CN114594198A - Method for detecting aloe in new compound aloe capsule - Google Patents
Method for detecting aloe in new compound aloe capsule Download PDFInfo
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- CN114594198A CN114594198A CN202011429076.8A CN202011429076A CN114594198A CN 114594198 A CN114594198 A CN 114594198A CN 202011429076 A CN202011429076 A CN 202011429076A CN 114594198 A CN114594198 A CN 114594198A
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- aloe
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- 241001116389 Aloe Species 0.000 title claims abstract description 54
- 235000011399 aloe vera Nutrition 0.000 title claims abstract description 54
- 239000002775 capsule Substances 0.000 title claims abstract description 23
- 150000001875 compounds Chemical class 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 238000012360 testing method Methods 0.000 claims description 21
- 239000012085 test solution Substances 0.000 claims description 17
- 239000012088 reference solution Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 3
- 238000007605 air drying Methods 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- INCWELKXTZCRSA-UHFFFAOYSA-N ethyl acetate;methanol;hydrate Chemical compound O.OC.CCOC(C)=O INCWELKXTZCRSA-UHFFFAOYSA-N 0.000 claims description 3
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 3
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000523 sample Substances 0.000 description 22
- 238000001514 detection method Methods 0.000 description 13
- 238000010998 test method Methods 0.000 description 13
- 239000013642 negative control Substances 0.000 description 10
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- 239000003814 drug Substances 0.000 description 7
- 238000000605 extraction Methods 0.000 description 7
- 229940079593 drug Drugs 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000012925 reference material Substances 0.000 description 5
- 238000011835 investigation Methods 0.000 description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- QQILFGKZUJYXGS-UHFFFAOYSA-N Indigo dye Chemical compound C1=CC=C2C(=O)C(C3=C(C4=CC=CC=C4N3)O)=NC2=C1 QQILFGKZUJYXGS-UHFFFAOYSA-N 0.000 description 1
- -1 Succinum Chemical compound 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N30/94—Development
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention provides a method for detecting aloe in a novel compound aloe capsule, and the specificity and durability of the method meet better technical requirements. The method for detecting the aloe in the new compound aloe capsule can more effectively monitor the product quality of the new compound aloe capsule.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicines. In particular to a method for detecting aloe in a new compound aloe capsule.
Background
The new compound aloe capsule is loaded in' national medicine standard YBZ00012012-2015 of State food and drug administration, and the aloe identification processing method in the standard is heating reflux, so that the operation is not easy, and the batch size of one-time detection is small.
In order to improve the detection efficiency, more quickly, more simply and accurately master the processing method and better ensure the quality of the finished product of the new compound aloe capsule, a special customized detection method is adopted. The same invention has not been found by inquiring about the related materials.
Disclosure of Invention
The invention aims to solve the technical problem of designing a new method for detecting aloe in compound aloe capsules so as to effectively control the product quality.
The object of the invention can be achieved by the following scheme:
instrument, reagent and test sample
(1) The instrument comprises the following steps: PL602E electronic balance, ML304T electronic balance, ultrasonic cleaning machine,
(2) Reagent and reagent: see fig. 1, reagent and reagent information.
(3) A sample to be tested: new compound aloe capsule, batch No. 1911105, 1911108, 2006114.
Second, test method
Preparing a test sample: taking 0.5g of the content of the new compound aloe capsule, placing the new compound aloe capsule in a triangular flask with a plug, adding 10ml of methanol, carrying out ultrasonic treatment for 5 minutes, and filtering to obtain filtrate as a test solution.
Preparing a reference medicinal material solution: taking 0.14g of aloe reference material, placing in a triangular flask with a plug, adding 10ml of methanol, performing ultrasonic treatment for 5 minutes, and filtering to obtain filtrate as reference solution.
And (3) determination: sucking 2 μ l of each of the four solutions, respectively dropping on the same silica gel G thin layer plate with sodium carboxymethylcellulose as binder, developing with ethyl acetate-methanol-water (100: 17: 13) as developing agent, taking out, air drying, and fumigating in ammonia vapor.
Third, technical standard of detection
According to the detection result of the identification of 3 batches of new compound aloe capsules and aloes, the applicability of the method is judged.
The aloe identification and detection standard of the new compound aloe capsule is as follows: displaying a same yellow main spot on the chromatogram of the test solution at the position corresponding to the chromatogram of the reference solution; inspecting under ultraviolet lamp (365nm) to obtain yellow fluorescent spots.
Fourth, the feasibility of the detection method can be demonstrated by the following tests
1. Specificity
1.1 purpose
The new compound aloe capsule is proved to have no interference to aloe medicinal materials and special property under the condition of the method when other components are left when the prescription does not contain aloe.
1.2 methods
Preparation of negative control sample: weighing indigo naturalis, Succinum, and magnesium stearate, and mixing.
The detection method comprises the following steps:
preparing a test sample: taking 0.5g of the content of the new compound aloe capsule, placing the new compound aloe capsule in a triangular flask with a plug, adding 10ml of methanol, carrying out ultrasonic treatment for 5 minutes, and filtering to obtain filtrate as a test solution.
Negative control sample preparation: taking 0.5g of negative control sample, placing the negative control sample in a triangular flask with a plug, adding 10ml of methanol, carrying out ultrasonic treatment for 5 minutes, and filtering to obtain filtrate as a negative control sample solution.
Preparing a reference medicinal material solution: taking 0.14g of aloe reference material, adding 10ml of methanol, carrying out ultrasonic treatment for 5 minutes, filtering, and taking the filtrate as reference material solution.
And (3) determination: sucking the above negative control solution, test solution and aloe control solution 2 μ l each, respectively dropping on the same silica gel G thin layer plate with sodium carboxymethylcellulose as binder, developing with ethyl acetate-methanol-water (100: 17: 13) as developing agent, taking out, air drying, and fumigating in ammonia vapor.
1.3 acceptance criteria
Displaying a same yellow main spot on the chromatogram of the test solution at the position corresponding to the chromatogram of the reference solution; inspecting under ultraviolet lamp (365nm) to obtain yellow fluorescent spots.
In the negative control chromatogram, the same yellow main spot is not required to be displayed at the position corresponding to the control medicinal material chromatogram and the sample chromatogram; when the fluorescent powder is inspected under an ultraviolet lamp (365nm), the spots can not show orange yellow fluorescence.
1.4 results of measurement
Displaying a same yellow main spot on the chromatogram of the test solution at the position corresponding to the chromatogram of the reference solution; inspecting under ultraviolet lamp (365nm) to obtain yellow fluorescent spots.
In the negative control chromatogram, no main yellow spot appears at the position corresponding to the control medicinal material chromatogram and the sample chromatogram; the spot was observed under an ultraviolet lamp (365nm) and did not show orange-yellow fluorescence. (see FIG. 2 and FIG. 3)
1.5 conclusion:
the results show that: when the prescription of the new compound aloe capsule does not contain aloe, other components are remained, the identification of the aloe is not interfered under the condition of the method, and the specificity meets the requirement.
2. Durability
2.1 investigation of solvent addition
2.1.1 purpose
It was confirmed that when the addition amount of the extraction solvent was in the range of 10 ml. + -. 2ml, the test results were not affected.
2.1.2 methods
Preparing three parts of a test solution with the same test sample and the same solvent according to the second test method and the test method, wherein the adding amount of the solvent is 8ml, 10ml and 12ml respectively; and the detection is carried out according to the determination method under the item of the second test method.
2.1.3 acceptance criteria
Displaying a same yellow main spot on the chromatogram of the test solution at the position corresponding to the chromatogram of the reference solution; inspecting under ultraviolet lamp (365nm) to obtain yellow fluorescent spots. And the spots are clear, and the separation degree is good.
2.1.4 results
Displaying a same yellow main spot on the chromatogram of the test solution at the position corresponding to the chromatogram of the reference solution; inspecting under ultraviolet lamp (365nm) to obtain yellow fluorescent spots. And the spots are clear, and the separation degree is good. (see FIG. 4 and FIG. 5)
2.2 extraction time study
2.2.1 purpose
It was confirmed that when the extraction time was within 5 min. + -. 2min, the test results were not affected.
2.2.2 methods
Preparing three parts of a test solution from the same test sample according to the method of the second test method and the test method, wherein the extraction time is 3min, 5min and 7min respectively; and detecting according to the test method under the item of the second test method and the test method.
2.2.3 acceptance criteria
Displaying a same yellow main spot on the chromatogram of the test solution at the position corresponding to the chromatogram of the reference solution; inspecting under ultraviolet lamp (365nm) to obtain yellow fluorescent spots. And the spots are clear.
2.2.4 results
Displaying a same yellow main spot on the chromatogram of the test solution at the position corresponding to the chromatogram of the reference solution; inspecting under ultraviolet lamp (365nm) to obtain yellow fluorescent spots. And the spots were clear. (see FIG. 6 and FIG. 7)
2.3 silica gel G thin layer plate investigation
2.3.1 purpose
And (3) confirming that the test result is not influenced when different brands of silica gel G thin-layer plates are used for detection.
2.3.2 methods
Taking the sample solution under the item of specificity, detecting according to the determination method under the item of the second test method and the test method, and using silica gel G thin-layer plates of different brands for testing.
2.3.3 acceptance criteria
Displaying a same yellow main spot on the chromatogram of the test solution at the position corresponding to the chromatogram of the control solution; inspecting under ultraviolet lamp (365nm) to obtain yellow fluorescent spots. And the spots are clear.
2.3.4 results
Displaying a same yellow main spot on the chromatogram of the test solution at the position corresponding to the chromatogram of the reference solution; inspecting under ultraviolet lamp (365nm) to obtain yellow fluorescent spots. And the spots are clear. (see FIG. 8, FIG. 9, FIG. 10, FIG. 11)
2.4 conclusion:
the results show that:
1. when the volume adding amount is 8ml, 10ml and 12ml, the test result is not influenced, and the volume adding amount meets the requirement.
2. When the extraction time is respectively 3min, 5min and 7min, the test result is not influenced, and the examination of the extraction time meets the requirement.
3. When different brands of silica gel G thin-layer plates are used for detection, the test result is not influenced, and the examination of the silica gel G thin-layer plates meets the requirements.
Fifth, sample detection
Firstly, a test method and a result are as follows:
3 batches of the new compound aloe capsules are taken and tested according to the test method.
Displaying a same yellow main spot on the chromatogram of the test solution at the position corresponding to the chromatogram of the reference solution; inspecting under ultraviolet lamp (365nm) to obtain yellow fluorescent spots. And the spots are clear. (see FIG. 12, FIG. 13)
Conclusion II: according to the detection result of 3 batches of new compound aloe capsules and aloe identification, the method is judged to have applicability.
Drawings
FIG. 1 is a graph of reagent and reagent information;
FIG. 2 is a thin layer chromatogram of a negative control and aloe control;
FIG. 3 is a thin-layer chromatogram of negative control and aloe control under UV lamp (365 nm);
FIG. 4 is a thin layer chromatogram of the test sample and aloe control drug with 8ml, 10ml and 12ml of solvent added;
FIG. 5 is a thin layer chromatogram obtained by examining an aloe reference drug and a sample containing 8ml, 10ml and 12ml of solvent under an ultraviolet lamp (365 nm);
FIG. 6 is a thin layer chromatogram of the test sample and aloe control material extracted for 3min, 5min, and 7 min;
FIG. 7 is a thin layer chromatogram obtained by examining a sample and aloe reference material under an ultraviolet lamp (365nm) for extraction time of 3min, 5min, and 7 min;
FIG. 8 is a merck plate chromatogram of the test sample and aloe reference drug;
FIG. 9 is a thin layer chromatogram obtained by subjecting the test sample and aloe control drug to UV light irradiation (365 nm);
FIG. 10 is a thin layer chromatogram of a commercially available standard plate of the test sample and the aloe control;
FIG. 11 is a thin layer chromatogram of a sample and aloe reference material inspected under an ultraviolet lamp (365nm) on a commercially available common plate;
FIG. 12 is a thin layer chromatogram of 3 test samples and aloe control;
FIG. 13 is a thin layer chromatogram obtained by examining 3 batches of the test sample and aloe control drug under an ultraviolet lamp (365 nm).
Claims (1)
1. A method for detecting aloe in a new compound aloe capsule comprises the following steps: the method is characterized by comprising the following steps:
preparing a test sample: taking 0.5g of the content of the new compound aloe capsule, placing the new compound aloe capsule in a triangular flask with a plug, adding 10ml of methanol, carrying out ultrasonic treatment for 5 minutes, and filtering to obtain filtrate as a test solution; preparing a reference medicinal material solution: mixing aloe control 0.14g with 10ml methanol, and making into control solution by the same method; and (3) determination: sucking the two solutions 2 μ l each, dropping on the same silica gel G thin layer plate with sodium carboxymethylcellulose as binder, spreading with ethyl acetate-methanol-water (100: 17: 13) as developing agent, taking out, air drying, and fumigating in ammonia vapor; the standard is as follows: displaying a same yellow main spot on the chromatogram of the test solution at the position corresponding to the chromatogram of the reference solution; inspecting under ultraviolet lamp (365nm) to obtain yellow fluorescent spots.
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| CN202011429076.8A CN114594198A (en) | 2020-12-07 | 2020-12-07 | Method for detecting aloe in new compound aloe capsule |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1868520A (en) * | 2005-05-23 | 2006-11-29 | 长春市新安药业集团有限公司 | Compound Barbados aloe soft-capsule prepn. and its preparing method |
| CN101239141A (en) * | 2008-03-13 | 2008-08-13 | 上海复星临西药业有限公司 | Compound aloe capsule and preparation thereof |
| CN106124685A (en) * | 2016-06-10 | 2016-11-16 | 鲁南厚普制药有限公司 | The quality determining method of first luxuriant growth Tongbian capsule |
-
2020
- 2020-12-07 CN CN202011429076.8A patent/CN114594198A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1868520A (en) * | 2005-05-23 | 2006-11-29 | 长春市新安药业集团有限公司 | Compound Barbados aloe soft-capsule prepn. and its preparing method |
| CN101239141A (en) * | 2008-03-13 | 2008-08-13 | 上海复星临西药业有限公司 | Compound aloe capsule and preparation thereof |
| CN106124685A (en) * | 2016-06-10 | 2016-11-16 | 鲁南厚普制药有限公司 | The quality determining method of first luxuriant growth Tongbian capsule |
Non-Patent Citations (2)
| Title |
|---|
| 梁其冰;朱毅;黄守良;: "六味芦荟膏质量标准研究" * |
| 陈丹 等: "HPLC法测定便秘舒胶囊中芦荟苷含量" * |
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Application publication date: 20220607 |