol and 5BV 60% ethanol in sequence, collecting 60% ethanol eluent, evaporating to dryness, dissolving residues in a 5mL measuring flask with methanol, diluting to a scale with methanol, shaking uniformly, and taking the solution as a negative sample solution of the astragalus membranaceus white-ascending oral liquid without the pearl ginseng;
the specific preparation method of the astragalus membranaceus oral liquid negative sample solution without liquorice comprises the following steps: according to the conventional process, preparing 2mL of astragalus membranaceus oral liquid without liquorice, weighing 5g of D101 macroporous resin, passing through a D101 macroporous resin column, eluting with 2BV water, 3BV 20% ethanol and 5BV 60% ethanol in sequence, collecting 60% ethanol eluent, evaporating to dryness, dissolving residues in a 5mL measuring flask with methanol, diluting to a scale with methanol, shaking uniformly, and taking the astragalus membranaceus oral liquid as a negative sample solution without liquorice.
The chromatographic conditions in step 2.2) above are: chromatographic column: an Inertsil ODS-3 column having a size of 4.6mm.times.250mm and a particle diameter of 5 μm; acetonitrile (A) of mobile phase to 0.1 percent of phosphoric acid water (B), and the elution process is 0 to 25min,15 to 20 percent of A; 25-37 min, 20-25% of A; 37-52 min, 25-30% A; 52-55 min, 30-35% of A, 55-60 min, 35-40% of A; 60-70 min, 40-42% of A; the detection wavelength is 203nm; the flow rate is 1.0 mL-min -1 The method comprises the steps of carrying out a first treatment on the surface of the The sample injection amount is 10 mu L; column temperature was 30 ℃.
The invention has the advantages that:
the invention provides a quality evaluation method of astragalus membranaceus oral liquid for whitening, which provides a basis for quality standard. The invention adopts a Thin Layer Chromatography (TLC) method to qualitatively identify astragalus, ginseng and angelica, adopts a Waters e2695 type high performance liquid chromatograph, adopts an Inertsil ODS-3 chromatographic column, adopts acetonitrile-0.1 percent phosphoric acid water as mobile phase for gradient elution, and detects the main medicinal effect ingredient tergirl in the measuring method with the wavelength of 203nmThe contents of glossy privet fruit glycoside, ginsenoside Ro, panax japonicus saponin IVa and ammonium glycyrrhizate. Results: the TLC has good spot separation degree and no negative interference; the mass concentration of the terprivet glycoside, the ginsenoside Ro and the panax japonicus saponin IVa and the ammonium glycyrrhizate are 0.1708 to 1.708 mg.mL respectively -1 、0.1～1.0mg·mL -1 、0.0856～0.856mg·mL -1 And 0.0856 to 0.856 mg/mL -1 The linear relation in the range is good, the average sample adding recovery rates are respectively 98.26%, 95.90%, 95.76% and 98.09%, and the RSD is respectively 1.68%, 2.78%, 1.84% and 2.58%. The method is stable and feasible, and can be used for quality evaluation of Qizhu oral liquid. The quality evaluation method of the astragalus membranaceus oral liquid for increasing white blood cells, which is established by the invention, can be used for quality evaluation and control of the astragalus membranaceus oral liquid for increasing white blood cells, and can also provide reference for the content determination and extraction method of the compound preparation containing the medicinal materials.
Drawings
FIG. 1 is an HPLC chromatogram;
FIG. 2 is a TLC chromatogram of Astragalus membranaceus;
FIG. 3 is a TLC chromatogram of a Panax ginseng C.A.;
FIG. 4 is a TLC chromatogram of Angelica sinensis.
Detailed Description
The astragalus and pearl whitening oral liquid is a compound traditional Chinese medicine preparation for chemo-radiotherapy leukopenia, which is composed of astragalus, glossy privet fruit, ginseng, angelica, ganoderma lucidum and liquorice and has the functions of increasing leucocyte and enhancing the immunity of organisms on the basis of long-term clinical practice and combining folk use experiences of affiliated hospitals of Shanxi university of traditional Chinese medicine. At present, primary researches on main pharmacodynamics of the preparation, including increasing white blood cells and improving immune function, are carried out, chemical components contained in the preparation are not qualitatively identified and quantitatively analyzed by a thin layer chromatography, and the quality of the medicine is difficult to accurately control. The study adopts thin layer chromatography to qualitatively identify radix astragali, rhizoma Panacis Quinquefolii and radix Angelicae sinensis; the method is established to quantitatively analyze the active ingredients of the ligustrum lucidum, the active ingredients of the rhizoma panacis majoris, the active ingredients of the liquorice, namely ammonium glycyrrhizinate, by a High Performance Liquid Chromatography (HPLC), and the relative density, the pH value and the like of the astragalus membranaceus oral liquid are measured by referring to Chinese pharmacopoeia (four parts) of 2020 edition so as to provide reference for quality control of the astragalus membranaceus oral liquid.
1. Material
1.1 instruments
Waters e2695 high performance liquid chromatograph (including autosampler, quaternary pump, column oven, 2998PDA detector); SQ8200HD ultrasonic cleaner (Shanghai crown ultrasonic instruments Co., ltd.); HH-2 constant temperature water bath (Beijing Uygur instrument Co., ltd.); GB204 electronic balance (ten-thousandth, meltre-tolido, switzerland); far infrared radiant heat furnace (Mi technology electric appliances Shanghai Co., ltd.).
1.2 pharmaceutical products and reagents
Astragalus root, pearl ginseng, glossy privet fruit, angelica, lucid ganoderma and liquorice decoction pieces are purchased from Shanxi Xingsheng and der pharmaceutical industry Limited liability company and all meet the Chinese medicinal decoction piece standard of Shanxi province through inspection; terligustrin, ginsenoside Ro, ginsenoside IVa and ammonium glycyrrhizate (batch numbers are respectively HS19515S1, HS19115B2, HS19215B1 and HM19115S2, and the content is 98 percent of the light biotechnology company of Baozhen); astragaloside IV (Chinese food and drug inspection institute, lot number: 0781-20008); chromatographic acetonitrile, phosphoric acid (Tianjin, denou chemical Co., ltd., analytical grade); d101 macroporous resin (Shanghai blue science and technology development Co., ltd., lot number: 170625); silica gel G plate (Qingdao ocean chemical Co., ltd., lot number: 20190903).
2 methods and results
2.1 content determination
2.1.1 chromatographic conditions
Chromatographic column: inertsil ODS-3 column (4.6mm. Times.250 mm,5 μm); acetonitrile (A) of mobile phase to 0.1 percent of phosphoric acid water (B), eluting procedure (0 to 25min,15 to 20 percent of A, 25 to 37min,20 to 25 percent of A, 37 to 52min,25 to 30 percent of A, 52 to 55min,30 to 35 percent of A,55 to 60min,35 to 40 percent of A, 60 to 70min,40 to 42 percent of A); the detection wavelength is 203nm; the flow rate is 1.0 mL-min -1 The method comprises the steps of carrying out a first treatment on the surface of the The sample injection amount is 10 mu L; column temperature was 30 ℃.
2.1.2 mixing control solutions
Precisely weighing terligustrin, ginsenoside Ro, ginsenoside IVa and ammonium glycyrrhizinate pair17.08mg, 10.00mg, 8.56mg and 8.56mg of reference substances are placed in a brown volumetric flask, 10mL of methanol is added, and the terprivet glycoside 1.708 mg.mL is prepared -1 Ginsenoside Ro 1.00 mg.mL -1 Panax japonicus saponin IVa 0.856 mg/mL -1 Ammonium glycyrrhizate 0.856 mg/mL -1 Is used as a reference solution. (preservation at 10 ℃ C. Or below).
2.1.3 sample solutions
Taking 2mL of oral liquid, weighing 5g of D101 macroporous resin, passing through a D101 macroporous resin column, eluting with 2BV water, 3BV 20% ethanol, 5BV 60% ethanol in sequence, collecting 60% ethanol eluent, evaporating to dryness, dissolving residues in a 5mL measuring flask with methanol, diluting to scale with methanol, shaking uniformly, and taking as a sample solution for later use.
2.1.4 negative sample solution
The negative sample of the oral liquid which does not contain glossy privet fruit, the pearl ginseng and the liquorice is prepared according to the prescription proportion and the production process respectively, and the negative sample is prepared according to the method of 2.1.3.
2.1.5 specificity investigation
Taking a sample solution, a reference substance solution and a negative sample solution, and measuring according to the chromatographic conditions under the condition of 2.1.1, wherein the negative is free from interference. The results are shown in fig. 1, a is a test solution, B is a control solution, C is a negative control solution without glossy privet fruit, D is a negative control solution without ginseng beads, E is a negative control solution without licorice, 1# peak represents terligustrin, 2# peak represents ginsenoside Ro, 3# peak represents panax japonicus saponin iv a, and 4# peak represents ammonium glycyrrhizate.
2.1.6 linear relationship investigation
Accurately sucking 2.1.2 pieces of prepared mixed reference substance solution 2mL, 1.5mL, 1mL, 0.5mL and 0.2mL, placing into a 2mL measuring flask, and adding methanol to fix volume to scale. The peak area was measured under the condition of 2.1.1, and the regression equation was obtained by taking the reference mass concentration (X) and the peak area (Y) as standard curves, and the results are shown in Table 1.
Table 1 4 results of linear Range investigation of index Components
2.1.7 precision test
10 mu L of the mixed reference substance solution is precisely sucked, sample injection is continuously repeated for 6 times, and peak areas are measured according to chromatographic conditions under 2.1.1 items, so that RSD of peak areas of the terprivet glycoside, the ginsenoside Ro, the panax japonicus saponin IVa and the ammonium glycyrrhetate are respectively 0.41%, 0.58%, 0.98% and 1.09%, which shows that the instrument has good precision.
2.1.8 repeatability test
Precisely transferring 2mL of the same oral liquid sample (batch number: 210301), preparing according to the method under 2.1.3, sucking 6 parts in parallel, precisely sucking 10 μL, and injecting into liquid chromatograph for determination, wherein the average contents of terligustrin, ginsenoside Ro, rhizoma Panacis Japonici saponin IVa and ammonium glycyrrhizate are respectively 0.704 mg.mL -1 、0.745mg·mL -1 、0.595mg·mL -1 、0.432mg·mL -1 RSD was 1.66%, 2.06%, 2.02%, 1.79%, respectively, indicating that the method was good in reproducibility.
2.1.9 stability test
The oral liquid (batch number: 210301) is respectively measured under the chromatographic conditions of 2.1.1 items in 0, 3, 6, 9, 12 and 24 hours, and the result shows that the peak areas of the specnuezhenide, the ginsenoside Ro, the panax japonicus saponin IVa and the ammonium glycyrrhizate have RSD of 1.44%, 1.32%, 1.87% and 2.01%, which indicates that the product has good internal stability in 24 hours.
2.1.10 sample recovery test
1mL of a sample under the repeatability test item is taken, 6 parts of the sample are parallel, a proper amount of terligustrin, ginsenoside Ro, ginsenoside IVa and ammonium glycyrrhizate reference substances are precisely added, the sample is prepared according to the method under the condition of 2.1.3, the content is measured, the average recovery rate is 98.26 percent, 95.90 percent, 95.76 percent and 98.09 percent respectively, and the RSD is 1.68 percent, 2.78 percent, 1.84 percent and 2.58 percent respectively, which shows that the recovery rate is good, and the result is shown in Table 2.
Table 2 recovery test results (n=6)
2.1.11 durability test
The present test examined Inertsil ODS-3 chromatography columns (4.6 mm. Times.250 mm,5 μm) and ThermoBDS Hypersil C 18 The chromatographic column (5 μm,4.6 mm. Times.150 mm) can achieve a more ideal separation of the components, and the method has good durability.
2.1.12 sample content measurement
8 batches of oral liquid are taken, prepared according to the method under the condition of 2.1.3, and measured according to the condition of 2.1.1. The results are shown in Table 3. Calculating average contents of terligustrin, ginsenoside Ro, ginsenoside IVa and ammonium glycyrrhizate in 8 batches of samples to be 0.683 mg/mL respectively -1 、0.718mg·mL -1 、0.605mg·mL -1 、0.540mg·mL -1 。
Table 3 contains the measurement results (n=1)
2.2 qualitative identification by TLC
2.2.1 Astragalus membranaceus
Referring to the thin layer chromatography of four general rules 0502 in the Chinese pharmacopoeia of 2020 edition, taking 20mL of oral liquid and 5g of negative control to prepare a test solution and a negative control solution; and adding methanol into astragaloside IV reference substance to obtain reference substance solution containing 1mg per 1 mL. Sucking 5 mu L of each of the three solutions, respectively spotting on the same silica gel G thin layer plate, taking a lower layer solution placed below 10 ℃ of chloroform-methanol-water (15:7:2) as a developing agent, developing, taking out, airing, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color of spots is clear, and respectively inspecting under sunlight and ultraviolet light (365 nm). In the chromatogram of the test sample, the same brown spots appear in the sunlight at the positions corresponding to the chromatogram of the reference sample; and orange-yellow fluorescent spots with the same color appear under ultraviolet light. The results are shown in figure 2, wherein in figure 2, A is a radix astragali TLC chromatogram under sunlight, B is a radix astragali TLC chromatogram under ultraviolet light, and 1-3 are sample solutions respectively; 4 is astragaloside IV; 5 is a negative control solution. Negative and no interference, and better spot separation.
2.2.2. Panax ginseng C.A. Meyer
Referring to the thin layer chromatography of four general rules 0502 in Chinese pharmacopoeia of 2020 edition, taking 5mL of oral liquid, 1g of reference medicinal material and 5g of negative reference, and preparing a sample solution, a reference medicinal material solution and a negative reference solution; and adding methanol into the ginsenoside Ro reference substance to obtain reference substance solution containing 2mg per 1 mL. And (3) sucking 5 mu L of each of the four solutions, respectively spotting on the same silica gel G thin layer plate, taking an upper layer solution of n-butyl alcohol-ethyl acetate-methanol-formic acid-water (15:10:0.5:0.3:2) as a developing agent, developing, taking out, airing, spraying a 10% sulfuric acid ethanol solution, heating at 105 ℃ until spots develop clearly, and checking under ultraviolet light (365 nm). The results are shown in figure 3, and 1-3 are shown in figure 3; 4. controlling the medicinal material solution; 5. ginsenoside Ro;6. negative control solution. And fluorescent spots with the same color are displayed on the positions corresponding to the chromatogram of the reference substance under ultraviolet light, no interference is caused in the negative, and the spot separation is good.
2.2.3 Angelica sinensis
Referring to the thin layer chromatography identification under the term of Chinese angelica in the Chinese pharmacopoeia of the 2020 edition and the thin layer chromatography of 0502 in the four general rules of the Chinese pharmacopoeia of the 2020 edition, 10mL of oral liquid, 1g of Chinese angelica control medicine and 5g of negative control are taken to prepare a sample solution, a control medicine solution and a negative control solution. 10 mu L of each of the three solutions is sucked and respectively spotted on the same silica gel G thin layer plate, and the three solutions are unfolded, taken out and dried by taking n-hexane-ethyl acetate (2:1) as an unfolding agent and are inspected under ultraviolet light (365 nm). The results are shown in FIG. 4, 1-3. Test sample solutions; 4. controlling the medicinal material solution; 5. negative control solution. In the chromatogram of the test sample, fluorescent spots with the same color appear under ultraviolet light at the positions corresponding to the chromatogram of the reference sample, and the negative is not interfered.
2.3 inspection
2.3.1 relative Density
The 3 samples were assayed by reference to the relative densitometry (chinese pharmacopoeia 2020 edition four 0601). The results are shown in Table 4.
Table 4 relative density measurement results (n=3)
2.3.2 pH value of
3 samples were assayed by reference to the pH assay (four 0631 of Chinese pharmacopoeia 2020 edition). The results are shown in Table 5.
Table 5 pH value results (n=3)
The invention respectively carries out thin-layer identification on astragalus, rhizoma panacis majoris and angelica in the astragalus oral liquid, the astragalus reference document and the Chinese pharmacopoeia (one part) of 2020 edition confirm that the method of ammonia test solution washing after n-butyl alcohol extraction is adopted to identify astragaloside, and the obtained map spots have better clear separation. The method for treating the Chinese angelica is the same as the method recorded in Chinese pharmacopoeia (one part) of 2020 edition, and the specific shift value is moderate and the spots are clear when the developing condition is optimized to be n-hexane-ethyl acetate (2:1).
Glossy privet fruit, rhizoma panacis majoris and liquorice in the formula of the astragalus membranaceus oral liquid are taken as tonic medicines in the formula, and have the effects of regulating immunity or increasing leucocytes, quantitative analysis is carried out on the terligustrin, ginsenoside Ro, panax japonicus saponin IVa and ammonium glycyrrhetate according to Chinese pharmacopoeia of 2020 edition, methanol-water, acetonitrile-0.1% formic acid water and acetonitrile-0.1% phosphoric acid water of different mobile phases are respectively examined, and finally acetonitrile-0.1% phosphoric acid water is selected for gradient elution, so that the spectrum baseline is stable, and the separation degree is good. The method is a sample treatment method of water decoction and containing 6 medicinal materials, the components are complex and the polarity is larger, 50% methanol and dilute ethanol are respectively adopted for dilution, n-butanol extraction and macroporous resin elution and collection, and the results show that although the methods of direct dilution and liquid-liquid extraction are simple, the operability is good, excessive sample impurities have larger influence, the effective separation of target components and impurity peaks is difficult to achieve, D101 macroporous resin is selected for extraction according to the characteristics of the literature and the target components, and 2BV water, 3BV 20% ethanol and 5 are determined by pre-experimentsBV 60% ethanol 2 BV.h -1 And the 60% ethanol eluent is collected after elution, and the sample solution is fully extracted at the moment without interference, so that the repeatability, the stability and the recovery rate are good. The thin layer identification and content measurement method established by the invention can be used for quality evaluation and control of astragalus membranaceus oral liquid and can also provide reference for the content measurement and extraction method of the compound preparation containing the medicinal materials.
Claims (5)
1. A quality evaluation method of astragalus membranaceus oral liquid for whitening is characterized by comprising the following steps of: the quality evaluation method of the astragalus membranaceus oral liquid for improving the white blood cells comprises the following steps of:
1) Qualitative identification of the raw materials in QIZHUQISHENGBAI oral liquid by thin layer chromatography; the raw materials for qualitative identification comprise radix astragali, radix Panacis Quinquefolii and radix Angelicae sinensis;
2) Quantitatively analyzing active ingredients of fructus Ligustri Lucidi, ginsenoside Ro and ginsenoside IVa and ammonium glycyrrhizae in raw materials according to high performance liquid chromatography; the specific implementation mode of the quantitative analysis is as follows:
2.1 Preparing a mixed reference solution, a test solution and a negative sample solution; the specific preparation mode of the sample solution is as follows: taking 2mL of astragalus membranaceus oral liquid for whitening, weighing 5g of D101 macroporous resin, passing through a D101 macroporous resin column, eluting with 2BV water, 3BV 20% ethanol and 5BV 60% ethanol in sequence, collecting 60% ethanol eluent, evaporating to dryness, dissolving residues in a 5mL measuring flask with methanol, diluting to a scale with methanol, and shaking uniformly to obtain a sample solution;
2.2 Quantitatively analyzing the mixed reference substance solution, the sample solution and the negative sample solution prepared in the step 2.1) by adopting the same chromatographic conditions; the chromatographic conditions are: chromatographic column: an Inertsil ODS-3 column having a size of 4.6mm.times.250mm and a particle diameter of 5 μm; acetonitrile (A) of mobile phase to 0.1 percent of phosphoric acid water (B), and the elution process is 0 to 25min,15 to 20 percent of A; 25-37 min, 20-25% of A; 37-52 min, 25-30% A; 52-55 min, 30-35% of A, 55-60 min, 35-40% of A; 60-70 min, 40-42% of A; the detection wavelength is 203nm;flow rate 1.0mL. Min -1 The method comprises the steps of carrying out a first treatment on the surface of the The sample injection amount is 10 mu L; column temperature is 30 ℃;
3) And (3) evaluating the quality of the astragalus membranaceus oral liquid by combining the relative density, the pH value and the qualitative identification result obtained in the step (1) with the quantitative analysis result obtained in the step (2).
2. The quality evaluation method of astragalus membranaceus whitening oral liquid according to claim 1, which is characterized in that: when the raw material in the step 1) is astragalus, the specific implementation manner of the step 1) is as follows:
taking 20mL of astragalus membranaceus oral liquid for whitening, adding water saturated n-butanol for extraction for 2 times, each time of 20mL, discarding water solution, combining n-butanol solution, washing for 2 times with ammonia test solution, each time of 20mL, and discarding washing solution; evaporating n-butanol solution in water bath, dissolving residue with methanol 4ml, and making into test solution; according to the preparation method of the sample solution, 5g of each negative control substance is prepared into a negative control solution, wherein the negative control substances are ginseng, angelica sinensis, glossy privet fruit, lucid ganoderma and liquorice; adding methanol into astragaloside IV reference substance to obtain reference substance solution containing 1mg per 1 mL; respectively sucking 5 mu L of the sample solution, the negative control solution and the control solution, respectively spotting on the same silica gel G thin layer plate, spreading with a lower layer solution placed below 10 ℃ of chloroform-methanol-water as a developing agent, taking out, airing, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color of spots is clear, and respectively inspecting under sunlight and ultraviolet light; in the chromatogram of the test sample, the same brown spots appear in the sunlight at the positions corresponding to the chromatogram of the reference sample; orange-yellow fluorescent spots with the same color appear under ultraviolet light; the volume ratio of chloroform-methanol-water is 15:7:2; the wavelength of the ultraviolet light is 365nm.
3. The quality evaluation method of astragalus membranaceus whitening oral liquid according to claim 1, which is characterized in that: when the raw material in the step 1) is the ginseng, the specific implementation mode of the step 1) is as follows:
extracting radix astragali oral liquid with water saturated n-butanol for 2 times (10 mL each time), discarding water solution, and mixing n-butanol solutions; evaporating n-butanol solution in water bath, dissolving residue with methanol 2ml, and making into test solution; taking 1g of a reference medicinal material of the rhizoma panacis majoris to prepare a reference medicinal material solution; according to the preparation method of the sample solution, 5g of each negative control substance is prepared into a negative control solution, wherein the negative control substances are astragalus, angelica, glossy privet fruit, lucid ganoderma and liquorice; adding methanol into ginsenoside Ro reference substance to obtain reference substance solution containing 2mg per 1 mL; respectively sucking 5 mu L of the sample solution, the control medicinal material solution, the negative control solution and the control solution, respectively spotting on the same silica gel G thin layer plate, spreading with the upper layer solution of n-butanol-ethyl acetate-methanol-formic acid-water as a developing agent, taking out, air drying, spraying 10% sulfuric acid ethanol solution, heating at 105deg.C until the spot color is clear, and inspecting under ultraviolet light; fluorescent spots with the same color are displayed on the positions corresponding to the chromatogram of the reference substance under ultraviolet light; the volume ratio of n-butanol-ethyl acetate-methanol-formic acid-water is 15:10:0.5:0.3:2; the wavelength of the ultraviolet light is 365nm.
4. The quality evaluation method of astragalus membranaceus whitening oral liquid according to claim 1, which is characterized in that: when the raw material in the step 1) is angelica, the specific implementation manner of the step 1) is as follows:
extracting radix astragali oral liquid with diethyl ether 10mL for 2 times, 15mL each time, discarding water solution, and mixing diethyl ether solutions; evaporating the diethyl ether solution in water bath, dissolving the residue with 2ml ethanol, and preparing into test solution; preparing 1g of radix Angelicae sinensis control medicinal material into control medicinal material solution; according to the preparation method of the sample solution, 5g of each negative control substance is prepared into a negative control solution, wherein the negative control substances are astragalus mongholicus, rhizoma panacis majoris, glossy privet fruit, ganoderma lucidum and liquorice; sucking 10 mu L of each of the sample solution, the control medicinal material solution and the negative control solution, respectively spotting on the same silica gel G thin layer plate, developing with n-hexane-ethyl acetate as developing agent, taking out, airing, and inspecting under ultraviolet light; in the chromatogram of the sample, fluorescent spots with the same color appear in the ultraviolet light at the positions corresponding to the chromatogram of the reference sample, and the negative is not interfered; the volume ratio of the n-hexane to the ethyl acetate is 2:1, a step of; the wavelength of the ultraviolet light is 365nm.
5. The quality evaluation method of astragalus membranaceus oral liquid for increasing white blood cells according to any one of claims 1 to 4, which is characterized by comprising the following steps of: the specific preparation method of the mixed reference substance solution in the step 2.1) is as follows: 17.08mg of terprivet glycoside, 10.00mg of ginsenoside Ro, 8.56mg of panax japonicus saponin IVa and 8.56mg of ammonium glycyrrhizinate reference substance are precisely weighed, placed in the same brown volumetric flask, 10mL of methanol is added into the volumetric flask, and 1.708 mg.mL of terprivet glycoside is prepared -1 Ginsenoside Ro 1.00 mg.mL -1 Panax japonicus saponin IVa 0.856 mg/mL -1 Ammonium glycyrrhizate 0.856 mg/mL -1 Is prepared from the mixed reference substance solution;
the negative sample solution comprises a astragalus membranaceus oral liquid negative sample solution without glossy privet fruits, a astragalus membranaceus oral liquid negative sample solution without bead ginseng, and a astragalus membranaceus oral liquid negative sample solution without liquorice;
the specific preparation method of the astragalus membranaceus whitening oral liquid negative sample solution without glossy privet fruits comprises the following steps: preparing 2mL of astragalus membranaceus oral liquid without glossy privet fruits according to a conventional process, weighing 5g of D101 macroporous resin, passing through a D101 macroporous resin column, eluting with 2BV water, 3BV 20% ethanol and 5BV 60% ethanol in sequence, collecting 60% ethanol eluent, evaporating to dryness, dissolving residues in a 5mL measuring flask with methanol, diluting to a scale with methanol, shaking uniformly, and taking the residues as a negative sample solution of the astragalus membranaceus oral liquid without glossy privet fruits;
the specific preparation method of the astragalus membranaceus whitening oral liquid negative sample solution without the pearl ginseng comprises the following steps: preparing 2mL of astragalus membranaceus white-ascending oral liquid without the pearl ginseng according to a conventional process, weighing 5g of D101 macroporous resin, passing through a D101 macroporous resin column, eluting with 2BV water, 3BV 20% ethanol and 5BV 60% ethanol in sequence, collecting 60% ethanol eluent, evaporating to dryness, dissolving residues in a 5mL measuring flask with methanol, diluting to a scale with methanol, shaking uniformly, and taking the solution as a negative sample solution of the astragalus membranaceus white-ascending oral liquid without the pearl ginseng;
the specific preparation method of the astragalus membranaceus oral liquid negative sample solution without liquorice comprises the following steps: according to the conventional process, preparing 2mL of astragalus membranaceus oral liquid without liquorice, weighing 5g of D101 macroporous resin, passing through a D101 macroporous resin column, eluting with 2BV water, 3BV 20% ethanol and 5BV 60% ethanol in sequence, collecting 60% ethanol eluent, evaporating to dryness, dissolving residues in a 5mL measuring flask with methanol, diluting to a scale with methanol, shaking uniformly, and taking the astragalus membranaceus oral liquid as a negative sample solution without liquorice.
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