CN107328765A - A kind of relevant material of α tropanols and isomers inspection method - Google Patents
A kind of relevant material of α tropanols and isomers inspection method Download PDFInfo
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- CN107328765A CN107328765A CN201710506395.6A CN201710506395A CN107328765A CN 107328765 A CN107328765 A CN 107328765A CN 201710506395 A CN201710506395 A CN 201710506395A CN 107328765 A CN107328765 A CN 107328765A
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Abstract
The invention discloses a kind of with method of the thin-layered chromatography inspection α tropanols about material and isomers.By preparing relevant material and isomer control product solution, applied sample amount is controlled, after solvent expansion, developer is sprayed, the relevant material and isomers of tropanol can be controlled below 0.5%.This method is simple to operate, convenient, fast, it is not necessary to special testing instrument, a kind of economical and practical effective ways is provided for the quick detection of tropanol.
Description
Technical field
The present invention relates to a kind of relevant material of α-tropanol and isomers inspection method, belong to Pharmaceutical Analysis technical field.
Background technology
Tropisetron HCl be a kind of peripheral neurons and central nervous system serotonin 3 (5-HT3) acceptor it is efficient,
High selectivity competes antagonist, for preventing and treating nausea and vomiting caused by cancer chemotherapy.The formulation of country's listing at present
There are tablet, capsule and injection.
Tropanol is a starting material for synthesizing Tropisetron, isomers β-tropanol and relevant thing in its quality control
Matter tropinone is by as important control object, to ensure the drug effect of Tropisetron HCl.But, tropanol and the like molecule
Amount is small, and alkalescence is big, and polarity is strong, no UV absorption, with DB-1 to point between isomers and principal component in gas phase process exploitation
Though good from spending, peak area and peak shape reappearance are very poor.Thin-layer chromatography developer extensively, can be used as a kind of semiquantitative determination hand
Section, develop it has preferable application value to the relevant material of tropanol and isomers inspection.
The content of the invention
In view of the shortcomings of the prior art, the problem to be solved in the present invention is, a kind of relevant material of α-tropanol and isomery are developed
Physical examination checking method, using the loading control product of debita spissitudo as test solution, is detected with thin-layered chromatography, obtains separating degree
Satisfactory result.
A kind of relevant material of α-tropanol of the present invention and isomers inspection method, comprise the following steps.
（1）Need testing solution is prepared：α-appropriate tropanol is taken, methylene chloride-methanol is used（1:1）Dissolve and be diluted to 1mg/
Ml ~ 2mg/ml solution, preferably 2mg/ml.
（2）Mixed reference substance solution is prepared：β-tropanol and appropriate tropinone are taken, methylene chloride-methanol is used（1:1）Dissolving
And the μ g/ml of 5 μ g/ml ~ 10 solution is diluted to, the preferably concentration of β-tropanol and tropinone is all 10 μ g/ml.
（3）Expansion：Above-mentioned need testing solution and appropriate mixed reference substance solution are taken, is put respectively in same silica gel thin-layer plate
On, after chromatography cylinder expansion, take out, cold wind drying；Solvent ratio is dichloromethane:Methanol:Water:Organic amine=40 ~ 60:30~
50:1~10:1 ~ 10, the preferably ratio of expansion is 50 ~ 60:35~45:4~6:2~5.
（4）Colour developing：Potassium iodobismuthate test solution is uniformly sprayed on lamellae, after cold wind drying, continues uniform sprinkling nitrous
Sour sodium test solution；Bismuth potassium iodide test solution compound method：A liquid：Take bismuth subnitrate/basic bismuth nitrate 0.85g, acetic acid 10ml and water on the rocks
40ml dissolves, and is used as stock solution；B liquid：40% KI（Brand-new）；Used time, A liquid and each 5ml of B liquid, plus 10% sulfuric acid is taken to be diluted to
50ml, is produced；Natrium nitrosum test solution compound method：Take natrium nitrosum appropriate, dissolved with 60% ethanol and be diluted to 10mg/ml's
Solution.
（5）As a result judge：Such as display β-tropanol and tropinone correspondence position spot in sample, with reference substance spot colors
Compare, must not be deeper.
Test sample sample applied sample amount need to be in below 20 μ g, preferably sample concentration 2mg/ml, the μ l of applied sample amount 10；It is deployed in silica gel
Carried out on plate, preferably high-efficient silica gel lamellae；Need to add a certain amount of polar protic solvent in solvent, to isomer separation
Degree just has an impact, otherwise without differentiating effect；But, if there was only protonic solvent in solvent, isomers is covered by principal point, is adjusted
Solvent ratio can not reach isomer separation purpose；Adding the water of proper proportion can be adjusted between tropinone and β-tropanol
Separating degree；Add organic amine makes after the expansion of impurity spot into wire as anti-hangover reagent, impurity spot is easy to relatively low
It is detected under concentration.Solvent ratio is dichloromethane:Methanol:Water:Organic amine=40 ~ 60:30~50:1~10:1 ~ 10, preferably
Solvent ratio is 50 ~ 60:35~45:4~6:2~5；Organic amine is the one kind, preferably isopropyl such as isopropylamine, triethylamine, diethylamine
Amine；Developer is bismuth potassium iodide test solution and natrium nitrosum test solution, wherein bismuth potassium iodide test solution preferably sulfuric acid improvement bismuth potassium iodide examination
Liquid, natrium nitrosum test solution preferably 60% ethanol solution makees solvent.
Beneficial effects of the present invention：
The present invention can effectively control starting by checking that TLC methods are groped to the relevant material of tropanol and isomers
The quality of material tropanol；This method is simple to operate, convenient, is the quick inspection of tropanol fast, it is not necessary to special testing instrument
Survey and a kind of economical and practical effective ways are provided.
Brief description of the drawings
Fig. 1 is the relevant material of α-tropanol and isomers inspection result figure of the embodiment of the present invention 1.
Fig. 2 is the relevant material of α-tropanol and isomers inspection result figure of the embodiment of the present invention 2.
Fig. 3 is the relevant material of α-tropanol and isomers inspection result figure of the embodiment of the present invention 3.
Embodiment
The present invention is described further with the following Examples.
Embodiment 1
α-appropriate tropanol is taken, accurately weighed, add methylene chloride-methanol（1:1）It is the molten of 2mg/ml to dissolve and be diluted to concentration
Liquid, is used as need testing solution.
β-tropanol and appropriate tropinone are taken, accurately weighed, add methylene chloride-methanol（1:1）Dissolve and be diluted to concentration
All it is 10 μ g/ml solution, is used as reference substance solution.
Above-mentioned need testing solution and each 10 μ l of reference substance solution are taken, puts respectively on same silica gel H SGF254 plates, uses dichloro
Methane:Methanol:Water:Isopropylamine=55:40:5:3 solvent expansion, cold wind drying.
First uniform sprinkling sulfuric acid improvement bismuth potassium iodide test solution is on lamellae during colour developing, and cold wind drying continues to spray nitrous
Sour sodium test solution；Bismuth potassium iodide test solution compound method：A liquid：Take bismuth subnitrate/basic bismuth nitrate 0.85g, acetic acid 10ml and water on the rocks
40ml dissolves, and is used as stock solution；B liquid：40% KI（Brand-new）；In use, A liquid and each 5ml of B liquid are taken, plus the dilution of 10% sulfuric acid
To 50ml, produce；Natrium nitrosum test solution compound method：Take natrium nitrosum appropriate, dissolved with 60% ethanol and be diluted to 10mg/ml
Solution.
As a result judge：Such as display β-tropanol and tropinone correspondence position spot in sample, with reference substance spot colors ratio
Compared with must not be deeper.
α-tropanol is shown in Fig. 1 about the inspection result of material and isomers, inspect result discovery, test sample in Rf values about
0.78 position spottiness, is compared with reference substance spot colors, without deeper, shows that tropinone residual quantity must not cross 0.5%；
The position spottiness of Rf values about 0.71, is compared with reference substance spot colors, without deeper, shows that β-tropanol residual quantity must not mistake
0.5%。
Embodiment 2
α-appropriate tropanol is taken, accurately weighed, add methylene chloride-methanol（1:1）It is the molten of 1mg/ml to dissolve and be diluted to concentration
Liquid, is used as need testing solution.
β-tropanol and appropriate tropinone are taken, accurately weighed, add methylene chloride-methanol（1:1）Dissolve and be diluted to concentration
All it is 5 μ g/ml solution, is used as reference substance solution.
Take above-mentioned need testing solution and each 5 μ l points of reference substance solution on same silica gel H SGF254 plates respectively, use dichloromethane
Alkane:Methanol:Water:Diethylamine=50:35:4:2 solvent expansion, cold wind drying.
First uniform sprinkling sulfuric acid improvement bismuth potassium iodide test solution is on lamellae during colour developing, and cold wind drying continues to spray nitrous
Sour sodium test solution；Bismuth potassium iodide test solution compound method：A liquid：Take bismuth subnitrate/basic bismuth nitrate 0.85g, acetic acid 10ml and water on the rocks
40ml dissolves, and is used as stock solution；B liquid：40% KI（Brand-new）；Used time, A liquid and each 5ml of B liquid, plus 10% sulfuric acid is taken to be diluted to
50ml, is produced；Natrium nitrosum test solution compound method：Take natrium nitrosum appropriate, dissolved with 60% ethanol and be diluted to 10mg/ml's
Solution.
As a result judge：Such as display β-tropanol and tropinone correspondence position spot in sample, with reference substance spot colors ratio
Compared with must not be deeper.
α-tropanol is shown in Fig. 2 about the inspection result of material and isomers, inspect result discovery, test sample in Rf values about
0.78 position spottiness, is compared with reference substance spot colors, without deeper, shows that tropinone residual quantity must not cross 0.5%；
The position spottiness of Rf values about 0.71, is compared with reference substance spot colors, without deeper, shows that β-tropanol residual quantity must not mistake
0.5%。
Embodiment 3
α-appropriate tropanol is taken, accurately weighed, add methylene chloride-methanol（1:1）It is the molten of 2mg/ml to dissolve and be diluted to concentration
Liquid, is used as need testing solution.
β-tropanol and appropriate tropinone are taken, accurately weighed, add methylene chloride-methanol（1:1）Dissolve and be diluted to concentration
All it is 8 μ g/ml solution, is used as reference substance solution.
Take above-mentioned need testing solution and each 10 μ l points of reference substance solution on same silica gel H SGF254 plates respectively, use dichloro
Methane:Methanol:Water:Isopropylamine=58:45:5:5 solvent expansion, cold wind drying.
First uniform sprinkling sulfuric acid improvement bismuth potassium iodide test solution is on lamellae during colour developing, and cold wind drying continues to spray nitrous
Sour sodium test solution；Bismuth potassium iodide test solution compound method：A liquid：Take bismuth subnitrate/basic bismuth nitrate 0.85g, acetic acid 10ml and water on the rocks
40ml dissolves, and is used as stock solution；B liquid：40% KI（Brand-new）；Used time, A liquid and each 5ml of B liquid, plus 10% sulfuric acid is taken to be diluted to
50ml, is produced；Natrium nitrosum test solution compound method：Take natrium nitrosum appropriate, dissolved with 60% ethanol and be diluted to 10mg/ml's
Solution.
As a result judge：Such as display β-tropanol and tropinone correspondence position spot in sample, with reference substance spot colors ratio
Compared with must not be deeper.
α-tropanol is shown in Fig. 3 about the inspection result of material and isomers, inspect result discovery, test sample in Rf values about
0.78 position spottiness, is compared with reference substance spot colors, without deeper, shows that tropinone residual quantity must not cross 0.5%；
The position spottiness of Rf values about 0.71, is compared with reference substance spot colors, without deeper, shows that β-tropanol residual quantity must not mistake
0.5%。
Claims (5)
1. a kind of relevant material of α-tropanol and isomers inspection method, are characterised by being checked using thin-layered chromatography, tool
Body comprises the following steps：
（1）Need testing solution is prepared：α-appropriate tropanol is taken, methylene chloride-methanol is used（1:1）Dissolve and be diluted to 1mg/ml ~
2mg/ml solution, preferably 2mg/ml；
（2）Mixed reference substance solution is prepared：β-tropanol and appropriate tropinone are taken, methylene chloride-methanol is used（1:1）Dissolve and dilute
The μ g/ml of 5 μ g/ml ~ 10 solution is interpreted into, the preferably concentration of β-tropanol and tropinone is all 10 μ g/ml；
（3）Expansion：Above-mentioned need testing solution and appropriate mixed reference substance solution are taken, is put respectively on same silica gel thin-layer plate,
After chromatography cylinder expansion, take out, cold wind drying；Solvent ratio is dichloromethane:Methanol:Water:Organic amine=40 ~ 60:30~50:1
~10:1 ~ 10, preferably solvent ratio is 50 ~ 60:35~45:4~6:2~5；
（4）Colour developing：Potassium iodobismuthate test solution is uniformly sprayed on lamellae, cold wind drying, continues uniform sprinkling natrium nitrosum examination
Liquid；Bismuth potassium iodide test solution compound method：A liquid：Take bismuth subnitrate/basic bismuth nitrate 0.85g, acetic acid 10ml and water 40ml on the rocks molten
Solution, is used as stock solution；B liquid：40% KI（Brand-new）；Used time, A liquid and each 5ml of B liquid, plus 10% sulfuric acid is taken to be diluted to 50ml, i.e.,
；Natrium nitrosum test solution compound method：Take natrium nitrosum appropriate, 10mg/ml solution is dissolved and be diluted to 60% ethanol；
（5）As a result judge：Such as display β-tropanol and tropinone correspondence position spot in sample, with reference substance spot colors ratio
Compared with must not be deeper.
2. a kind of relevant material of α-tropanol and isomers inspection method, test sample applied sample amount according to claims 1
Need to be in below 20 μ g, preferably sample concentration 2mg/ml, the μ l of applied sample amount 10.
3. a kind of relevant material of α-tropanol and isomers inspection method according to claims 1, are deployed in silica gel plate
Upper progress, preferably high-efficient silica gel lamellae.
4. the relevant material of a kind of α-tropanol according to claims 1 and isomers inspection method, solvent ratio is
Dichloromethane:Methanol:Water:Organic amine=40 ~ 60:30~50:1~10:1 ~ 10, preferably solvent ratio is 50 ~ 60:35~45:4~
6:2~5；Organic amine is the one kind, preferably isopropylamine such as isopropylamine, triethylamine, diethylamine.
5. a kind of relevant material of α-tropanol and isomers inspection method according to claims 1, developer is iodate
Bismuth potassium test solution and natrium nitrosum test solution, wherein bismuth potassium iodide test solution preferably sulfuric acid improve bismuth potassium iodide test solution, natrium nitrosum test solution
It is preferred that 60% ethanol solution makees solvent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110646540A (en) * | 2019-09-30 | 2020-01-03 | 武汉嘉诺康医药技术有限公司 | HPLC-ELSD detection method for Retamolin starting material and intermediate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1727890A (en) * | 2005-07-28 | 2006-02-01 | 山东齐都药业有限公司 | Method for testing tropine alcohol of residual intermediate product in synthesizing Troipisetron |
| CN102495170A (en) * | 2011-11-26 | 2012-06-13 | 山东齐都药业有限公司 | Method for detecting alpha-tropine in tropisetron hydrochloride injection |
-
2017
- 2017-06-28 CN CN201710506395.6A patent/CN107328765A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1727890A (en) * | 2005-07-28 | 2006-02-01 | 山东齐都药业有限公司 | Method for testing tropine alcohol of residual intermediate product in synthesizing Troipisetron |
| CN1316245C (en) * | 2005-07-28 | 2007-05-16 | 山东齐都药业有限公司 | Method for testing tropine alcohol of residual intermediate product in synthesizing Troipisetron |
| CN102495170A (en) * | 2011-11-26 | 2012-06-13 | 山东齐都药业有限公司 | Method for detecting alpha-tropine in tropisetron hydrochloride injection |
Non-Patent Citations (1)
| Title |
|---|
| 张晶等主编: "《中药化学》", 30 April 2015, 北京：中国农业大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110646540A (en) * | 2019-09-30 | 2020-01-03 | 武汉嘉诺康医药技术有限公司 | HPLC-ELSD detection method for Retamolin starting material and intermediate |
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Application publication date: 20171107 |