CN114137142A - Thin-layer chromatography identification method for rhus chinensis - Google Patents
Thin-layer chromatography identification method for rhus chinensis Download PDFInfo
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The invention relates to the technical field of traditional Chinese medicine identification, and particularly relates to a thin-layer chromatography identification method of rhus chinensis. The thin-layer chromatography identification method is characterized in that myricitrin is used as a reference substance and is matched with a rhus chinensis control medicinal material to identify a rhus chinensis sample. The thin-layer chromatography obtained by analyzing the rhus chinensis by adopting the method has good separation effect, round and clear spots, moderate specific displacement value and good reproducibility; the method is simple to operate, simple in equipment, easy in color development, high in development speed, and easy to judge the result, provides a basis for identifying the rhus chinensis, and provides a reliable guarantee for the medication safety of the rhus chinensis.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine identification, and particularly relates to a thin-layer chromatography identification method of rhus chinensis.
Background
The Rhus chinensis Mill is Rhus chinensis Mill of AnacardiaceaeRhus chinensis Mill.Drying the whole plant. Harvesting in summer and autumn, cleaning, and drying; alias: salt frost cypress, haloxylon, tabebuia sinensis, cattail root salt and common monkshood mother rootSalt and quintuplet. Rhus chinensis Mill is sour, slightly bitter and cool; has antitussive, hemostatic, astringent, and toxic materials clearing away effects; it can be used for treating phlegm cough, hematochezia, bloody dysentery, night sweat, superficial infection, ulcer, eczema, and snake and insect bite. Except northeast, inner Mongolia and Xinjiang, other provinces of China all have the elevation in sunny hillsides, valleys and creeks with elevation of 170 + 2700 m; distributed in india, central and south peninsula, malaysia, indonesia, japan and korea; the herbs are commonly used in Guangxi provinces.
Rhus chinensis is a traditional Chinese medicine and is recorded as early as Shanhai Jing, the salt on fruits and wood can be eaten, the plants can be used as the medicine for all people, and the effect is good when the Rhus chinensis is used alone without being compatible with other traditional Chinese medicines. The medicine for each part is generally divided into 2 types for oral administration and 2 types for external use, the decoction is taken orally, and the pounding, decoction and water washing or grinding and mixing for external use are performed. All parts of the Rhus chinensis Mill plant such as root leaves, stems, fruits and barks have medicinal value, and the root of the Rhus chinensis Mill has the effects of reducing phlegm, relieving asthma, regulating middle warmer and benefiting vital energy; the leaf has effects of relieving swelling and removing toxic substance; the flower and fruit have the effects of astringing lung and intestine, nourishing kidney and arresting seminal emission, stopping bleeding and stopping sweating. The root is mainly used for treating chronic bronchitis, coronary heart disease, fatigue and debilitation, rheumatic arthralgia, sciatica, lumbar muscle strain, sprain and traumatic injury; the root bark is mainly used for treating inappetence, infantile malnutrition and postpartum uterine dyspnea; the leaf is mainly used for treating skin allergy, eczema, dermatitis and aphtha; the flowers and fruits are mainly used for treating cough due to lung deficiency, night sweat, spermatorrhea, leg ulcer, chronic diarrhea, rectocele and traumatic hemorrhage. The Rhus chinensis Mill is clinically applied to chronic tracheitis, infectious hepatitis, functional uterine bleeding and rheumatic arthralgia. At present, the clinically used water decoction of the root of Chinese sumac is used for treating coronary heart disease, angina, chest distress, suffocating, lung abscess, infantile chronic diarrhea and the like, and has high efficiency and little side effect. At present, some relevant reports are made on the chemical components and content measurement of rhus chinensis, but few reports are made on the identification method of rhus chinensis.
Disclosure of Invention
The invention aims to provide a thin-layer chromatography identification method of rhus chinensis. The thin-layer chromatography obtained by analyzing the rhus chinensis by adopting the method has good separation effect, round and clear spots, moderate specific displacement value and good reproducibility; the method is simple to operate, simple in equipment and easy to judge the result, and provides a basis for identifying the rhus chinensis.
In order to achieve the purpose, the invention adopts the following technical scheme:
a thin layer chromatography identification method of rhus chinensis, comprising the following steps:
(1) preparing a test solution and a reference medicinal material solution: taking 1g of Rhus chinensis Mill powder, adding 25ml of 60 vol% ethanol, performing ultrasonic treatment for 30 minutes, filtering, evaporating filtrate, and dissolving residue with 2ml of methanol to obtain a sample solution; preparing 1g of Rhus chinensis Mill reference medicinal material powder, and preparing reference medicinal material solution by the same method;
(2) preparation of control solutions: taking myricitrin reference substance, adding 60% ethanol to make into 0.2mg solution per 1ml as reference substance solution;
(3) according to the test of thin-layer chromatography of 0502 of the general Law of the Chinese pharmacopoeia 2015, absorbing 2 mu L of each of a test solution, a reference medicinal material solution and a reference solution, respectively dropping the test solution, the reference medicinal material solution and the reference solution on the same silica gel G thin-layer plate, developing by taking trichloromethane-methanol-formic acid as a developing agent in a volume ratio of 17:5:2, taking out, drying in the air, spraying an aluminum trichloride reagent, drying by hot air, and inspecting under 365nm ultraviolet lamps; in the chromatogram of the test solution, fluorescent spots of the same color appear at the positions corresponding to the chromatogram of the reference solution and the chromatogram of the reference solution.
The invention has the beneficial effects that:
the thin-layer chromatography obtained by analyzing the rhus chinensis by adopting the method has good separation effect, round and clear spots, moderate specific shift value and good reproducibility; the method is simple to operate, simple in equipment, easy in color development, high in development speed, easy to judge the result and provides a basis for identifying the rhus chinensis. According to the invention, by investigating factor conditions such as different brands of thin-layer plates, different development temperatures and humidities, different sample application modes and the like, the result shows that the thin-layer chromatography identification method for the rhus chinensis, which is established by the invention, has good durability and strong applicability to different brands of prefabricated plates, development temperatures, relative humidities and sample application modes. The method for identifying the rhus chinensis by the thin-layer chromatography is used for qualitatively analyzing the rhus chinensis, is simple to operate, can quickly identify the truth of the rhus chinensis, and provides reliable guarantee for the medication safety of the rhus chinensis.
Drawings
Figure 1 is a chromatogram for thin layer chromatography identification of 15 batches of rhus chinensis samples, identified in the figure: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7, YFM-7, 8, a reference substance, 9, YFM-8, 10, YFM-9, 11, YFM-10, 12, YFM-11, 13, YFM-12, 14, YFM-13, 15, YFM-14, 16 and YFM-15; chromatographic conditions are as follows: merck silica gel G plate, strip spotting, spot size 2 μ l, temperature: 25 ℃, relative humidity: 65% under ultraviolet lamp (365 nm).
Figure 2 is a chromatogram for thin layer chromatography identification of 15 batches of rhus chinensis samples, identified in the figure: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7, YFM-7, 8, a reference substance, 9, YFM-8, 10, YFM-9, 11, YFM-10, 12, YFM-11, 13, YFM-12, 14, YFM-13, 15, YFM-14, 16 and YFM-15; chromatographic conditions are as follows: qingdao silica gel G plate, strip sample application, sample application amount of 2 mul, temperature: 25 ℃, relative humidity: 65% under ultraviolet lamp (365 nm).
FIG. 3 is a TLC chromatogram of different extraction solvents under otherwise identical conditions for the thin layer chromatography identification of Rhus chinensis Mill according to the invention, wherein the symbols: 1. YFM-1, 60% ethanol; 2. YFM-2, 60% ethanol; 3. YFM-3, 60% ethanol; 4. YFM-4, 60% ethanol; 5. YFM-5, ethanol; 6. YFM-6, ethanol; 7. myricitrin reference substance.
FIG. 4 is a TLC chromatogram of a different extraction method under otherwise identical conditions, according to the thin layer chromatography identification method of Rhus chinensis Mill of the present invention, wherein: 1. YFM-12, ultrasonic for 30 minutes; 2. YFM-15, ultrasonic treatment for 30 minutes; heating and refluxing YFM-12 for 30 minutes; heating and refluxing YFM-15 for 30 minutes; 5. YFM-12, ultrasonic for 60 minutes; 6. YFM-15, ultrasonic treatment for 60 minutes; 7. myricitrin reference substance.
Fig. 5 is a TLC chromatogram obtained by detection with chloroform-methanol-formic acid (10:5:1) as developing agent according to the thin layer chromatography identification method of rhus chinensis, wherein the marks in the chromatogram are as follows: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7 and a reference substance.
FIG. 6 is a TLC chromatogram obtained by detection with chloroform-methanol-formic acid (15:5:2) as developing agent according to the thin layer chromatography identification method of Rhus chinensis Mill of the present invention, wherein the symbols are as follows: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7 and a reference substance.
FIG. 7 is a TLC chromatogram obtained by detection with chloroform-methanol-formic acid (16:5:2) as developing agent according to the thin layer chromatography identification method of Rhus chinensis Mill of the present invention, wherein the symbols are as follows: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7 and a reference substance.
FIG. 8 is a TLC chromatogram obtained by detection with chloroform-methanol-formic acid (17:5:2) as developing agent according to the thin layer chromatography identification method of Rhus chinensis Mill of the present invention, wherein the symbols are as follows: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7 and a reference substance.
FIG. 9 is a TLC chromatogram obtained by detection with chloroform-methanol-formic acid (18:5:2) as developing agent according to the thin layer chromatography identification method of Rhus chinensis Mill of the present invention, wherein the symbols are as follows: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7 and a reference substance.
FIG. 10 is a TLC chromatogram obtained by detection with chloroform-methanol-formic acid (20:5:2) as developing agent according to the thin layer chromatography identification method of Rhus chinensis Mill of the present invention, wherein the symbols are as follows: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7 and a reference substance.
Fig. 11 is a TLC chromatogram obtained by detection at a development temperature of 4 ℃ according to the thin layer chromatography identification method of rhus chinensis, wherein the symbols in the chromatogram are as follows: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7 and a reference substance.
Fig. 12 is a TLC chromatogram obtained by detection at a development temperature of 25 ℃ according to the thin layer chromatography identification method of rhus chinensis, wherein the symbols in the chromatogram are as follows: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7 and a reference substance.
Fig. 13 is a TLC chromatogram obtained by detection under development conditions with a relative humidity RH of 65% according to the thin layer chromatography identification method of rhus chinensis, wherein the symbols are as follows: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7 and a reference substance.
Fig. 14 is a TLC chromatogram obtained by detection under the development condition of 85% relative humidity RH according to the thin layer chromatography identification method of rhus chinensis, wherein the symbols are as follows: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7 and a reference substance.
Fig. 15 is a TLC chromatogram obtained by detection in a dot spotting manner according to the thin layer chromatography identification method of rhus chinensis, wherein the symbols in the chromatogram are as follows: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7 and a reference substance.
Fig. 16 is a TLC chromatogram obtained by detection in a striped spotting manner according to the thin layer chromatography identification method of rhus chinensis, wherein the following marks are marked: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7 and a reference substance.
FIG. 17 is a TLC chromatogram obtained by performing detection on a silica gel G pre-fabricated thin-layer plate of the institute of chemical industry, cigarette Taiwan (batch No. 20161125, 100X 100 mm) brand according to the thin-layer chromatography identification method of Rhus chinensis Mill of the present invention, wherein the symbols: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7 and a reference substance.
Fig. 18 is a TLC chromatogram obtained by detection under the condition of using a silica gel G prefabricated thin-layer plate of Qingdao ocean chemical Co., Ltd (batch number 20181220, 100 × 100 mm) according to the thin-layer chromatography identification method of rhus chinensis, wherein the chromatogram is marked as follows: 1. YFM-1, 2, YFM-2, 3, YFM-3, 4, YFM-4, 5, YFM-5, 6, YFM-6, 7 and a reference substance.
Detailed Description
In order to describe the present invention in more detail, the present invention will be further described with reference to the following examples.
Example 1
A thin layer chromatography identification method of rhus chinensis, comprising the following steps:
(1) preparing a test solution and a reference medicinal material solution: taking 1g of Rhus chinensis Mill powder, adding 25ml of 60 vol% ethanol, performing ultrasonic treatment for 30 minutes, filtering, evaporating filtrate, and dissolving residue with 2ml of methanol to obtain a sample solution; preparing 1g of Rhus chinensis Mill reference medicinal material powder, and preparing reference medicinal material solution by the same method;
(2) preparation of control solutions: taking myricitrin reference substance, adding 60% ethanol to make into 0.2mg solution per 1ml as reference substance solution;
(3) according to the thin layer chromatography (2015 version of Chinese pharmacopoeia 0502), absorbing 2 μ L of each of the test solution, the reference medicinal material solution and the reference solution, respectively dropping on the same silica gel G thin layer plate, developing with chloroform-methanol-formic acid as developing agent at volume ratio of 17:5:2, taking out, air drying, spraying with aluminum trichloride reagent, drying with hot air, and inspecting under 365nm ultraviolet lamp; in the chromatogram of the test solution, fluorescent spots of the same color appear at the positions corresponding to the chromatogram of the reference solution and the chromatogram of the reference solution.
The applicant collects 15 batches of rhus chinensis samples from Guangxi, the detailed information is shown in the following table 1, wherein, the rhus chinensis samples YFM-3 and YFM-13 are simultaneously prepared into cured tobacco leaf specimens, and the results are determined to be rhus chinensis of the family Anacardiaceae through the identification of auxiliary researchers of West Song base professor of Guangxi traditional Chinese medicine university and Huangyunfeng research institute of Guangxi traditional Chinese medicineRhus chinensis Mill.YFM-3 and YFM-13 are used as reference medicinal materials of rhus chinensis and are compared with other samples in the experiment. After completion of sample collection, all 15 samples (about 500 g) were subjected to a pulverization treatment and sieved through a 40-mesh sieve for use.
The applicant identifies 15 batches of samples in the table 1 according to the thin-layer chromatography identification method of rhus chinensis, and the chromatogram is shown in fig. 1-2. The result shows that 15 batches of samples are tested according to the method and all meet the specification, and the thin-layer chromatography separation effect is good, spots are round and clear, the specific displacement value is moderate, and the reproducibility is good. Spots of the same color appear in the 15 chromatogram of the test solution at the positions corresponding to the chromatogram of the reference solution; YFM-3 and YFM-13 samples are used as reference medicinal materials, and spots with the same color are displayed on other 13 batches of samples at the positions corresponding to the chromatogram of the reference medicinal materials.
In addition, the applicant also conducts durability test investigation on the thin-layer chromatography identification method of rhus chinensis, and specifically comprises the following steps: according to the general rules of the four parts of the 2015 version of the Chinese pharmacopoeia, the factors and conditions of different extraction solvents, different extraction modes, different developing agents, different brands of thin-layer plates, different developing temperatures and humidity, different sample application modes and the like are investigated respectively. The method comprises the following specific steps:
1. different extraction solvents: according to the thin-layer chromatography identification method of rhus chinensis, under the condition of the same other conditions, the extraction solvent: ultrasonic extraction of 60% ethanol and ethanol. As a result: the separation effect of the two solvent extractions is good. See fig. 3.
2. Investigation of different extraction modes: according to the thin-layer chromatography identification method of rhus chinensis, under the condition of the same other conditions, different extraction methods of 30 minutes of ultrasonic treatment, 60 minutes of ultrasonic treatment and 30 minutes of heating reflux are respectively considered. As a result: the TLC separation effect under the three extraction methods is good. See fig. 4.
3. Selecting a spreading agent proportion gradient: according to the thin-layer chromatography identification method of rhus chinensis disclosed by the invention, under the same other conditions, chloroform-methanol-formic acid (10:5:1), chloroform-methanol-formic acid (15:5:2), chloroform-methanol-formic acid (16:5:2), chloroform-methanol-formic acid (17:5:2), chloroform-methanol-formic acid (18:5:2) and chloroform-methanol-formic acid (20:5:2) are subjected to chromatography investigation by using developing agents with different concentrations. As a result: referring to fig. 5-10, the separation of chloroform-methanol-formic acid (17:5:2) was better (fig. 8).
4. Investigation of different development temperatures: according to the thin-layer chromatography identification method of the rhus chinensis, chromatography investigation is respectively carried out on two different temperature conditions of 4 ℃ and 25 ℃ under the condition of the same other conditions. As a result: the TLC separation effect is good under the two temperature conditions. See fig. 11-12.
5. Examination of different relative humidities: according to the thin-layer chromatography identification method of the rhus chinensis, two different relative humidity conditions with the relative humidity of 65% and 85% are respectively subjected to chromatography investigation under the same other conditions. As a result: the TLC separation effect under the two relative humidity conditions is good. See fig. 13-14.
6. Investigation of different spotting patterns: according to the thin-layer chromatography identification method of rhus chinensis, the chromatography investigation is respectively carried out on the dot-shaped spotting mode and the strip-shaped spotting mode under the condition of the same other conditions. As a result: the TLC separation effect of the two sample application modes is good. See fig. 15-16.
7. Investigation of different brands of thin-layer plates: according to the thin-layer chromatography identification method of rhus chinensis, chromatography investigation is respectively carried out on silica gel G prefabricated thin-layer plates of two brands of Nicoti city chemical industry research institute (batch number 20161125, 100 x 100 mm) and Qingdao ocean chemical industry Co., Ltd (batch number 20181220, 100 x 100 mm) under the same other conditions. As a result: TLC of silica gel G precast slabs of two brands can achieve the separation effect. See fig. 17-18.
And (4) conclusion: the TLC identification method established by the invention has good durability and strong applicability to the precast slabs of different brands, the development temperature, the relative humidity and the sample application mode.
Claims (1)
1. The thin-layer chromatography identification method of rhus chinensis is characterized by comprising the following steps of:
(1) preparing a test solution and a reference medicinal material solution: taking 1g of Rhus chinensis Mill powder, adding 25ml of 60 vol% ethanol, performing ultrasonic treatment for 30 minutes, filtering, evaporating filtrate, and dissolving residue with 2ml of methanol to obtain a sample solution; preparing 1g of Rhus chinensis Mill reference medicinal material powder, and preparing reference medicinal material solution by the same method;
(2) preparation of control solutions: taking myricitrin reference substance, adding 60% ethanol to make into 0.2mg solution per 1ml as reference substance solution;
(3) according to the test of thin-layer chromatography of 0502 of the general Law of the Chinese pharmacopoeia 2015, absorbing 2 mu L of each of a test solution, a reference medicinal material solution and a reference solution, respectively dropping the test solution, the reference medicinal material solution and the reference solution on the same silica gel G thin-layer plate, developing by taking trichloromethane-methanol-formic acid as a developing agent in a volume ratio of 17:5:2, taking out, drying in the air, spraying an aluminum trichloride reagent, drying by hot air, and inspecting under 365nm ultraviolet lamps; in the chromatogram of the test solution, fluorescent spots of the same color appear at the positions corresponding to the chromatogram of the reference solution and the chromatogram of the reference solution.
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