CN114387856A - Micro-drug chemical experiment and chemical examination integrated teaching method - Google Patents
Micro-drug chemical experiment and chemical examination integrated teaching method Download PDFInfo
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- CN114387856A CN114387856A CN202011067090.8A CN202011067090A CN114387856A CN 114387856 A CN114387856 A CN 114387856A CN 202011067090 A CN202011067090 A CN 202011067090A CN 114387856 A CN114387856 A CN 114387856A
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- 238000002474 experimental method Methods 0.000 title claims abstract description 29
- 239000000126 substance Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000003814 drug Substances 0.000 title claims abstract description 7
- 229940079593 drug Drugs 0.000 title claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 238000002844 melting Methods 0.000 claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 15
- 238000012360 testing method Methods 0.000 claims abstract description 10
- 238000004809 thin layer chromatography Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000376 reactant Substances 0.000 claims abstract description 7
- 238000003556 assay Methods 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000741 silica gel Substances 0.000 claims abstract description 5
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- 238000013461 design Methods 0.000 claims abstract description 3
- 239000012535 impurity Substances 0.000 claims abstract description 3
- 230000035484 reaction time Effects 0.000 claims abstract description 3
- 239000013558 reference substance Substances 0.000 claims abstract description 3
- 238000004088 simulation Methods 0.000 claims abstract description 3
- 230000010354 integration Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000004904 shortening Methods 0.000 claims 1
- 239000012295 chemical reaction liquid Substances 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 3
- 238000013459 approach Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 17
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 12
- 239000000047 product Substances 0.000 description 9
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 6
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 6
- 229930003268 Vitamin C Natural products 0.000 description 6
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 6
- 235000019154 vitamin C Nutrition 0.000 description 6
- 239000011718 vitamin C Substances 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 3
- 229960004889 salicylic acid Drugs 0.000 description 3
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical compound CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 description 2
- 229960001138 acetylsalicylic acid Drugs 0.000 description 2
- 238000007605 air drying Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 240000003537 Ficus benghalensis Species 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- -1 n-pentanol-chloroform-methanol Chemical compound 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
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- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09B—EDUCATIONAL OR DEMONSTRATION APPLIANCES; APPLIANCES FOR TEACHING, OR COMMUNICATING WITH, THE BLIND, DEAF OR MUTE; MODELS; PLANETARIA; GLOBES; MAPS; DIAGRAMS
- G09B23/00—Models for scientific, medical, or mathematical purposes, e.g. full-sized devices for demonstration purposes
- G09B23/24—Models for scientific, medical, or mathematical purposes, e.g. full-sized devices for demonstration purposes for chemistry
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- General Physics & Mathematics (AREA)
- Mathematical Analysis (AREA)
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- Algebra (AREA)
- Computational Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Mathematical Optimization (AREA)
- Medicinal Chemistry (AREA)
- Pure & Applied Mathematics (AREA)
- Business, Economics & Management (AREA)
- Chemical & Material Sciences (AREA)
- Educational Administration (AREA)
- Educational Technology (AREA)
- Theoretical Computer Science (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention provides a micro-drug chemical experiment and assay integrated teaching method, which comprises the following steps: a micro (ul grade) disposable reaction vessel and a micro (ul grade) reaction vessel are used. The chemical experiment reaction is heated by normal temperature or water bath, air is extruded to a melting point tube of reaction liquid by using a quantitative sample application capillary tube for bubble stirring, the reaction time is shortened by three quarters, and the reaction liquid is subjected to thin layer chromatography directly or after being dissolved by organic solution after the reaction is finished. The students take pictures of results and compare the results for analysis by carrying out thin layer chromatography on the samples of the control initial reactant and the teacher reaction product. Separation and simulation of related species approach the impurity experiment: the students scrape the related substance reference substances from the silica gel plate to dissolve again and perform point plate comparison with the second reactant, and can simulate two to three condition tests and perform TCL test by design experiments in the traditional experiment time.
Description
Technical Field
The invention relates to a micro-drug chemical experiment and assay integrated teaching method, belonging to the field of education.
Background
The modern pharmaceutical chemistry industry needs more thinking, can analyze and produce results, and chemical workers in industry master the technical basic operation requirements of a plurality of enterprises, particularly the international customized product industry, of three hatchets (scientific inquiry, chemical laboratory and product thin layer separation). The traditional chemical experiment teaching is far from meeting the requirements: when phenomena such as dissolution, discoloration, precipitation, gas generation and the like are observed, devices such as beakers and test tubes are often adopted, and a large amount of chemical reagents are often consumed. Under the condition, on one hand, the experiment cost is high, so that part of valuable reagents cannot be applied to experiment teaching; on the other hand, more products after reaction are not easy to treat, easily cause environmental pollution and do not accord with the concept of green chemistry; thirdly, some manufacturers develop instruments for micro-chemical reaction, but the cost is often high, the instruments only stay in phenomenon observation, students do not test immediately, and the essence is seen through the phenomenon, so that the instruments are not popularized in teaching; finally, the experiment time of students is too long, and because the devices and the reagents are less, the chance of operation is less, and no related substances are used for exploring the time, the experiment skill of the students is not improved, and the spirit of craftsmen is cultivated.
The traditional board of the college of medical sciences of Guizhou medical sciences, DongyongYonxi and the like publishes 'improvement and exploration of a teaching mode of a chemical experiment of medicine', and proposes a teaching method adopting a new reagent new process and a semi-micro experiment method, which is a milli-upgrading reaction, not a micro-scale reaction, does not use a disposable reaction container, and does not cause substantial exploration of experimental and chemical examination integration. Guoni, a chemical and chemical institute of academy of sciences and professors of Xiyang, is published in "research on trace and greening of organic chemistry experiment teaching" and is only a proposition with no specific equipment and teaching method. A patent for observing the ultra-micro chemical reaction without container (application No. 202010136214.7) invented by the Observation device of the origin-origin Yao of the Zhaoqing college mentions the chemical reaction of micro-upgrade, but the device has higher cost than a disposable melting point tube, is not easy to popularize and does not mention the teaching method of experimental assay integration. The Liu hong Yan of Shanxi university has invented a novel micro-chemical reaction device (application No. 201720292735.5), which is also complex in structure, high in cost as the invention of a long-lived Yao, not easy to popularize to one hand, and inconvenient to operate. And the microchemical system (application number: 03825441.7) invented by Shankouchun of Japan Banyan Kaisha has high technical content, can mix, react, separate, extract, detect and the like liquid-based samples, can meet the requirement of integrated teaching of pharmaceutical chemistry experimental tests, but has high cost and is difficult to popularize.
Disclosure of Invention
Aiming at the problems, the invention provides a pharmaceutical chemistry experiment teaching method which is lower in cost, more convenient to operate, more efficient in teaching, safer in process and less in pollution, and can solve the four problems: the capillary melting point tube with one sealed end is used as a disposable experimental device, so that the cost is extremely low, and the consumption of chemical reagents is extremely low; environmental pollution is not easily caused after the experimental reaction, and the green chemical concept is met; thirdly, because the reagent is less and the reaction experiment time is shorter, the reagent can be immediately tested and separated, so that students can see the essence through the phenomenon, and chemical products can be hidden everywhere; the students can use several melting point tubes, so that the chance of using the device is greatly increased, the exploration time of related substances is sufficient, the imagination of the students can be fully exerted, the experimental skills of the students are improved, and the spirit of craftsmen is cultivated.
In general, the invention provides a micro-drug chemical experiment and assay integrated teaching method, which comprises the following steps:
1. a micro (ul grade) disposable reaction vessel and a micro (ul grade) reaction vessel are used.
2. The chemical experiment reaction is heated by normal temperature or water bath, air is extruded to a melting point tube of reaction liquid by using a quantitative sample application capillary tube for bubble stirring, the reaction time is shortened by three quarters, and the reaction liquid is subjected to thin layer chromatography directly or after being dissolved by organic solution after the reaction is finished.
3. The students take pictures of results and compare the results for analysis by carrying out thin layer chromatography on the samples of the control initial reactant and the teacher reaction product.
4. Separation and simulation of related species approach the impurity experiment: the students scrape the related substance reference substances from the silica gel plate to dissolve again and perform point plate comparison with the second reactant, and can simulate two to three condition tests and perform TCL test by design experiments in the traditional experiment time.
In the above operation step 1, a micro (ul grade) disposable reaction container is used as a capillary melting point tube (0.9-1.1 × 100mm) with one end sealed, and a micro (ul grade) reaction measuring device is used as a dropper for quantitatively sampling capillary tubes 1ul, 5ul, 10ul and 20ul by thin layer chromatography.
In the above operation step 2, a quantitative spotting capillary is used to extrude air into the melting point tube of the reaction solution for bubble stirring, as shown in the attached figure.
The silica gel plate used in the TCL thin layer analysis in operation step 3 above is a model GF254 specification 25 × 100mm silica gel glass plate.
The parameters which can be changed by simulating two to three conditions in the operation step 4 include temperature, the mixture ratio of reactants, catalyst addition and the like.
Drawings
Fig. 1 is a diagram of a feeding device of a method for preparing aspirin in the second embodiment of the present invention.
The specific implementation mode is as follows:
example one (teaching of vitamin C oxidation reaction):
a vitamin C (2ml) injection is cut off by a grinding wheel, the solution is poured into a 10ml test tube, 40ul of vitamin C solution is taken by a quantitative spotting capillary and added into a capillary melting point tube, the capillary melting point tube is heated for 5 minutes in boiling water, and the color change is observed.
40ul of vitamin C solution is taken by a quantitative spotting capillary, added into a capillary melting point tube, added with 5ul of 3 percent hydrogen peroxide, heated in boiling water for 5 minutes, and the color change is observed.
Taking 40ul of vitamin C solution by using a quantitative spotting capillary, adding the vitamin C solution into a capillary melting point tube, adding 2% sodium sulfite solution, adding 5ul of 3% hydrogen peroxide, heating in boiling water for 5 minutes, and observing color change.
Using 1ul of capillary sample tube to dot the plates on GF254 according to the sequence of vitamin initial solution, [0014] product solution, [0015] product solution and [0016] product solution, after air drying, developing in n-pentanol-chloroform-methanol (6:2:1) developing agent, taking out and air drying, observing related substances under (254nm) ultraviolet lamp, and taking pictures for uploading.
Example two (teaching of aspirin synthesis):
40ul of 25% acetic anhydride solution of newly formulated salicylic acid (previously dropped with 5 drops of concentrated sulfuric acid) was drawn into a melting point tube by a quantitative spotting capillary and heated in a water bath at 50-55 deg.C for 5 minutes.
40ul of 25% acetic anhydride solution of newly formulated salicylic acid (previously dropped with 5 drops of concentrated sulfuric acid) was drawn into a melting point tube by a quantitative spotting capillary and heated in a water bath at 70-75 ℃ for 5 minutes.
Quantitatively spotting on GF254 thin layer plate by using 1ul capillary sample tube according to the sequence of salicylic acid initial solution, [0018] product solution, and [0019] product solution, developing with petroleum ether-ethyl acetate-glacial acetic acid (12:6:0.1) as developing agent, inspecting related substances under 254nm ultraviolet lamp, and taking pictures for uploading.
Claims (5)
1. A micro-drug chemical experiment and assay integrated teaching method is characterized by comprising the following steps: teachers used disposable experimental reaction vessels: one end of the capillary melting point tube (0.9-1.1 × 100mm) is sealed, teachers use a fixed experiment reaction volume and bubble stirring, and droppers of 1ul, 5ul, 10ul and 20ul of thin layer chromatography quantitative sample application capillary tubes are adopted; heating a chemical experiment reaction by using a normal temperature or a water bath, extruding air to a melting point tube of a reaction solution by using a quantitative sample application capillary tube for stirring, shortening the reaction time by three quarters, and carrying out thin layer chromatography after the reaction solution is directly dissolved or is dissolved by using an organic solution after the reaction is finished; carrying out thin-layer chromatography on the sample contrast initial reactant and the teacher reaction product by students, and photographing and analyzing the result; the separation and simulation of relevant substances are close to the impurity experiment, students can scrape relevant substance reference substances from a silica gel plate to contrast with a second reactant, and two to three conditions of tests can be simulated by design experiments in the traditional experiment time and TCL tests can be carried out.
2. The container of claim 1, wherein: a micro (ul grade) disposable reaction vessel and a micro (ul grade) reaction vessel are used.
3. The process of claim 1, wherein: after the reaction is finished, the reaction solution is directly or after being dissolved by organic solution, thin layer chromatography is carried out.
4. The result of claim 1 is characterized by: and (3) contrast teaching, wherein the mobile phone is used for photographing to directly evaluate an experimental result.
5. The structure of claim 1 is characterized in that: exploratory teaching, extension of experimental conditions and integration with assays.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011067090.8A CN114387856A (en) | 2020-10-05 | 2020-10-05 | Micro-drug chemical experiment and chemical examination integrated teaching method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011067090.8A CN114387856A (en) | 2020-10-05 | 2020-10-05 | Micro-drug chemical experiment and chemical examination integrated teaching method |
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| Publication Number | Publication Date |
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| CN114387856A true CN114387856A (en) | 2022-04-22 |
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| CN202011067090.8A Pending CN114387856A (en) | 2020-10-05 | 2020-10-05 | Micro-drug chemical experiment and chemical examination integrated teaching method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101148437A (en) * | 2007-11-05 | 2008-03-26 | 南京大学 | Biinomenine derivative connected with C-C bond, preparation method and application thereof |
| CN107589193A (en) * | 2017-10-25 | 2018-01-16 | 南京工业大学 | A kind of method that protein inhibitor is screened using micro-reaction device |
| CN110412104A (en) * | 2019-08-15 | 2019-11-05 | 福州大学 | Interface and preparation method thereof associated with a kind of temperature control capillary electrophoresis-chemiluminescence |
-
2020
- 2020-10-05 CN CN202011067090.8A patent/CN114387856A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101148437A (en) * | 2007-11-05 | 2008-03-26 | 南京大学 | Biinomenine derivative connected with C-C bond, preparation method and application thereof |
| CN107589193A (en) * | 2017-10-25 | 2018-01-16 | 南京工业大学 | A kind of method that protein inhibitor is screened using micro-reaction device |
| CN110412104A (en) * | 2019-08-15 | 2019-11-05 | 福州大学 | Interface and preparation method thereof associated with a kind of temperature control capillary electrophoresis-chemiluminescence |
Non-Patent Citations (1)
| Title |
|---|
| 赵庆 等: "毛细管反应在天然产物研究中的应用", 《天然产物研究与开发》, vol. 11, no. 05, pages 24 - 28 * |
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Application publication date: 20220422 |