CN106468688A - A kind of detection method of urethanes residual quantity - Google Patents
A kind of detection method of urethanes residual quantity Download PDFInfo
- Publication number
- CN106468688A CN106468688A CN201510515089.XA CN201510515089A CN106468688A CN 106468688 A CN106468688 A CN 106468688A CN 201510515089 A CN201510515089 A CN 201510515089A CN 106468688 A CN106468688 A CN 106468688A
- Authority
- CN
- China
- Prior art keywords
- urethanes
- residual quantity
- reference substance
- ethanol solution
- detection method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention discloses a kind of detection method of urethanes residual quantity, take testing sample 0.2-0.4g, accurately weighed, it is placed in 150ml round-bottomed flask, add the ethanol solution for 60-90% for the mass fraction of 5-8ml, connect 42-48 DEG C of condensing tube water-bath and be heated to reflux 15-25min, place after cooling, as need testing solution；Precision measures urethanes reference substance 200 μ l, is placed in 50ml volumetric flask, the ethanol solution constant volume being 60-90% with mass fraction, and precision measures 2ml and is placed in 10ml volumetric flask, then is settled to scale with 60-90% ethanol solution, places, as reference substance solution；According to the test of residual solvent algoscopy, take reference substance solution sample introduction, record chromatogram, determine final residual quantity.The present invention is accurate for the testing result of urethanes residual quantity, and sample pre-treatments are simple and effective, and analysis time is short, and sensitivity is high.Detection method is more convenient and flexible.
Description
Technical field
The present invention relates to a kind of detection method, specifically a kind of detection method of urethanes residual quantity.
Background technology
Urethanes are the important source material in Chemical Manufacture, and tool has been widely used.Can the organic synthesiss such as used as pesticides, medicine intermediate it can also be used to synthesizing isocyanate, nontoxic polyurethane, melamine derivative, policapram are it is also possible to synthesize the heterocyclic compounds such as pyrroles, triazolone and triazine.
Urethanes are less than chloral hydrate to the inhibitory action of maincenter, also little on breathing and sanguimotor impact.Before barbiturate finds, once it was widely used as the anesthetics of laboratory animal, effect is fast and strong.To dog only as hypnotic, cause sleep.Even if anaesthetic effect also will not be produced to the big animal application heavy dose such as horse.Urethanes are weaker to the inhibitory action of medullary respiratory center, are the safer anesthetics of laboratory animal, and anesthesia can maintain 2～4 hours.But in existing technology, the detection method for urethanes is not easy, accuracy is not high.
Content of the invention
It is an object of the invention to provide a kind of detection method of urethanes residual quantity, to solve the problems, such as to propose in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme：
A kind of detection method of urethanes residual quantity, take testing sample 0.2-0.4g, accurately weighed, it is placed in 150ml round-bottomed flask, add the ethanol solution for 60-90% for the mass fraction of 5-8ml, connect 42-48 DEG C of condensing tube water-bath and be heated to reflux 15-25min, place after cooling, as need testing solution；Precision measures urethanes reference substance 200 μ l, is placed in 50ml volumetric flask, the ethanol solution constant volume being 60-90% with mass fraction, and precision measures 2ml and is placed in 10ml volumetric flask, then is settled to scale with 60-90% ethanol solution, places, as reference substance solution；According to residual solvent algoscopy（2010 editions annex of Chinese Pharmacopoeia VIII P the second method）Test, the capillary column with modified poly (ethylene glycol) as fixing phase as chromatographic column, 80 DEG C of column temperature；230 DEG C of injector temperature；Fid detector, detection room temperature is 250 DEG C；Take reference substance solution sample introduction, record chromatogram, determine final residual quantity.
As the further scheme of the present invention：The mass fraction of ethanol solution is 75%.
As the further scheme of the present invention：Heating in water bath reflux temperature is 45 DEG C.
Compared with prior art, the invention has the beneficial effects as follows：
The present invention is accurate for the testing result of urethanes residual quantity, and sample pre-treatments are simple and effective, and analysis time is short, and sensitivity is high.Detection method is more convenient and flexible.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained under the premise of not making creative work, broadly fall into the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of detection method of urethanes residual quantity, take testing sample 0.2g, accurately weighed, it is placed in 150ml round-bottomed flask, the mass fraction of addition 5ml is 60% ethanol solution, connects 42 DEG C of condensing tube water-bath and is heated to reflux 15min, place after cooling, as need testing solution；Precision measures urethanes reference substance 200 μ l, is placed in 50ml volumetric flask, the ethanol solution constant volume being 60% with mass fraction, and precision measures 2ml and is placed in 10ml volumetric flask, then is settled to scale with 60% ethanol solution, places, as reference substance solution；According to residual solvent algoscopy（2010 editions annex of Chinese Pharmacopoeia VIII P the second method）Test, the capillary column with modified poly (ethylene glycol) as fixing phase as chromatographic column, 80 DEG C of column temperature；230 DEG C of injector temperature；Fid detector, detection room temperature is 250 DEG C；Take reference substance solution sample introduction, record chromatogram, determine final residual quantity.
Embodiment 2
In the embodiment of the present invention, a kind of detection method of urethanes residual quantity, take testing sample 0.4g, accurately weighed, it is placed in 150ml round-bottomed flask, the mass fraction of addition 8ml is 90% ethanol solution, connects 48 DEG C of condensing tube water-bath and is heated to reflux 25min, place after cooling, as need testing solution；Precision measures urethanes reference substance 200 μ l, is placed in 50ml volumetric flask, the ethanol solution constant volume being 90% with mass fraction, and precision measures 2ml and is placed in 10ml volumetric flask, then is settled to scale with 90% ethanol solution, places, as reference substance solution；According to residual solvent algoscopy（2010 editions annex of Chinese Pharmacopoeia VIII P the second method）Test, the capillary column with modified poly (ethylene glycol) as fixing phase as chromatographic column, 80 DEG C of column temperature；230 DEG C of injector temperature；Fid detector, detection room temperature is 250 DEG C；Take reference substance solution sample introduction, record chromatogram, determine final residual quantity.
Embodiment 3
In the embodiment of the present invention, a kind of detection method of urethanes residual quantity, take testing sample 0.3g, accurately weighed, it is placed in 150ml round-bottomed flask, the mass fraction of addition 6ml is 75% ethanol solution, connects 45 DEG C of condensing tube water-bath and is heated to reflux 20min, place after cooling, as need testing solution；Precision measures urethanes reference substance 200 μ l, is placed in 50ml volumetric flask, the ethanol solution constant volume being 75% with mass fraction, and precision measures 2ml and is placed in 10ml volumetric flask, then is settled to scale with 75% ethanol solution, places, as reference substance solution；According to residual solvent algoscopy（2010 editions annex of Chinese Pharmacopoeia VIII P the second method）Test, the capillary column with modified poly (ethylene glycol) as fixing phase as chromatographic column, 80 DEG C of column temperature；230 DEG C of injector temperature；Fid detector, detection room temperature is 250 DEG C；Take reference substance solution sample introduction, record chromatogram, determine final residual quantity.
According to the step described in embodiment 3, reference substance adds test sample precision formula to be tested and the results are shown in Table 1.Same operation repeats six times.
Table 1 reference substance adds test sample precision test each component measured quantity result
| 1 | 2 | 3 | 4 | 5 | 6 | RSD | |
| Urethanes | 11892 | 11735 | 11659 | 11359 | 11861 | 11754 | 1.64 |
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and without departing from the spirit or essential characteristics of the present invention, the present invention can be realized in other specific forms.Therefore, no matter from the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is limited by claims rather than described above, it is intended that all changes in the implication and scope of the equivalency of claim that fall are included in the present invention.
In addition, it should be understood that, although this specification is been described by according to embodiment, but not each embodiment only comprises an independent technical scheme, this narrating mode of description is only for clarity, those skilled in the art should using description as an entirety, the technical scheme in each embodiment can also through appropriately combined, formed it will be appreciated by those skilled in the art that other embodiment.
Claims (3)
1. a kind of detection method of urethanes residual quantity, it is characterized in that, take testing sample 0.2-0.4g, accurately weighed, it is placed in 150ml round-bottomed flask, add the ethanol solution for 60-90% for the mass fraction of 5-8ml, connect 42-48 DEG C of condensing tube water-bath and be heated to reflux 15-25min, place after cooling, as need testing solution；Precision measures urethanes reference substance 200 μ l, is placed in 50ml volumetric flask, the ethanol solution constant volume being 60-90% with mass fraction, and precision measures 2ml and is placed in 10ml volumetric flask, then is settled to scale with 60-90% ethanol solution, places, as reference substance solution；According to residual solvent algoscopy test, the capillary column with modified poly (ethylene glycol) as fixing phase as chromatographic column, 80 DEG C of column temperature；230 DEG C of injector temperature；Fid detector, detection room temperature is 250 DEG C；Take reference substance solution sample introduction, record chromatogram, determine final residual quantity.
2. the detection method of urethanes residual quantity according to claim 1 is it is characterised in that the mass fraction of ethanol solution is 75%.
3. the detection method of urethanes residual quantity according to claim 1 is it is characterised in that heating in water bath reflux temperature is 45 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510515089.XA CN106468688B (en) | 2015-08-21 | 2015-08-21 | A kind of detection method of urethanes residual quantity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510515089.XA CN106468688B (en) | 2015-08-21 | 2015-08-21 | A kind of detection method of urethanes residual quantity |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106468688A true CN106468688A (en) | 2017-03-01 |
| CN106468688B CN106468688B (en) | 2018-08-24 |
Family
ID=58229176
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510515089.XA Active CN106468688B (en) | 2015-08-21 | 2015-08-21 | A kind of detection method of urethanes residual quantity |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106468688B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004046714A1 (en) * | 2002-11-19 | 2004-06-03 | Daicel Chemical Industries, Ltd. | Separating agent for optical isomer |
| CN102353728A (en) * | 2011-06-29 | 2012-02-15 | 中国食品发酵工业研究院 | Rapid detection method for production process quality control of yellow wine |
| CN102393434A (en) * | 2011-11-01 | 2012-03-28 | 江南大学 | Method for rapidly measuring ethyl carbamate content in distilled liquor |
| CN102608226A (en) * | 2011-12-20 | 2012-07-25 | 江南大学 | Method for quickly measuring ethyl carbamate in yeast, fermented grains or fermenting mash |
| CN103344725A (en) * | 2013-07-25 | 2013-10-09 | 四川剑南春（集团）有限责任公司 | Method for simultaneously and quantitatively detecting content of ethyl carbamate and phthalate in distilled white wine |
-
2015
- 2015-08-21 CN CN201510515089.XA patent/CN106468688B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004046714A1 (en) * | 2002-11-19 | 2004-06-03 | Daicel Chemical Industries, Ltd. | Separating agent for optical isomer |
| CN102353728A (en) * | 2011-06-29 | 2012-02-15 | 中国食品发酵工业研究院 | Rapid detection method for production process quality control of yellow wine |
| CN102393434A (en) * | 2011-11-01 | 2012-03-28 | 江南大学 | Method for rapidly measuring ethyl carbamate content in distilled liquor |
| CN102608226A (en) * | 2011-12-20 | 2012-07-25 | 江南大学 | Method for quickly measuring ethyl carbamate in yeast, fermented grains or fermenting mash |
| CN103344725A (en) * | 2013-07-25 | 2013-10-09 | 四川剑南春（集团）有限责任公司 | Method for simultaneously and quantitatively detecting content of ethyl carbamate and phthalate in distilled white wine |
Non-Patent Citations (3)
| Title |
|---|
| JIAO, ZHIHUA等: "Ethyl Carbamate in Fermented Beverages: Presence, Analytical Chemistry, Formation Mechanism, and Mitigation Proposals", 《COMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY》 * |
| 王博等: "发酵酒中氨基甲酸乙酯的研究进展", 《生物信息学》 * |
| 罗杰等: "氨基甲酸乙酯检测方法研究进展", 《酿酒科技》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106468688B (en) | 2018-08-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110320293B (en) | Method for determining residual solvent in phthalide compound | |
| CN104931595A (en) | Method using high performance liquid chromatography (HPLC) to measure Rivaroxaban intermediate content | |
| CN106645508B (en) | The construction method of FENGRE GANMAO KELI HPLC characteristic spectrum | |
| CN107064350A (en) | Method for detecting suspected genotoxic impurity of tofacitinib citrate | |
| CN111855871A (en) | Method for measuring iprovalicarb and fluopyram in tobacco by combination of filtration type solid-phase extraction and supercritical fluid chromatography-mass spectrometry | |
| Yang et al. | Development of a new certified reference material of tinidazole for quality and safety of agro-products | |
| CN105092761B (en) | The detection method of antivirus oral liquid volatile ingredient | |
| CN106468688A (en) | A kind of detection method of urethanes residual quantity | |
| CN100491998C (en) | Pericarpium Trichosanthis or Pericarpium Trichosanthis injection liquid chromatography fingerprint test method | |
| CN104950045A (en) | Detection method for contents of six volatile components in vegetable drugs of Longhurendan | |
| CN104374841B (en) | Tablet of antelope's horn for common cold quality control is with reference to product and purposes | |
| CN103864646B (en) | The impurity preparation of rasagiline mesilate and the method for analysis | |
| CN104502491B (en) | A kind of headspace sampling measures the method for crude drug oxfendazole dissolvent residual | |
| CN102901784A (en) | Method for performing headspace gas chromatographic detection on formic acid in aceclofenac bulk pharmaceutical chemicals | |
| CN113514588B (en) | High performance liquid chromatography analysis method of relevant substances of cysteamine for injection | |
| CN103543231B (en) | The method for separating and analyzing of chloroform residual quantity in a kind of meclozine hydrochloride | |
| CN111208215A (en) | Method for detecting impurity 2-mercaptobenzothiazole in ceftriaxone sodium | |
| Sigvardson et al. | The isolation and identification of a toxic impurity in XP315 drug substance | |
| Uchiyama et al. | A phenethylamine derivative 2-(4-iodo-2, 5-dimethoxyphenyl)-N-[(3, 4-methylenedioxyphenyl) methyl] ethanamine (25I-NB34MD) and a piperazine derivative 1-(3, 4-difluoromethylenedioxybenzyl) piperazine (DF-MDBP), newly detected in illicit products | |
| CN104237406A (en) | Method for detecting residual amount of chloropropanol | |
| Yadav et al. | Characterization of forced degradation products & related substances of bilastine by online LC-Q-TOF-MS and in-silico study of characterized compounds | |
| CN105628807B (en) | A kind of quality determining method of the amino piperidines of 1 Boc 4 | |
| CN110146622A (en) | The measuring method and quality assessment method of mangiferin in a kind of common bombax flower | |
| CN113791149B (en) | Detection method of 1-chloro-3-methoxypropane related substance | |
| CN112630346B (en) | Quantitative analysis method for residual solvent in ibrutinib |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 274200 Datianji Town, Chengwu County, Heze City, Shandong Province (north of Chen Hutong Village and north of Dongfeng Highway) Patentee after: Heze Tianhong fruit and vegetable Limited by Share Ltd Address before: 274200 Datianji Town, Chengwu County, Heze City, Shandong Province (north of Chen Hutong Village and north of Dongfeng Highway) Patentee before: HEZE TIANHONG FRUITS & VEGETABLES CO., LTD. |
|
| CP01 | Change in the name or title of a patent holder |