CN115389694B - Thin layer chromatography for simultaneously identifying Notopterygii rhizoma, radix Angelicae Pubescentis, radix Angelicae sinensis and rhizoma Ligustici Chuanxiong in Juanbi decoction - Google Patents
Thin layer chromatography for simultaneously identifying Notopterygii rhizoma, radix Angelicae Pubescentis, radix Angelicae sinensis and rhizoma Ligustici Chuanxiong in Juanbi decoction Download PDFInfo
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Abstract
The invention belongs to the technical field of detection of traditional Chinese medicine components, and particularly relates to a thin layer chromatography method for simultaneously identifying notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii in Juanbi decoction. The thin layer chromatography for simultaneously identifying notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii in Juanbi decoction provided by the invention comprises the following steps: s1, preparing a sample solution; s2, preparing a control medicinal material solution; s3, preparing a reference substance solution; s4, thin-layer chromatography analysis. The thin layer identification method provided by the invention can be used for simultaneously identifying the notopterygium root, the radix angelicae pubescentis, the angelica sinensis and the ligusticum wallichii of the Jubi decoction, has the advantages of strong specificity of thin layer identification, simple and convenient operation, rapidness, strong durability and high detection efficiency, effectively reduces the detection cost, provides an important technical means for quality control of the Jubi decoction, and is an important guarantee for realizing the safety and the effectiveness of the Jubi decoction.
Description
Technical Field
The invention belongs to the technical field of detection of traditional Chinese medicine components, and particularly relates to a thin layer chromatography method for simultaneously identifying notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii in Juanbi decoction.
Background
The Juanbi decoction comes from medical heart understanding of Qing Dynasty Cheng Songling and has the effects of dispelling wind and removing dampness and relieving arthralgia and pain. The medicine composition of the prescription comprises: qiang, duhuo, qin Marcrophylla, kadsura pepper stem, mulberry twig, chuan-xiong rhizome, dang Gui, gui Xin Wu, mu Xiang, ru Xiang and prepared Licorice root five minutes. In the formula, the notopterygium root and the radix angelicae pubescentis are taken as monarch drugs for dispelling wind and removing dampness, the gentiana macrophylla, the kadsura pepper stem and the mulberry twig are taken as ministerial drugs for helping the notopterygium root and the radix angelicae pubescentis to dispel wind and remove dampness, the ligusticum wallichii and the angelica are taken as ministerial drugs for assisting the blood nourishing and regulating nutrient, the costustoot, the frankincense and the blood are taken as analgesic drugs, the cassia bark is taken as ministerial drugs for warming the channel to dispel cold, the blood vessel is taken as the blood vessel. The prescription takes wind damp-dispelling medicines as main materials, and is matched with blood-nourishing, blood-activating, qi-flowing and pain-relieving medicines, and the compatibility of the prescription focuses on the conditioning of qi and blood while dispelling wind and eliminating dampness and relieving arthralgia and pain.
Modern pharmacological studies have demonstrated that: the water-soluble component of Notopterygium root can inhibit delayed type allergy and inflammatory reaction; the single water extract has anti-inflammatory and analgesic effects; ferulic acid in radix Angelicae sinensis and rhizoma Ligustici Chuanxiong has effects of enhancing myocardial blood supply and relieving myocardial ischemia; the gentiana macrophylla has the effects of anti-inflammatory, analgesic and antipyretic, and indirectly influences pituitary gland through a nerve and body fluid system, so that the adrenal cortex function is enhanced, and the secretion of corticoids is increased; the whole prescription has the functions of resisting inflammation, easing pain, regulating immunity and improving microcirculation, thereby increasing blood and oxygen supply of nerve tissues and promoting repair of peripheral nerve injury, is a common prescription for clinically treating wind-cold-dampness arthralgia, and has the effects of dispelling wind and cold, eliminating dampness and dispersing arthralgia. Along with the deep research, the clinical application range of the Juanbi decoction is continuously expanded, and the modified prescription of the Juanbi decoction along with the symptoms is used for a plurality of symptoms.
The Juanbi decoction belongs to 79 th classical names of 100 classical names in the ancient classical names catalog (first batch) made by the national drug administration of the national Chinese medicine administration of 2018. The classical prescription has definite clinical curative effect, and the modern scientific technology is used for developing the traditional Chinese medicine preparation which is convenient to carry and take, thereby not only being the inheritance of traditional Chinese medicine, but also better promoting the clinical application of the classical prescription.
The quality of the traditional Chinese medicine is the fundamental guarantee of the clinical curative effect of the traditional Chinese medicine, and is also the basic stone for the high-quality development and the international trend of the traditional Chinese medicine. The quality standard of the traditional Chinese medicine is an important measure for ensuring the quality of the traditional Chinese medicine. Thin layer identification is an important analytical means for controlling the quality of traditional Chinese medicines. The technical guidelines for the quality standard study of new traditional Chinese medicines (trial) for trial 5 months in 2020 encourages the establishment of thin-layer chromatography methods for simultaneously identifying multiple medicines. The thin layer identification method carried in a formulation of Chinese pharmacopoeia (2020 edition) is known from the longitudinal observation, and basically, the preparation method, developing agent and developing condition of the test sample are optimized for each medicine. The Chinese patent application CN 113325125A discloses a method for identifying the thin layer of a Chinese reference sample of an ancient classical prescription compound preparation and measuring the total flavone content, and the method also adopts three thin layer chromatography methods to identify the notopterygium root, the radix angelicae pubescentis and the gentiana macrophylla in the Chinese reference sample, so that the detection efficiency is low, the detection period is long, and the time, the labor and the reagent are wasted. Therefore, finding a simple and quick detection method for the traditional Chinese medicine compound preparation is a difficult problem that the quality control of the traditional Chinese medicine must be overcome.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a thin layer chromatography for simultaneously identifying notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii in Juanbi decoction. The invention establishes a thin-layer identification method of 'one-test multi-medicine', namely in a thin-layer system, four medicine flavors of notopterygium root, radix angelicae pubescentis, angelica and ligusticum wallichii in the Juanbi decoction are identified simultaneously, the operation is simple and convenient, the operation is quick, the durability is strong, the detection efficiency can be effectively improved, the specificity of thin-layer identification is strong, the detection cost is effectively reduced, the quality of the Juanbi decoction product can be effectively controlled, an important technical means is provided for the quality control of the Juanbi decoction, and the important guarantee of the safety and the effectiveness is realized.
The technical scheme of the invention is as follows:
thin layer chromatography for identifying Notopterygii rhizoma, radix Angelicae Pubescentis, radix Angelicae sinensis and rhizoma Ligustici Chuanxiong in Juanbi decoction simultaneously comprises the following steps:
s1, preparing a sample solution: adding methanol into a reference sample of the Juanbi decoction for ultrasonic treatment, filtering, evaporating filtrate to dryness, adding water into residues, extracting with petroleum ether, mixing petroleum ether solutions, evaporating to dryness, and dissolving residues with ethyl acetate to obtain a sample solution;
s2, preparing a control medicinal material solution: extracting radix Angelicae Pubescentis with methanol, performing ultrasonic treatment, and filtering to obtain filtrate as radix Angelicae Pubescentis control solution;
s3, preparing a reference substance solution: taking ligustilide reference substance and notopterygium alcohol reference substance, and respectively adding methanol to prepare reference substance solutions;
s4, thin-layer chromatography analysis: sucking the sample solution, the control medicinal material solution and the control solution, respectively spotting on the same thin layer plate, spreading with spreading agent, taking out, air drying, inspecting under ultraviolet lamp, and identifying radix Angelicae sinensis and rhizoma Ligustici Chuanxiong; spraying color-developing agent, heating until the spots develop clearly, and inspecting under ultraviolet lamp to identify Notopterygii rhizoma and radix Angelicae Pubescentis.
Further, the developing agent in the step S4 is cyclohexane, dichloromethane, ethyl acetate, and formic acid according to a volume ratio of 5:1:2: 0.2.
The developing agent adopted in the invention is prepared from cyclohexane, dichloromethane, ethyl acetate and formic acid according to the volume ratio of 5:1:2:0.2, the separation degree of each component is good, and when the composition is applied to thin layer chromatography detection, the composition is negative without interference, and the composition has strong specificity and good durability.
Further, the preparation method of the reference sample of the Juanbi decoction in the step S1 is as follows:
taking eleven decoction pieces of 3.73g of notopterygium root, 3.73g of radix angelicae pubescentis, 1.87g of cinnamon, 3.73g of gentiana macrophylla, 11.19g of angelica sinensis, 2.61g of ligusticum wallichii, 1.87g of honey-fried licorice root, 7.46g of kadsura pepper stem, 11.19g of mulberry twig, 2.98g of frankincense and 2.98g of costustoot, adding 400mL of water, soaking for 30 minutes, boiling with strong fire, boiling with slow fire, filtering with a 350-mesh screen while hot, and freeze-drying the filtrate to obtain a reference sample of the Juanbi decoction.
Further, the preparation method of the sample solution in the step S1 is as follows: taking 2g of a reference sample of the Juanbi decoction, adding 25mL of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, dissolving the residue in 20mL of water, adding petroleum ether, shaking and extracting for 2 times, each time for 20mL, combining petroleum ether solutions, evaporating to dryness, and dissolving the residue in 2mL of ethyl acetate to obtain a sample solution; the boiling range of the petroleum ether is 60-90 ℃.
Further, the preparation method of the control medicinal material solution in the step S2 is as follows:
taking 0.2g of radix angelicae pubescentis reference medicine, adding 5mL of methanol, carrying out ultrasonic treatment for 15 minutes, filtering, and taking filtrate as radix angelicae pubescentis reference medicine solution.
Further, in the step S3, the preparation method of the reference solution is as follows:
taking ligustilide control and notopterygium alcohol control, and respectively adding methanol to obtain solutions containing 1mg and 0.3mg per 1mL, and taking as control solution.
Further, in the step S4, the sample application amount of the sample solution is 3 to 5 μl, and the sample application mode is dot sample application or tape sample application.
Further, the thin-layer plate in the step S4 is silica gel GF 254 Thin layer plate, HSGF 254 Thin layer plate, merck GF 254 One of the thin layer plates.
Further, the expanding mode in the step S4 is as follows: adopting a double-groove unfolding cylinder to unfold, slowly adding the unfolding agent into the two sides, putting filter paper into one side to be attached to the cylinder wall, putting a thin layer plate with good points into the other side, and sealing by a cover, wherein the unfolding time is 30 minutes.
Further, the color reagent in the step S4 is 10% sulfuric acid ethanol solution, and the preparation method is as follows:
and (3) slowly injecting 5.7mL of sulfuric acid into a proper amount of absolute ethyl alcohol, cooling to room temperature, diluting to 100mL by using the absolute ethyl alcohol, and shaking uniformly to obtain the product.
Further, in the step S4, the inspection wavelength is 254nm when identifying the angelica and the ligusticum wallichii; the inspection wavelength for distinguishing Notopterygii rhizoma and radix Angelicae Pubescentis is 365nm.
Compared with the prior art, the thin layer chromatography for simultaneously identifying the notopterygium root, the radix angelicae pubescentis, the angelica sinensis and the ligusticum wallichii in the Jubi decoction has the following advantages:
(1) In the thin-layer chromatography for simultaneously identifying notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii in Juanbi decoction, the sample spot separation degree is good, the method is negative and has no interference, four medicinal flavors of notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii can be identified specifically, and the durability of the thin-layer chromatography is examined in a test example, so that the detection process of the thin-layer chromatography identification method is not easily influenced by the change of external conditions such as a thin-layer plate, temperature and humidity, and the method is proved to be not harsh to the external conditions, and has good durability and wide applicability.
(2) The thin-layer chromatography for simultaneously identifying the notopterygium root, the radix angelicae pubescentis, the angelica sinensis and the ligusticum wallichii in the Juanbi decoction provided by the invention can simultaneously identify four medicinal herbs of the notopterygium root, the radix angelicae pubescentis, the angelica sinensis and the ligusticum wallichii in the Juanbi decoction by adopting only one thin-layer system, is simple and quick to operate, greatly improves the detection efficiency, and is convenient for efficiently controlling the quality of products of the Juanbi decoction.
Drawings
In the attached figures 1-21, A is a thin layer chromatogram at 254nm of an ultraviolet lamp, and B is a thin layer chromatogram at 365nm of the ultraviolet lamp.
FIG. 1 is a thin layer chromatogram of the test performed on 1 to 8 batches of the test substance solution prepared in example 2 in example 6; wherein, 1: ligustilide control solution, 2: notopterygol control solution, 3: radix angelicae pubescentis control medicinal material solution, 4: test solution (JB 211108-1), 5: test solution (JB 211108-2) 6: test solution (JB 211108-3), 7: test solution (JB 211109-4), 8: test solution (JB 211109-5), 9: test solution (JB 211109-6), 10: test solution (JB 211111-7), 11: test solution (JB 211111-8);
FIG. 2 is a thin layer chromatogram of the test performed on 9 to 15 batches of the test solution prepared in example 2 in example 6; wherein 1: ligustilide control solution, 2: notopterygol control solution, 3: radix angelicae pubescentis control medicinal material solution, 4: test solution (JB 211111-9), 5: test solution (JB 211125-10), 6: test solution (JB 211125-11), 7: test solution (JB 211125-12), 8: test solution (JB 211115-13), 9: test solution (JB 211115-14), 10: test solution (JB 211115-15);
FIG. 3 is a thin layer chromatogram examined by test example one test sample solution preparation method, wherein 1: ligustilide control solution, 2: negative solution of angelica and ligusticum wallichii, 3: notopterygol control solution, 4: negative solution of notopterygium root, 5: radix angelicae pubescentis control medicinal material solution, 6: negative solution of radix Angelicae Pubescentis, 7: sample solution, 8 of example 2: the test solution of comparative example 1;
FIG. 4 is a thin layer chromatogram of a test example two spotting volume study, wherein 1: ligustilide control solution, 2: negative solution of angelica and ligusticum wallichii, 3: notopterygol control solution, 4: negative solution of notopterygium root, 5: radix angelicae pubescentis control medicinal material solution, 6: negative solution of radix angelicae pubescentis, 7-11: 1. Mu.L, 3. Mu.L, 5. Mu.L, 7. Mu.L and 10. Mu.L of test solution;
fig. 5 is a thin layer chromatogram examined in a test example three spotting mode, wherein 1: ligustilide control solution, 2: negative solution of angelica and ligusticum wallichii, 3: notopterygol control solution, 4: negative solution of notopterygium root, 5: radix angelicae pubescentis control medicinal material solution, 6: negative solution of radix angelicae pubescentis, 7-11: sample solutions (spot, 2mm, 4mm, 6mm, 8mm, 10 mm);
fig. 6 to 8 are thin layer chromatograms of test example four development systems 1, 2, 3, respectively, wherein 1: ligustilide control solution, 2: negative solution of angelica and ligusticum wallichii, 3: notopterygol control solution, 4: negative solution of notopterygium root, 5: radix angelicae pubescentis control medicinal material solution, 6: negative solution of radix Angelicae Pubescentis, 7: a test solution;
fig. 9 to 11 are thin layer chromatograms of test examples five heated for 1, 2, and 5min, respectively, wherein 1: ligustilide control solution, 2: negative solution of angelica and ligusticum wallichii, 3: notopterygol control solution, 4: negative solution of notopterygium root, 5: radix angelicae pubescentis control medicinal material solution, 6: negative solution of radix Angelicae Pubescentis, 7: a test solution;
FIGS. 12 to 14 show Qingdao ocean GF in test example six 254 Board, silver dragon HSGF 254 Plates, merck GF 254 Plate thin layer chromatogram, wherein 1: ligustilide control solution, 2: negative solution of angelica and ligusticum wallichii, 3: notopterygol control solution, 4: negative solution of notopterygium root, 5: radix angelicae pubescentis control medicinal material solution, 6: negative solution of radix Angelicae Pubescentis, 7: a test solution;
FIGS. 15 to 17 are respectively thin layer chromatograms of test example seven at low temperature 4 ℃, normal temperature 24 ℃ and high temperature 40 ℃; wherein 1: ligustilide control solution, 2: negative solution of angelica and ligusticum wallichii, 3: notopterygol control solution, 4: negative solution of notopterygium root, 5: radix angelicae pubescentis control medicinal material solution, 6: negative solution of radix Angelicae Pubescentis, 7: a test solution;
fig. 18 to 20 are thin layer chromatograms of test example eight in relative humidity of 25%, 50%, 75%, respectively, wherein 1: ligustilide control solution, 2: negative solution of angelica and ligusticum wallichii, 3: notopterygol control solution, 4: negative solution of notopterygium root, 5: radix angelicae pubescentis control medicinal material solution, 6: negative solution of radix Angelicae Pubescentis, 7: a test solution;
fig. 21 is a thin layer chromatogram of a test example nine specificity study, wherein 1: ligustilide control solution, 2: negative solution of angelica and ligusticum wallichii, 3: notopterygol control solution, 4: negative solution of notopterygium root, 5: radix angelicae pubescentis control medicinal material solution, 6: negative solution of radix Angelicae Pubescentis, 7: test solution.
Note that: in the A diagrams in fig. 3-21, the black and white pictures can not be displayed, the ligustilide spots are dark blue, and the band 2 angelica sinensis and ligusticum chuanxiong negative solution displays black spots at the upper part of the corresponding position of the ligustilide, so that the angelica sinensis and ligusticum chuanxiong negative solution has no interference to detection.
Detailed Description
The invention is further illustrated by the following description of specific embodiments, which are not intended to be limiting, and various modifications or improvements can be made by those skilled in the art in light of the basic idea of the invention, but are within the scope of the invention as long as they do not depart from the basic idea of the invention.
In the following examples and comparative examples, the reagents not specifically described were conventional reagents, and were purchased from conventional reagent manufacturers and sales companies, and the information of some raw material manufacturers and the like was as follows:
the invention adopts the following instruments and reagents:
1. instrument: a kama (CAMAG) semi-automatic thin-layer spotting and imaging system; analytical balance, model BT25S; numerical control ultrasonic cleaner, model KQ-500DE, power 500W, frequency 40kHz, kunshan ultrasonic instruments Inc.; EYELA rotary evaporator model N-1100, shanghai Ironman instruments Co., ltd; a low-speed high-capacity multi-tube centrifuge, model LXJ-IIB, which is used by Shanghai Anting scientific instruments factory; temperature-regulating electrothermal sleeve, model DZTW, yongguangming medical instruments Co., ltd.
2. Thin layer plate: detailed in the following table
3. Reagent: methanol, chromatographic purity, lot 213476, fisher; ethyl acetate, analytically pure, lot 20211012; absolute ethanol, analytically pure, lot number 20220113; petroleum ether (60-90 ℃), analytically pure, lot number 20210202; n-hexane, analytically pure, lot 20210524; cyclohexane, analytically pure, lot 20210825; dichloromethane, analytically pure, lot number 20210714, all purchased from the general fine chemical company of beijing; sulfuric acid, analytically pure, lot number 20201105, available from modern eastern (Beijing) technology development Co., ltd; formic acid, analytically pure, lot a2106152, aladine.
Control: notopterygium alcohol, batch No. 111820-201705, purity 99.9%; ligustilide, lot 111737-201608, was purchased from China food and drug testing institute.
Control medicinal materials: radix Angelicae Pubescentis, lot number 120940-201612, purchased from China food and drug inspection institute.
Medicinal taste: notopterygii rhizoma, radix Angelicae Pubescentis, cortex Cinnamomi, radix Gentianae Marcrophyllae, radix Angelicae sinensis, rhizoma Ligustici Chuanxiong, glycyrrhrizae radix, caulis Piperis Kadsurae, ramulus Mori, olibanum, and radix aucklandiae all are purchased from autonomous or district. The identification shows that the notopterygium root is the dry root and stem of the Umbelliferae plant notopterygium root Notopterygium incisum Ting exH.T.Chang; radix Angelicae Pubescentis is dry root of Angelica acutiloba Anglica pubescens Maxim.f. bisearata Shan et Yuan of Umbelliferae; the cortex Cinnamomi is dried bark of Cinnamomum cassia Cinnamomum cassia Presl belonging to Lauraceae; the radix Gentianae Marcrophyllae is dry root of Gentiana Marcrophyllae Gentiana macrophylla pall. Angelica sinensis is the dry root of Angelica sinensis Angelica sinensis (Oliv.) Diels of Umbelliferae; rhizoma Ligustici Chuanxiong is dried rhizome of Ligusticum chuanxiong Hort Ligusticum chuanxiong Hort of Umbelliferae; glycyrrhrizae radix is dry root and rhizome of Glycyrrhrizae radix Glycyrrhiza uralensis Fisch of Leguminosae; the caulis Piperis Kadsura (Choisy) Ohwi is dried stem of Piperaceae plant caulis Piperis Kadsura; ramulus Mori is dry tender branch of Morus alba L of Moraceae; the Olibanum is resin exuded from bark of Boswellia carterii birdw of Rutaceae plant; the radix aucklandiae is dry root of Aucklandia lappa Decne. The 11 medicinal materials are qualified according to the inspection of Chinese pharmacopoeia of 2020 edition. The decoction pieces of notopterygium root, radix angelicae pubescentis, cinnamon, gentiana macrophylla, angelica sinensis, ligusticum wallichii, liquorice, kadsura pepper stem, mulberry twig, frankincense and costustoot are prepared according to the Chinese pharmacopoeia of 2020 edition; the frankincense decoction pieces are prepared by referring to 2019 edition of Anhui province Chinese medicine decoction piece processing Specification.
Example 1 preparation method of Juanbi decoction reference sample
The preparation method of the reference sample of the Juanbi decoction comprises the following steps:
taking eleven decoction pieces of 3.73g of notopterygium root, 3.73g of radix angelicae pubescentis, 1.87g of cinnamon, 3.73g of gentiana macrophylla, 11.19g of angelica sinensis, 2.61g of ligusticum wallichii, 1.87g of honey-fried licorice root, 7.46g of kadsura pepper stem, 11.19g of mulberry twig, 2.98g of frankincense and 2.98g of costustoot, adding 400mL of water, soaking for 30 minutes, boiling with strong fire, boiling with slow fire, filtering with a 350-mesh screen while hot, and freeze-drying the filtrate to obtain a reference sample of the Juanbi decoction.
The total preparation of 16 batches of Juanbi Shang Jizhun products: batch numbers JB211108-1, JB211108-2, JB211108-3, JB211109-4, JB211109-5, JB211109-6, JB211111-7, JB211111-8, JB211111-9, JB211125-10, JB211125-11, JB211125-12, JB211115-13, JB211115-14, JB211115-15, JB211011.
Example 2 preparation of sample solution
The preparation method of the sample solution comprises the following steps: respectively taking 2g of the reference Jubi soup samples of different batches prepared in the example 1, adding 25mL of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, dissolving residues in 20mL of water, adding petroleum ether (60-90 ℃) for shaking and extracting for 2 times, 20mL each time, combining petroleum ether solutions, evaporating to dryness, and dissolving residues in 2mL of ethyl acetate to prepare 16 batches of test sample solutions.
Example 3 preparation of control drug solution
Taking 0.2g of radix angelicae pubescentis reference medicine, adding 5mL of methanol, carrying out ultrasonic treatment for 15 minutes, filtering, and taking filtrate as radix angelicae pubescentis reference medicine solution.
EXAMPLE 4 preparation of negative solution
Taking the medicinal herbs of the Juanbi decoction, wherein the medicinal herbs do not comprise notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii, and preparing notopterygium root negative solution, radix angelicae pubescentis negative solution, angelica sinensis and ligusticum wallichii negative solution according to the preparation method of the embodiment 1.
EXAMPLE 5 preparation of control solution
Taking ligustilide control and notopterygium alcohol control, and respectively adding methanol to obtain solutions containing 1mg and 0.3mg per 1mL, and taking as control solution.
EXAMPLE 6 thin layer chromatography detection
According to the thin layer chromatography (China Pharmacopeia, general rule 0502) test, the sample solution of 15 batches (JB 211108-1, JB211108-2, JB211108-3, JB211109-4, JB211109-5, JB211109-6, JB211111-7, JB211111-8, JB211111-9, JB211125-10, JB211125-11, JB211125-12, JB211115-13, JB211115-14, JB 211115-15) prepared in example 2, the control medicinal material solution prepared in example 3 and the control solution prepared in example 5 are respectively 2. Mu.L, and are respectively applied to the same silica gel GF 254 On the thin layer plate, cyclohexane-dichloromethane-ethyl acetate-formic acid (5:1:2:0.2) is used as a developing agent for developing, and the developing mode is as follows: adopting a double-groove unfolding cylinder to unfold, slowly adding the unfolding agent into the two sides, putting filter paper into one side to be attached to the cylinder wall, putting a thin layer plate with good points into the other side, and sealing by a cover, wherein the unfolding time is 30 minutes. Taking out, air drying, and inspecting under ultraviolet lamp (254 nm). In the chromatogram of the sample, spots with the same color appear at the positions corresponding to the chromatogram of the ligustilide control; spraying color-developing agent (5.7 mL sulfuric acid, slowly injecting into proper amount of absolute ethanol, cooling to room temperature, diluting with absolute ethanol to 100mL, shaking, and getting the final product), heating at 105deg.C until the color of spots is clear, placing under ultraviolet lamp (365 nm), and inspecting to obtain fluorescent spots of the same color on the positions corresponding to radix Angelicae Pubescentis control medicine chromatogram and Notopterygii rhizoma alcohol control chromatogram in the sample chromatogram.
The detection results are shown in figures 1-2. The results show that spots with the same color appear on the positions corresponding to the control chromatogram and the control chromatogram in the sample chromatogram. The method has good durability, and can be used for specifically identifying Notopterygii rhizoma, radix Angelicae Pubescentis, radix Angelicae sinensis, and rhizoma Ligustici Chuanxiong in Juanbi decoction reference sample.
Comparative example 1 preparation of test solution
2g of the Juanbi decoction reference sample (JB 211011) prepared in example 1 is taken, 20mL of water is added for dissolution, petroleum ether (60-90 ℃) is added for shaking extraction for 2 times, 20mL of petroleum ether liquid is combined each time, the mixture is evaporated to dryness, and 2mL of ethyl acetate is added for dissolution of residues to serve as a test solution.
Examination of test example one, test article solution preparation method
The control solution of example 5 and the control solution of example 3 were each aspirated at 2. Mu.L, and the negative solution of example 4, the sample solution of example 2 (JB 211011) and comparative example 1 were each aspirated at 3. Mu.L, respectively, on the same silica gel GF 254 Performing thin layer chromatography detection on the thin layer plate, using cyclohexane-dichloromethane-ethyl acetate-formic acid (5:1:2:0.2) as developing agent, developing, taking out, air drying, and inspecting under ultraviolet lamp (254 nm) to identify radix Angelicae sinensis and rhizoma Ligustici Chuanxiong; spraying 10% sulfuric acid ethanol solution, heating at 105deg.C until the spots appear clearly, and inspecting under ultraviolet lamp (365 nm) to identify Notopterygii rhizoma and radix Angelicae Pubescentis.
The detection result is shown in FIG. 3. The results showed that, although spots of the same color were developed at the positions corresponding to the control chromatogram and the control chromatogram in example 2 and comparative example 1, the sample solution prepared in comparative example 1 was severely emulsified during the preparation.
Investigation of test example two, sample application amount
The control solution of example 5 and the control solution of example 3 were each aspirated at 2. Mu.L, the negative solution of example 4 at 3. Mu.L, the test solution of example 2 (JB 211011) at 1. Mu.L, 3. Mu.L, 5. Mu.L, 7. Mu.L, 10. Mu.L, and spotted on the same silica gel GF, respectively 254 Spreading on the thin layer plate with cyclohexane-dichloromethane-ethyl acetate-formic acid (5:1:2:0.2) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp (254 nm) to identify radix Angelicae sinensis and rhizoma Ligustici Chuanxiong; spraying 10% sulfuric acid ethanol solution, heating to 105deg.CThe spots are clearly developed, and are inspected under an ultraviolet lamp (365 nm) to identify the notopterygium root and the radix angelicae pubescentis. The results are shown in FIG. 4.
The result shows that when the sample application amount of the sample solution is 3-5 mu L, the spot color of the sample chromatogram at the corresponding position of the control medicine chromatogram and the control medicine chromatogram is clearer and more moderate, so the sample application amount of the sample solution is 3-5 mu L.
Examination of test example III, sample application mode
(1) Spotting in a dot shape: the control solution of example 5 and the control solution of example 3 were each aspirated at 2. Mu.L, the negative solution of example 4 and the sample solution of example 2 (JB 211011) at 3. Mu.L, and spotted on the same silica gel GF 254 Spreading on the thin layer plate with cyclohexane-dichloromethane-ethyl acetate-formic acid (5:1:2:0.2) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp (254 nm) to identify radix Angelicae sinensis and rhizoma Ligustici Chuanxiong; spraying 10% sulfuric acid ethanol solution, heating at 105deg.C until the spots appear clearly, and inspecting under ultraviolet lamp (365 nm) to identify Notopterygii rhizoma and radix Angelicae Pubescentis.
(2) Tape spotting: the control solution of example 5 and the control solution of example 3 were each aspirated at 2. Mu.L, the negative solution of example 4 and the sample solution of example 2 (JB 211011) at 3. Mu.L, and spotted on the same silica gel GF 254 The sample application strips of the sample solution are respectively 2mm, 4mm, 6mm, 8mm and 10mm in width on the thin layer plate, cyclohexane-dichloromethane-ethyl acetate-formic acid (5:1:2:0.2) are used as developing agents, and are developed, taken out, dried and inspected under an ultraviolet lamp (254 nm) to identify the angelica and the ligusticum wallichii; spraying 10% sulfuric acid ethanol solution, heating at 105deg.C until the spots appear clearly, and inspecting under ultraviolet lamp (365 nm) to identify Notopterygii rhizoma and radix Angelicae Pubescentis. The results are shown in FIG. 5.
The results show that the sample application mode has little influence on thin layer identification of angelica sinensis, ligusticum wallichii, notopterygium root and radix angelicae pubescentis, and the invention selects 8mm as the strip width for subsequent research.
Examination of test example IV, deployment System
The influence of 3 different unfolding systems on thin-layer identification of angelica sinensis, ligusticum wallichii, notopterygium root and radix angelicae pubescentis is examined. Aspiration of control solution from example 5 and implementationThe control medicinal material solution of example 3 was 2. Mu.L each, the negative solution of example 4 and the sample solution of example 2 (JB 211011) were each 3. Mu.L each, spotted on the same silica gel GF 254 On the thin layer plate, three unfolding systems are used as unfolding agents respectively, and the thin layer plate is unfolded, taken out, dried, inspected under an ultraviolet lamp (254 nm) and identified to be angelica sinensis and ligusticum wallichii; spraying 10% sulfuric acid ethanol solution, heating at 105deg.C until the spots appear clearly, and inspecting under ultraviolet lamp (365 nm) to identify Notopterygii rhizoma and radix Angelicae Pubescentis.
The three unfolding systems are respectively as follows:
developing agent 1: cyclohexane-dichloromethane-ethyl acetate-formic acid (5:1:2:0.2)
Developing agent 2: n-hexane-ethyl acetate-formic acid (6:2:0.2)
Developing agent 3: petroleum ether (60-90 ℃ C.) ethyl acetate-formic acid (6:2:0.2)
The results are shown in FIGS. 6 to 8. The results show that when the developing system is cyclohexane-dichloromethane-ethyl acetate-formic acid (5:1:2:0.2), the spots of the test sample are clearer, the specific shift value is moderate, and the developing system is negative and has no interference, so that the developing system adopted by the invention can better identify the specificity of the angelica sinensis, the ligusticum wallichii, the notopterygium root and the radix angelicae pubescentis in the product.
Examination of test example five, heating time
The influence of different heating time on thin-layer identification of notopterygium root, radix angelicae pubescentis, chinese angelica and ligusticum wallichii is examined.
The control solution of example 5 and the control solution of example 3 were each aspirated at 2. Mu.L, the negative solution of example 4 and the sample solution of example 2 (JB 211011) at 3. Mu.L, and spotted on the same silica gel GF 254 Spreading on the thin layer plate with cyclohexane-dichloromethane-ethyl acetate-formic acid (5:1:2:0.2) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp (254 nm) to identify radix Angelicae sinensis and rhizoma Ligustici Chuanxiong; spraying 10% sulfuric acid ethanol solution, heating at 105deg.C for 1min, 2min, and 5min, and inspecting with ultraviolet lamp (365 nm) to identify Notopterygii rhizoma and radix Angelicae Pubescentis. The results are shown in FIGS. 9 to 11.
The result shows that when the heating time exceeds 2min, the spots of the test sample are clear, the negative is free from interference, and the special identification of the notopterygium root and the radix angelicae pubescentis in the product can be realized.
Test example six, investigation of lamina plate
Respectively inspect German Merck GF 254 Thin layer plate, qingdao ocean GF 254 Thin layer plate, smoke table silver dragon HSGF 254 A thin layer plate.
The control solution of example 5 and the control solution of example 3 were each aspirated at 2. Mu.L, the negative solution of example 4 and the test solution of example 2 (JB 211011) at 3. Mu.L, respectively, and spotted on Merck GF in Germany 254 Thin layer plate, qingdao ocean GF 254 Lepium Okavalae HSGF 254 Spreading on the thin layer plate with cyclohexane-dichloromethane-ethyl acetate-formic acid (5:1:2:0.2) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp (254 nm) to identify radix Angelicae sinensis and rhizoma Ligustici Chuanxiong; spraying 10% sulfuric acid ethanol solution, heating at 105deg.C until the spots appear clearly, and inspecting under ultraviolet lamp (365 nm) to identify Notopterygii rhizoma and radix Angelicae Pubescentis. The results are shown in FIGS. 12 to 14.
The results show that the 3 brands of thin-layer plates can be used for carrying out exclusive identification on the notopterygium root, the radix angelicae pubescentis, the angelica sinensis and the ligusticum wallichii in the product, and the invention has good durability and wide applicability. The invention selects Merck GF for subsequent research 254 A thin layer plate.
Test example seven, investigation of temperature
The control solution of example 5 and the control solution of example 3 were each aspirated at 2. Mu.L, the negative solution of example 4 and the sample solution of example 2 (JB 211011) at 3. Mu.L, and spotted on the same silica gel GF 254 Spreading on the thin layer plate with cyclohexane-dichloromethane-ethyl acetate-formic acid (5:1:2:0.2) as developing agent under different temperature environments (low temperature 4 deg.C, normal temperature 24 deg.C, high temperature 40 deg.C), taking out, air drying, and inspecting under ultraviolet lamp (254 nm) to identify radix Angelicae sinensis and rhizoma Ligustici Chuanxiong; spraying 10% sulfuric acid ethanol solution, heating at 105deg.C until the spots appear clearly, and inspecting under ultraviolet lamp (365 nm) to identify Notopterygii rhizoma and radix Angelicae Pubescentis. The results are shown in FIGS. 15 to 17.
The results show that the spot inspection effects of the chromatograms of the test samples at different temperatures are not greatly different. The thin-layer chromatography identification method provided by the invention has the advantages of less influence of temperature change and good durability.
Test example eight, investigation of relative humidity
The control solution of example 5 and the control solution of example 3 were each aspirated at 2. Mu.L, the negative solution of example 4 and the sample solution of example 2 (JB 211011) at 3. Mu.L, and spotted on the same silica gel GF 254 Spreading on the thin layer plate with cyclohexane-dichloromethane-ethyl acetate-formic acid (5:1:2:0.2) as developing agent under different relative humidity environments (relative humidity 25%, relative humidity 50%, and relative humidity 75%), taking out, air drying, and inspecting under ultraviolet lamp (254 nm) to identify radix Angelicae sinensis and rhizoma Ligustici Chuanxiong; spraying 10% sulfuric acid ethanol solution, heating at 105deg.C until the spots appear clearly, and inspecting under ultraviolet lamp (365 nm) to identify Notopterygii rhizoma and radix Angelicae Pubescentis. The results are shown in FIGS. 18 to 20.
The results show that the spot inspection effects of the sample chromatograms at different relative humidities are not greatly different. The thin-layer chromatography identification method provided by the invention has small influence by humidity change and good durability.
Investigation of specificity of test example nine
The control solution of example 5 and the control solution of example 3 were each aspirated at 2. Mu.L, the negative solution of example 4 and the sample solution of example 2 (JB 211011) at 3. Mu.L, and spotted on the same silica gel GF 254 Spreading on the thin layer plate with cyclohexane-dichloromethane-ethyl acetate-formic acid (5:1:2:0.2) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp (254 nm) to identify radix Angelicae sinensis and rhizoma Ligustici Chuanxiong; spraying 10% sulfuric acid ethanol solution, heating at 105deg.C until the spots appear clearly, and inspecting under ultraviolet lamp (365 nm) to identify Notopterygii rhizoma and radix Angelicae Pubescentis. The results are shown in FIG. 21.
The result shows that the fluorescence spots with the same color appear on the positions corresponding to the chromatogram of the control substance and the chromatogram of the control medicinal material in the chromatogram of the test substance. The thin-layer chromatography detection method provided by the invention has better durability, and can be used for carrying out specific identification on notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii in a reference sample of Juanbi decoction.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (7)
1. A thin layer chromatography method for simultaneously identifying notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii in Juanbi decoction is characterized by comprising the following steps:
s1, preparing a sample solution: adding methanol into the Juanbi decoction sample for ultrasonic treatment, filtering, evaporating filtrate to dryness, adding water into residue, extracting with petroleum ether, mixing petroleum ether solutions, evaporating to dryness, and dissolving residue with ethyl acetate to obtain sample solution;
s2, preparing a control medicinal material solution: extracting radix Angelicae Pubescentis with methanol, performing ultrasonic treatment, filtering, and collecting filtrate as radix Angelicae Pubescentis control solution;
s3, preparing a reference substance solution: taking ligustilide reference substance and notopterygium alcohol reference substance, and respectively adding methanol to prepare reference substance solutions;
s4, thin-layer chromatography analysis: sucking the sample solution, the control medicinal material solution and the control solution, respectively spotting on the same thin layer plate, spreading with spreading agent, taking out, air drying, inspecting under ultraviolet lamp, and identifying radix Angelicae sinensis and rhizoma Ligustici Chuanxiong; spraying color-developing agent, heating until the spots develop clearly, and inspecting under ultraviolet lamp to identify Notopterygii rhizoma and radix Angelicae Pubescentis;
the developing agent in the step S4 is cyclohexane, methylene dichloride, ethyl acetate and formic acid according to the volume ratio of 5:1:2: 0.2;
the thin-layer plate in the step S4 is silica gel GF 254 A thin layer plate;
the color reagent in the step S4 is 10% sulfuric acid ethanol solution, and the preparation method is as follows: taking 5.7mL of sulfuric acid, injecting a proper amount of absolute ethyl alcohol, cooling to room temperature, diluting to 100mL by using absolute ethyl alcohol, and shaking uniformly to obtain the product;
in the step S4, after being sprayed with the color developing agent, the color developing agent is heated for 2 to 5 minutes at the temperature of 105 ℃ and then is inspected;
in the step S4, the inspection wavelength is 254nm when identifying the angelica and the ligusticum wallichii; the inspection wavelength for distinguishing Notopterygii rhizoma and radix Angelicae Pubescentis is 365nm.
2. The thin layer chromatography for simultaneously identifying notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii in the Juanbi decoction according to claim 1, wherein the preparation method of the Juanbi decoction sample in the step S1 is as follows:
taking eleven decoction pieces of 3.73g of notopterygium root, 3.73g of radix angelicae pubescentis, 1.87g of cinnamon, 3.73g of gentiana macrophylla, 11.19g of angelica sinensis, 2.61g of ligusticum wallichii, 1.87g of honey-fried licorice root, 7.46g of kadsura pepper stem, 11.19g of mulberry twig, 2.98g of frankincense and 2.98g of costustoot, adding 400mL of water, soaking for 30 minutes, boiling with strong fire, boiling with slow fire, filtering with a 350-mesh screen while hot, and freeze-drying the filtrate to obtain a pain relieving soup sample.
3. The thin layer chromatography for simultaneously identifying notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii in Juanbi decoction according to claim 1, wherein the preparation method of the sample solution in the step S1 is as follows: taking Shang Yangpin g of a arthralgia relieving agent, adding 25mL of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, dissolving residues in 20mL of water, adding petroleum ether, shaking and extracting for 2 times, 20mL each time, combining petroleum ether solutions, evaporating to dryness, and dissolving residues in 2mL of ethyl acetate to obtain a sample solution; the boiling range of the petroleum ether is 60-90 ℃.
4. The thin layer chromatography for simultaneously identifying notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii in Juanbi decoction according to claim 1, wherein the preparation method of the reference medicinal material solution in the step S2 is as follows:
taking 0.2g of radix angelicae pubescentis reference medicine, adding 5mL of methanol, carrying out ultrasonic treatment for 15 minutes, filtering, and taking filtrate as radix angelicae pubescentis reference medicine solution.
5. The thin layer chromatography for simultaneously identifying notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii in Juanbi decoction according to claim 1, wherein in the step S3, the preparation method of the reference substance solution is as follows:
taking ligustilide control and notopterygium alcohol control, and respectively adding methanol to obtain solutions containing 1mg and 0.3mg per 1mL, and taking as control solution.
6. The thin layer chromatography for simultaneously identifying notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii in Juanbi decoction according to claim 1, wherein in the step S4, the sample application amount of the sample solution is 3-5 μl, and the sample application mode is point-like sample application or strip-like sample application.
7. The thin layer chromatography for simultaneously identifying notopterygium root, radix angelicae pubescentis, angelica sinensis and ligusticum wallichii in Juanbi decoction according to claim 1, wherein the developing mode in the step S4 is as follows: adopting a double-groove unfolding cylinder for unfolding, adding an unfolding agent on two sides, putting filter paper on one side for being attached to the cylinder wall, putting a thin layer plate on the other side for being well pointed, and sealing by a cover for 30 minutes.
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