CN115166128A - Method for identifying Scutellaria Yunnanensis and Scutellaria baicalensis - Google Patents
Method for identifying Scutellaria Yunnanensis and Scutellaria baicalensis Download PDFInfo
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- IKIIZLYTISPENI-ZFORQUDYSA-N baicalin Chemical compound O1[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IKIIZLYTISPENI-ZFORQUDYSA-N 0.000 claims abstract description 57
- 229960003321 baicalin Drugs 0.000 claims abstract description 57
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- LNOHXHDWGCMVCO-NTKSAMNMSA-N wogonin 7-O-beta-D-glucuronide Chemical compound C1=C(O)C(C(C=C(O2)C=3C=CC=CC=3)=O)=C2C(OC)=C1O[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LNOHXHDWGCMVCO-NTKSAMNMSA-N 0.000 claims abstract description 49
- 238000004809 thin layer chromatography Methods 0.000 claims abstract description 18
- 238000004811 liquid chromatography Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 84
- 239000000463 material Substances 0.000 claims description 78
- 239000000243 solution Substances 0.000 claims description 58
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 34
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- 238000001816 cooling Methods 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 18
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 17
- 235000019253 formic acid Nutrition 0.000 claims description 17
- 238000005303 weighing Methods 0.000 claims description 17
- 241000006814 Scutellaria amoena Species 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 11
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- 238000004128 high performance liquid chromatography Methods 0.000 claims description 6
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- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 6
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- 238000009738 saturating Methods 0.000 claims description 6
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- 241000207929 Scutellaria Species 0.000 claims description 5
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- 238000002360 preparation method Methods 0.000 claims description 5
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- 238000001704 evaporation Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 3
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- 239000003814 drug Substances 0.000 abstract description 6
- 229940079593 drug Drugs 0.000 abstract description 4
- 241000196324 Embryophyta Species 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 241000202726 Bupleurum Species 0.000 description 2
- 206010011224 Cough Diseases 0.000 description 2
- 206010012735 Diarrhoea Diseases 0.000 description 2
- 206010023126 Jaundice Diseases 0.000 description 2
- 241000207923 Lamiaceae Species 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 210000004072 lung Anatomy 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 206010036067 polydipsia Diseases 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 206010000242 Abortion threatened Diseases 0.000 description 1
- FXNFHKRTJBSTCS-UHFFFAOYSA-N Baicalein Natural products C=1C(=O)C=2C(O)=C(O)C(O)=CC=2OC=1C1=CC=CC=C1 FXNFHKRTJBSTCS-UHFFFAOYSA-N 0.000 description 1
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- 208000005985 Threatened Abortion Diseases 0.000 description 1
- HIMJIPRMECETLJ-UHFFFAOYSA-N Wogonin Natural products COc1cc(O)c(O)c2C(=O)C=C(Oc12)c3ccccc3 HIMJIPRMECETLJ-UHFFFAOYSA-N 0.000 description 1
- 206010000210 abortion Diseases 0.000 description 1
- 231100000176 abortion Toxicity 0.000 description 1
- UDFLTIRFTXWNJO-UHFFFAOYSA-N baicalein Chemical compound O1C2=CC(=O)C(O)=C(O)C2=C(O)C=C1C1=CC=CC=C1 UDFLTIRFTXWNJO-UHFFFAOYSA-N 0.000 description 1
- 229940015301 baicalein Drugs 0.000 description 1
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- 239000012567 medical material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
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- 239000003053 toxin Substances 0.000 description 1
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- XLTFNNCXVBYBSX-UHFFFAOYSA-N wogonin Chemical compound COC1=C(O)C=C(O)C(C(C=2)=O)=C1OC=2C1=CC=CC=C1 XLTFNNCXVBYBSX-UHFFFAOYSA-N 0.000 description 1
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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
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
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Abstract
The invention provides a method for identifying Yunnan baikal skullcap root and baikal skullcap root, belonging to the field of drug identification, which comprises thin-layer chromatography identification using Yunnan baikal skullcap root as reference drug, and also comprises an identification method for judging the peak area of baicalin and the peak area ratio of wogonoside in the Yunnan baikal skullcap root and baikal skullcap root liquid chromatography.
Description
Technical Field
The invention relates to the field of medicine identification, in particular to an identification method of Scutellaria Yunnanensis and Scutellaria baicalensis.
Background
The Scutellaria baicalensis is collected in one part of the 2020 edition of Chinese pharmacopoeia, is a common traditional Chinese medicinal material, is a perennial herb plant of the Labiatae, has the latin name of Scutellaria baicalensis Georgi, is a dry root of a medicinal herb, has the functions and main functions of clearing heat and drying dampness, purging intense heat and detoxifying, stopping bleeding and preventing abortion, and is used for treating damp warmth, summer heat dampness, chest distress and nausea, damp heat and fullness, diarrhea and dysentery, jaundice, lung heat cough, hyperpyrexia and polydipsia, blood heat and hematemesis and epistaxis, carbuncle and sore toxin and threatened abortion. Scutellaria rigescens is also a perennial herb of Labiatae, latin is Scutellaria amoena C.H.Wright, is a local traditional medicine, is a dry root of a medicinal herb, and has the effects of treating high fever, polydipsia, lung heat cough, damp-heat diarrhea, jaundice, heat stranguria and the like. The two plants have different efficacies, but the appearance traits of the two plants are difficult to distinguish, and the two plants contain baicalein, wogonin, baicalin, wogonoside and other components, so the two plants are also difficult to distinguish in terms of components. Baikal skullcap root is collected in the Chinese pharmacopoeia 2020 edition, but the qualitative identification of the quality standard is incomplete, only simple thin-layer identification by taking a reference substance and a reference medicinal material as a reference is carried out, and the Baikal skullcap root and the Yunnan Baikal skullcap root cannot be substantially distinguished. Scutellaria Yunnanensis has a history of local use in the southwest region, and some drug growers and drug manufacturers do not distinguish or can not distinguish the Scutellaria Yunnanensis from the Scutellaria Yunnanensis, so that a certain degree of confusion phenomenon exists for a long time, which causes low quality controllability and poor specificity of the Scutellaria baicalensis, and the quality of the Scutellaria baicalensis cannot be effectively managed and controlled. In addition, in recent years, the price of the scutellaria baicalensis is increased due to the extremely large dosage of the scutellaria baicalensis, so that the price difference between the scutellaria baicalensis and the scutellaria baicalensis is large, and poor marketability cannot avoid mixing the scutellaria baicalensis with the scutellaria baicalensis or using the scutellaria baicalensis as the scutellaria baicalensis. Because the two are difficult to identify from the appearance and the identification method in the related standard can not completely identify the two, the method for identifying the Scutellaria delavayi and the Scutellaria baicalensis is urgently needed in the field of traditional Chinese medicines at present.
Disclosure of Invention
The invention aims to provide a method for identifying Scutellaria Yunnanensis and Scutellaria baicalensis, which increases thin-layer chromatography identification by using a Scutellaria Yunnanensis contrast medicinal material as a contrast, and also increases an identification method for judging the peak area of baicalin and the peak area ratio of wogonoside in the liquid chromatography of Scutellaria Yunnanensis and Scutellaria baicalensis, and detects Scutellaria Yunnanensis which is a medicinal material easy to be confused, so that the quality of the Scutellaria baicalensis medicinal material can be effectively managed and monitored, the medicinal material is safe and effective, the clinical curative effect of the Scutellaria baicalensis medicinal material is ensured, the benefit of a patient is maintained, and the situation that Scutellaria Yunnanensis is mixed into Scutellaria baicalensis by a poor dealer or the Scutellaria Yunnanensis is used as the Scutellaria baicalensis is avoided.
The technical scheme provided by the invention is as follows:
a method for identifying Scutellaria Yunnanensis and Scutellariae radix comprises thin layer chromatography identification using Scutellaria Yunnanensis contrast medicinal material and Scutellariae radix contrast medicinal material as contrast and identification method using ratio of baicalin peak area and wogonoside peak area in Scutellaria Yunnanensis and Scutellariae radix liquid chromatography.
The thin-layer chromatography identification method using Scutellaria Yunnanensis contrast medicinal material and Scutellaria baicalensis contrast medicinal material as contrast comprises: taking Scutellaria Yunnanensis contrast medicinal material and Scutellaria baicalensis contrast medicinal material as contrast, adopting thin layer chromatography, taking ethyl acetate, ethanol and formic acid = 4: 1: 1.5 as developing agent, and in the chromatogram of the test solution, at the position corresponding to the chromatogram of the Scutellaria Yunnanensis contrast medicinal material, if all the spots with the same color are displayed, then the Scutellaria Yunnanensis is taken; and if spots with the same color are all displayed on the positions corresponding to the color spectrum of the radix scutellariae reference medicinal material, the radix scutellariae is obtained.
The thin-layer chromatography identification method taking the Scutellaria amoena reference medicinal material and the Scutellaria baicalensis reference medicinal material as the references comprises the steps of taking 20g of a Scutellaria baicalensis sample, 0.8-l.2g of the Scutellaria amoena reference medicinal material and 0.8-l.2g of the Scutellaria baicalensis reference medicinal material, drying for 1-4 hours at 50-70 ℃, cooling, crushing, sieving by a No. 3 sieve, taking 1.5-2.5g of sieved powder, adding 30-50ml of a mixed solution of ethyl acetate and ethanol = 4: 1, carrying out ultrasonic treatment for 40-60 minutes under the conditions of the power of 250W and the frequency of 40kHz, taking out, cooling, filtering, evaporating filtrate to dryness, adding 4-6ml of methanol into residues for dissolving, taking supernate, and preparing a test solution, a Scutellaria amoena baicalensis reference medicinal material solution and a Scutellaria baicalensis reference medicinal material solution; performing thin layer chromatography test, collecting the sample solution, scutellaria amoena reference medicinal material solution and Scutellaria baicalensis reference medicinal material solution 1-3 μ l respectively, dropping on the same polyamide film, pre-saturating with ethyl acetate, ethanol and formic acid = 4: 1: 1.5 as developing agent for 20-40 min, developing, taking out, air drying, and inspecting under 365nm ultraviolet lamp.
The thin-layer chromatography identification method taking the Scutellaria rigescens reference medicinal material and the Scutellaria baicalensis reference medicinal material as the reference comprises the more specific steps of: taking 20g of a scutellaria baicalensis sample, lg of a Yunnan scutellaria baicalensis control medicinal material and lg of a scutellaria baicalensis control medicinal material, respectively placing the scutellaria baicalensis sample, the lg of the Yunnan scutellaria baicalensis control medicinal material and the lg of the scutellaria baicalensis control medicinal material in an electrothermal constant-temperature drying box, drying for 2-3 hours at 60 ℃, cooling, crushing, sieving by a No. 3 sieve, taking 2g of sieved powder, adding 40ml of a mixed solution of ethyl acetate and ethanol = 4: 1, carrying out ultrasonic treatment for 45 minutes under the conditions of power of 250W and frequency of 40kHz, taking out, cooling, filtering, drying filtrate by distillation, dissolving residues by adding 5ml of methanol, taking supernatant liquid, and preparing a test solution, the Yunnan scutellaria baicalensis control medicinal material and the scutellaria baicalensis control medicinal material; performing thin layer chromatography test, collecting the sample solution, scutellaria amoena reference medicinal material solution and Scutellaria baicalensis reference medicinal material solution 2 μ l respectively, dropping on the same polyamide film, pre-saturating with ethyl acetate, ethanol and formic acid = 4: 1: 1.5 as developing agent for 30 min, developing, taking out, air drying, and inspecting under 365nm ultraviolet lamp.
The identification method for judging by the peak area ratio of baicalin to the peak area of wogonoside in liquid chromatogram comprises the following steps: respectively measuring the peak areas of baicalin and wogonoside by high performance liquid chromatography with baicalin and wogonoside as reference substances, acetonitrile as mobile phase A, and 0.3-0.6% formic acid solution as mobile phase B, and gradient eluting, wherein the ratio of the peak area of baicalin to the peak area of wogonoside is less than or equal to 10, and the sample is Scutellariae radix; if the peak area of baicalin is more than 10, the Scutellaria Yunnanensis is obtained.
The identification method for determining the ratio of the baicalin peak area to the wogonoside peak area in the liquid chromatogram further comprises the following steps:
measuring by high performance liquid chromatography.
(1) Octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile is used as a mobile phase A, 0.3-0.6% formic acid solution is used as a mobile phase B, a gradient elution method is adopted, when the elution time is 0-10 minutes, the mobile phase A is 3-10%, the mobile phase B is 90-97%, when the elution time is 11-20 minutes, the mobile phase A is 11-27%, the mobile phase B is 73-89%, when the elution time is 21-55 minutes, the mobile phase A is 28-40%, the mobile phase B is 60-72%, when the elution time is 56-70 minutes, the mobile phase A is 41-92%, and the mobile phase B is 8-59; the column temperature is 25-35 ℃; the detection wavelength is 270mm; the number of theoretical plates is not less than 5000 calculated according to baicalin peak; (2) The reference solution is prepared by collecting baicalin and wogonoside as reference, precisely weighing, and adding methanol to obtain solutions containing 40-60 μ g of baicalin and wogonoside per 1ml as reference solutions; the preparation of the test solution is that 20g of scutellaria baicalensis sample is taken and placed in an electrothermal constant-temperature drying oven to be dried for 1-4 hours at 50-70 ℃, cooled and crushed, and is sieved by a No. 3 sieve, 1.5-2.5g of sieved powder is taken and precisely weighed, 25ml of 50 percent ethanol is precisely added, the mixture is sealed and weighed, the mixture is subjected to ultrasonic treatment for 40-60 minutes under the conditions of 250W of power and 40kHz of frequency, taken out and cooled, the weight is weighed again, the weight loss is compensated by 50 percent ethanol, the mixture is shaken up and filtered, and the subsequent filtrate is taken as the test solution; (3) Precisely sucking 5 μ l of control solution and 10 μ l of test solution, respectively, injecting into liquid chromatograph, measuring, respectively recording the peak areas of baicalin and wogonoside in the control solution, and respectively recording the peak areas of baicalin and wogonoside in the test solution and the control solution.
The identification method for judging the ratio of the baicalin peak area to the wogonoside peak area in the liquid chromatogram comprises the following more specific steps:
measuring by high performance liquid chromatography.
(1) Octadecylsilane chemically bonded silica is used as a filling agent; using acetonitrile as a mobile phase A, using a 0.5% formic acid solution as a mobile phase B, and adopting a gradient elution method, wherein when the elution time is 0-10 minutes, the mobile phase A is 3-10%, the mobile phase B is 90-97%, when the elution time is 11-20 minutes, the mobile phase A is 11-27%, the mobile phase B is 73-89%, when the elution time is 21-55 minutes, the mobile phase A is 28-40%, the mobile phase B is 60-72%, when the elution time is 56-70 minutes, the mobile phase A is 41-92%, and the mobile phase B is 8-59%; the column temperature is 30 ℃; the detection wavelength is 270mm; the number of theoretical plates is not less than 5000 calculated according to baicalin peak; (2) The reference solution is prepared by collecting baicalin and wogonoside as reference, precisely weighing, and adding methanol to obtain solutions containing 50 μ g of baicalin and wogonoside per 1ml as reference solutions; preparing a test solution by taking 20g of a scutellaria baicalensis sample, placing the scutellaria baicalensis sample in an electrothermal constant-temperature drying oven, drying for 2 hours at 60 ℃, cooling, crushing, sieving by a No. 3 sieve, taking 2g of sieved powder, precisely weighing, precisely adding 25ml of 50% ethanol, sealing, weighing, ultrasonically treating for 50 minutes under the conditions of the power of 250W and the frequency of 40kHz, taking out, cooling, weighing again, complementing the weight loss by using 50% ethanol, shaking up, filtering, and taking a subsequent filtrate as the test solution; (3) Precisely sucking 5 μ l of control solution and 10 μ l of test solution, respectively, injecting into liquid chromatograph, measuring, respectively recording the peak areas of baicalin and wogonoside in the control solution, and respectively recording the peak areas of baicalin and wogonoside in the test solution and the control solution.
The ratio of the mobile phase A to the mobile phase B is volume percent.
The ratio of the ethyl acetate to the ethanol to the formic acid is volume ratio.
The ratio of the ethyl acetate to the ethanol is volume ratio.
The invention manages and controls the Scutellaria amoena which is a medical material easy to be confused by adding a thin-layer chromatography identification method taking Scutellaria amoena reference medicinal material as reference and an identification method for judging the ratio of the peak area of baicalin and the peak area of wogonoside in the liquid chromatography of Scutellaria amoena and Scutellaria baicalensis, thereby effectively monitoring the quality of the Scutellaria baicalensis medicinal material, ensuring the safety and effectiveness of the medicinal material, further ensuring the clinical curative effect of using the Scutellaria baicalensis medicinal material and maintaining the benefit of patients. So as to avoid the inconvenience that the poor vendor mixes the Yunnan Baikal skullcap root into the Baikal skullcap root or uses the Yunnan Baikal skullcap root as the Baikal skullcap root.
Drawings
FIG. 1 is a high performance liquid chromatogram obtained in example 1
FIG. 2 is a high performance liquid chromatogram obtained in example 2
Detailed Description
Example 1
(1) Taking 20g of a bupleurum sample with a batch number of 211201, placing the sample in an electrothermal constant-temperature drying oven, drying the sample at 65 ℃ for 2 hours, cooling the sample, crushing the powder, sieving the powder by a No. 3 sieve, taking 2g of the sieved powder, adding 30ml of a mixed solution of ethyl acetate and ethanol = 4: 1, carrying out ultrasonic treatment (power 250W and frequency 40 kHz) for 40 minutes, taking out the powder, cooling the powder, filtering the powder, evaporating the filtrate to dryness, adding 5ml of methanol into residues to dissolve the residues, and taking supernatant as a sample solution; taking 1g of Scutellaria Yunnanensis contrast medicinal material and 1g of Scutellaria baicalensis contrast medicinal material respectively, and preparing Scutellaria Yunnanensis contrast medicinal material solution and Scutellaria baicalensis contrast medicinal material solution in the same way; performing thin layer chromatography test, collecting the sample solution, scutellaria Yunnanensis radix reference medicinal material solution and Scutellaria baicalensis radix reference medicinal material solution 2 μ l each, respectively dropping on the same polyamide film, pre-saturating with ethyl acetate, ethanol and formic acid = 4: 1: 1.5 as developing agent for 30 min, developing, taking out, air drying, and inspecting under ultraviolet lamp (365 nm).
In the chromatogram of the test solution, not all spots with the same color are displayed at the corresponding positions of the chromatogram of the Scutellaria amoena reference medicinal material; and all spots with the same color are displayed at the positions corresponding to the color spectrum of the radix scutellariae reference medicinal material, and the result is judged to be the radix scutellariae.
(2) And (3) measuring according to a high performance liquid chromatography:
the chromatographic condition and the system applicability test take octadecylsilane chemically bonded silica as a filler; acetonitrile is taken as a mobile phase A, 0.5 percent formic acid solution is taken as a mobile phase B, and gradient elution is carried out according to the content in the table 1; the column temperature is 30 ℃; the detection wavelength is 270mm; the number of theoretical plates is not less than 5000 calculated according to baicalin peak.
TABLE 1 time of gradient elution and ratio of mobile phases A and B in example 1
| Time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0～10 | 3～10 | 90～97 |
| 11～20 | 11～27 | 73～89 |
| 21～55 | 28～40 | 60～72 |
| 56～70 | 41～92 | 8～59 |
Preparation of control solutions: taking appropriate amount of baicalin and wogonoside as reference substances, precisely weighing, and adding methanol to obtain solutions containing 40 μ g of baicalin and wogonoside per 1ml as reference substance solutions.
Preparing a test solution: taking 20g of radix bupleuri sample with the batch number of 211201, placing the radix bupleuri sample in an electrothermal constant-temperature drying oven, drying for 2 hours at 55 ℃, cooling, crushing, sieving by a No. 3 sieve, taking 2.5g of sieved powder, precisely weighing, precisely adding 25ml of 50% ethanol, carrying out ultrasonic treatment (power 250W and frequency 40 kHz) for 40 minutes, taking out, cooling, weighing again, complementing the weight loss by 50% ethanol, shaking up, filtering, and taking the subsequent filtrate as a test solution.
The determination method comprises the following steps: precisely sucking 5 μ l of control solution and 10 μ l of test solution, injecting into liquid chromatograph, measuring, recording the peak areas of baicalin and wogonoside in the control solution, and recording the peak areas of baicalin and wogonoside in the test solution and the control solution, respectively, with the results as shown in Table 2:
TABLE 2 area of peak of test solution and peak of control solution in example 1
| Peak area of baicalin | Peak area of wogonoside | The peak area of baicalin is the peak area of wogonoside |
| 1145077 | 236045 | 4.85 |
The high performance liquid chromatogram obtained in example 1 has the chromatographic information shown in table 3:
table 3 chromatographic information of the high performance liquid chromatogram in example 1
| Peak number | Retention time | Area of | Height | Concentration of |
| 1 | 28.834 | 1141163 | 104562 | 82.759 |
| 2 | 34.327 | 237736 | 16857 | 17.241 |
| Total of | - | 1378899 | 121419 | - |
The peak area of baicalin and the peak area of wogonoside are 4.85 and less than 10, and the medicinal materials in the sample are judged to be scutellaria baicalensis.
Example 2
(1) Taking 20g of a radix bupleuri sample with a lot number of 211201, placing the radix bupleuri sample in an electrothermal constant-temperature drying oven, drying the radix bupleuri sample for 3 hours at 60 ℃, cooling the radix bupleuri sample, crushing the radix bupleuri sample, sieving the radix bupleuri sample by a No. 3 sieve, taking 2g of sieved powder, adding 30ml of mixed solution of ethyl acetate and ethanol = 4: 1, carrying out ultrasonic treatment (power 250W and frequency 40 kHz) for 30 minutes, taking out the radix bupleuri sample, cooling the radix bupleuri sample, filtering the radix bupleuri sample, drying the filtrate by distillation, adding 5ml of methanol into residues to dissolve the residues, and taking supernate as a test solution; taking 1g of Scutellaria Yunnanensis contrast medicinal material and 1g of Scutellaria baicalensis contrast medicinal material respectively, and preparing Scutellaria Yunnanensis contrast medicinal material solution and Scutellaria baicalensis contrast medicinal material solution by the same method; performing thin layer chromatography test, collecting the sample solution, scutellaria Yunnanensis radix reference medicinal material solution and Scutellaria baicalensis radix reference medicinal material solution 3 μ l each, respectively dropping on the same polyamide film, pre-saturating with ethyl acetate, ethanol and formic acid = 4: 1: 1.5 as developing agent for 20 min, developing, taking out, air drying, and inspecting under ultraviolet lamp (365 nm).
In the chromatogram of the test solution, spots with the same color are all displayed at the positions corresponding to the chromatogram of the Scutellaria Yunnanensis contrast medicinal material; and at the position corresponding to the chromatogram of the radix scutellariae reference medicinal material, not all the spots with the same color are displayed, and the result is judged to be the Scutellaria delavayi.
(2) Measuring by high performance liquid chromatography:
chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile is taken as a mobile phase A, 0.4% formic acid solution is taken as a mobile phase B, and gradient elution is carried out according to the content in the table 4; the column temperature was 25 ℃; the detection wavelength is 270mm; the number of theoretical plates is not less than 5000 calculated according to baicalin peak.
Table 4 time of gradient elution and ratio of mobile phases a and B in example 2
| Time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0～10 | 3～10 | 90～97 |
| 11～20 | 11～27 | 89～73 |
| 21～55 | 28～40 | 72～60 |
| 56～70 | 41～92 | 59～8 |
Preparation of control solutions: taking appropriate amount of baicalin and wogonoside as reference substances, precisely weighing, and adding methanol to obtain solutions containing 40 μ g of baicalin and wogonoside per 1ml as reference substance solutions.
Preparation of a test solution: taking 20g of a bupleurum sample with the batch number of 211201, placing the sample in an electrothermal constant-temperature drying oven, drying the sample for 3 hours at the temperature of 60 ℃, cooling the sample, crushing the powder, sieving the powder by a No. 3 sieve, taking 2.0g of sieved powder, accurately weighing the powder, accurately adding 25ml of 50 percent ethanol, sealing the powder, weighing the powder, carrying out ultrasonic treatment (the power is 250W and the frequency is 40 kHz) for 30 minutes, taking out the powder, cooling the powder, weighing the powder again, complementing the lost weight with 50 percent ethanol, shaking the powder evenly, filtering the powder, and taking a subsequent filtrate to serve as a test solution.
The determination method comprises the following steps: precisely sucking 5 μ l of the control solution and 10 μ l of the sample solution, injecting into a liquid chromatograph, measuring, respectively recording the peak areas of baicalin and wogonoside in the control solution, and respectively recording the peak areas of baicalin and wogonoside corresponding to the sample solution and the control solution, wherein the results are shown in Table 5:
TABLE 5 Peak areas of test solution and control solution in example 2
| Peak area of baicalin | Peak area of wogonoside | The peak area of baicalin is larger than that of wogonoside |
| 775525 | 54880 | 14.13 |
The high performance liquid chromatogram obtained in example 2 has the chromatographic information shown in table 6:
TABLE 6 chromatographic information of high performance liquid chromatogram obtained in example 2
| Peak number | Retention time | Area of | Height | Concentration of |
| 1 | 28.801 | 778651 | 69325 | 93.443 |
| 2 | 34.265 | 54636 | 3880 | 6.557 |
| Total of | - | 833287 | 73206 | - |
The peak area of baicalin and the peak area of wogonoside are 14.13 and more than 10, and the Scutellaria baicalensis is judged.
Claims (5)
1. A Yunnan baikal skullcap root and identification method of baikal skullcap root, including using Yunnan baikal skullcap root reference medicinal material and baikal skullcap root reference medicinal material as the thin-layer chromatography identification method of the reference substance and using the liquid chromatogram in the peak area of baicalin and the peak area ratio of wogonoside to judge some or all in the identification method, characterized by that: (1) The thin-layer chromatography identification method taking the Scutellaria Yunnanensis contrast medicinal material and the Scutellaria baicalensis contrast medicinal material as the contrast is characterized in that the Scutellaria Yunnanensis contrast medicinal material and the Scutellaria baicalensis contrast medicinal material are used as the contrast, the thin-layer chromatography is adopted, ethyl acetate, ethanol and formic acid = 4: 1: 1.5 are used as developing agents, spots with the same color are all displayed on the positions corresponding to the chromatogram of the Scutellaria Yunnanensis contrast medicinal material in the chromatogram of a test sample, the spots are Scutellaria Yunnanensis, and the spots with the same color are all displayed on the positions corresponding to the chromatogram of the Scutellaria baicalensis contrast medicinal material, and the Scutellaria baicalensis is selected; (2) The identification method for judging by the ratio of the area of the baicalin peak to the area of the wogonoside peak in the liquid chromatogram is to respectively determine the area of the baicalin peak and the wogonoside peak by using a high performance liquid chromatography, taking a baicalin and wogonoside reference substance as a reference, acetonitrile as a mobile phase A, and a 0.3-0.6% formic acid solution as a mobile phase B, and adopting a gradient elution method, wherein the area of the baicalin peak to the area of the wogonoside peak is less than or equal to 10, the baicalin peak is baical skullcap root, and the area of the baicalin peak to the area of the wogonoside peak is greater than 10, the Scutellaria baicalensis is Yunnanensis.
2. The method for identifying Scutellaria yunnanensis and Scutellaria baicalensis Georgi according to claim 1, wherein: taking 20g of scutellaria baicalensis sample, 0.8-l.2g of scutellaria baicalensis control medicinal material and 0.8-l.2g of scutellaria baicalensis control medicinal material, drying for 1-4 hours at 50-70 ℃, cooling, crushing, sieving by a No. 3 sieve, taking 1.5-2.5g of sieved powder, adding 30-50ml of mixed solution of ethyl acetate and ethanol = 4: 1, carrying out ultrasonic treatment for 40-60 minutes under the conditions of power of 250W and frequency of 40kHz, taking out, cooling, filtering, evaporating filtrate to dryness, adding 4-6ml of methanol into residues for dissolving, and taking supernate to prepare a test solution, a scutellaria baicalensis control medicinal material solution and a scutellaria baicalensis control medicinal material solution; performing thin layer chromatography test, collecting the sample solution, scutellaria amoena reference medicinal material solution and Scutellaria baicalensis reference medicinal material solution 1-3 μ l respectively, dropping on the same polyamide film, pre-saturating with ethyl acetate, ethanol and formic acid = 4: 1: 1.5 as developing agent for 20-40 min, developing, taking out, air drying, and inspecting under 365nm ultraviolet lamp.
3. The method for identifying Scutellaria yunnanensis and Scutellaria baicalensis Georgi according to claim 2, wherein: the thin-layer chromatography identification method taking the Yunnan Baikal skullcap root reference medicinal material and the Baikal skullcap root reference medicinal material as the references comprises the steps of taking 20g of a Baikal skullcap root sample, lg of the Yunnan Baikal skullcap root reference medicinal material and lg of the Baikal skullcap root reference medicinal material, respectively placing the Baikal skullcap root sample, the Yunnan Baikal skullcap root reference medicinal material and the Baikal skullcap root reference medicinal material in an electrothermal constant-temperature drying oven, drying for 2-3 hours at 60 ℃, cooling, crushing, sieving by a No. 3 sieve, taking 2g of sieved powder, adding 40ml of mixed solution of ethyl acetate and ethanol = 4: 1, carrying out ultrasonic treatment for 45 minutes under the conditions of 250W power and 40kHz frequency, taking out, cooling, filtering, evaporating filtrate, dissolving residues by adding 5ml of methanol, taking supernatant, and preparing a test solution, the Yunnan Baikal skullcap root reference medicinal material and the Baikal skullcap root reference medicinal material; performing thin layer chromatography test, collecting the sample solution, scutellaria amoena reference medicinal material solution and Scutellaria baicalensis reference medicinal material solution 2 μ l each, respectively dropping on the same polyamide film, pre-saturating with ethyl acetate, ethanol and formic acid = 4: 1: 1.5 as developing agent for 30 min, developing, taking out, air drying, and inspecting under 365nm ultraviolet lamp.
4. The method for identifying Scutellaria yunnanensis and Scutellaria baicalensis Georgi according to claim 1, wherein: the identification method for judging by the peak area ratio of baicalin to the peak area of wogonoside in liquid chromatography comprises the steps of (1) taking octadecylsilane chemically bonded silica as a filler; acetonitrile is used as a mobile phase A, 0.3-0.6% formic acid solution is used as a mobile phase B, a gradient elution method is adopted, when the elution time is 0-10 minutes, the mobile phase A is 3-10%, the mobile phase B is 90-97%, when the elution time is 11-20 minutes, the mobile phase A is 11-27%, the mobile phase B is 73-89%, when the elution time is 21-55 minutes, the mobile phase A is 28-40%, the mobile phase B is 60-72%, when the elution time is 56-70 minutes, the mobile phase A is 41-92%, and the mobile phase B is 8-59; the column temperature is 25-35 ℃; the detection wavelength is 270mm; the number of theoretical plates is not less than 5000 calculated according to baicalin peak; (2) The reference solution is prepared by collecting baicalin and wogonoside as reference, precisely weighing, and adding methanol to obtain solutions containing 40-60 μ g of baicalin and wogonoside per 1ml as reference solutions; the preparation of the test solution is that 20g of scutellaria baicalensis sample is taken and placed in an electrothermal constant temperature drying oven to be dried for 1 to 4 hours at the temperature of 50 to 70 ℃, the mixture is cooled and crushed, the powder is sieved by a No. 3 sieve, 1.5 to 2.5g of the sieved powder is taken and precisely weighed, 25ml of 50 percent ethanol is precisely added, a plug is sealed, the weight is weighed, ultrasonic treatment is carried out for 40 to 60 minutes under the conditions of the power of 250W and the frequency of 40kHz, the mixture is taken out and cooled, the weight is weighed again, the weight loss is compensated by 50 percent ethanol, shaking up and filtering are carried out, and the subsequent filtrate is taken as the test solution; (3) Precisely sucking 5 μ l of control solution and 10 μ l of test solution, respectively, injecting into liquid chromatograph, measuring, respectively recording the peak areas of baicalin and wogonoside in the control solution, and respectively recording the peak areas of baicalin and wogonoside in the test solution and the control solution.
5. The method for identifying Scutellaria yunnanensis and Scutellaria baicalensis Georgi according to claim 4, wherein: the identification method for judging by the peak area ratio of baicalin to the peak area of wogonoside in liquid chromatography comprises the steps of (1) taking octadecylsilane chemically bonded silica as a filler; acetonitrile is used as a mobile phase A, 0.5% formic acid solution is used as a mobile phase B, a gradient elution method is adopted, when the elution time is 0-10 minutes, the mobile phase A is 3-10%, the mobile phase B is 90-97%, when the elution time is 11-20 minutes, the mobile phase A is 11-27%, the mobile phase B is 73-89%, when the elution time is 21-55 minutes, the mobile phase A is 28-40%, the mobile phase B is 60-72%, when the elution time is 56-70 minutes, the mobile phase A is 41-92%, and the mobile phase B is 8-59; the column temperature is 30 ℃; the detection wavelength is 270mm; the number of theoretical plates is not less than 5000 calculated according to baicalin peak; (2) The reference solution is prepared by collecting baicalin and wogonoside as reference, precisely weighing, and adding methanol to obtain solutions containing 50 μ g of baicalin and wogonoside per 1ml as reference solutions; preparing a test solution by taking 20g of a scutellaria baicalensis sample, placing the scutellaria baicalensis sample in an electrothermal constant-temperature drying oven, drying for 2 hours at 60 ℃, cooling, crushing, sieving by a No. 3 sieve, taking 2g of sieved powder, precisely weighing, precisely adding 25ml of 50% ethanol, sealing, weighing, ultrasonically treating for 50 minutes under the conditions of the power of 250W and the frequency of 40kHz, taking out, cooling, weighing again, complementing the weight loss by using 50% ethanol, shaking up, filtering, and taking a subsequent filtrate as the test solution; (3) Precisely sucking 5 μ l of control solution and 10 μ l of test solution, respectively, injecting into liquid chromatograph, measuring, respectively recording the peak areas of baicalin and wogonoside in the control solution, and respectively recording the peak areas of baicalin and wogonoside in the test solution and the control solution.
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