CN106706780A - Detection method for thiamphenicol and kit - Google Patents
Detection method for thiamphenicol and kit Download PDFInfo
- Publication number
- CN106706780A CN106706780A CN201611112562.0A CN201611112562A CN106706780A CN 106706780 A CN106706780 A CN 106706780A CN 201611112562 A CN201611112562 A CN 201611112562A CN 106706780 A CN106706780 A CN 106706780A
- Authority
- CN
- China
- Prior art keywords
- thiamphenicol
- solution
- detection method
- dimethylformamide
- kit
- 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.)
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Classifications
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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
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- 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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The invention relates to the technical field of medicines and discloses a detection method for thiamphenicol and a kit. A mobile phase in a high-performance liquid chromatography adopts a mixed solution of dimethyl formamide, methyl alcohol, a monopotassium phosphate solution, a silver nitrate solution and ethyl acetate. The detection method for thiamphenicol and the kit have the advantages that the thiamphenicol can be effectively detected, valid data can be obtained by detection of water solubility of the thiamphenicol, and simultaneously the stability of the thiamphenicol also can be effectively detected, so that when the thiamphenicol is processed, the real quality of the product can be obtained; and by arrangement of pressure-reducing foam boards, pressure-reducing springs, a limiting board and limiting holes, a reagent bottle can not be broken by squeezing when being put in a main kit body, so that the condition of medicine damage is avoided.
Description
Technical field
The present invention relates to pharmaceutical technology field, specially a kind of Thiamphenicol detection method and kit.
Background technology
Thiamphenicol, this product is white crystalline powder；Odorless is uncommon for sensitive bacteria such as haemophilus influenzae, large intestine angstrom
The caused respiratory tract such as bacterium and Salmonella, urinary tract and enteron aisle etc. infect., also known as thiomycin, chemical entitled 1- is to first for Thiamphenicol
Sulfonyl-phenyl -2- dichloro acetamide -1,3 propane diols.Its structure similar in appearance to chloramphenicol, its antimicrobial spectrum and the basic phase of chloramphenicol
Seemingly.Meanwhile, it is also a kind of powerful immunodepressant, and this effect is stronger than chloramphenicol 6 times, is mainly synthesized with suppression protein
It is relevant with antibody generation is suppressed.China started to try out in 1971, but due to its poorly water-soluble, formulation is restricted.It is domestic
There are many families in the enterprise of current production and sales Thiamphenicol preparation, but due to previous reasons, at present clinically widely used MSM
Mycin preparation is solid pharmaceutical preparation, such as tablet and capsule.
Thiamphenicol is the congener of chloramphenicol, and antimicrobial spectrum and antibacterial action are similar with chloramphenicol, has broad spectrum antimicrobial
Effect, including aerobic gram-negative bacteria and gram positive bacteria, anaerobic bacteria, rickettsiae, conveyor screw and chlamydiaceae.MSM is mould
Element has bactericidal action to following bacterium：Haemophilus influenzae, streptococcus pneumonia and Neisseria meningitidis.Only has suppression to following bacterium
Bacterium acts on：Staphylococcus aureus, micrococcus scarlatinae, Streptococcus viridans, B groups hemolytic streptococcus, EHEC, lung
The anaerobic bacterias such as scorching klebsiella, proteus mirabilis, Salmonella typhi, bacillus paratyphosus, Shigella and bacteroides fragilis.
Following bacterium is generally to chloramphenicol resistance：Pseudomonas aeruginosa, acinetobacter, Enterobacter, serratia marcesens, indole-positive
Proteus, methicillin-resistant Staphylococci and enterococcus spp.
Thiamphenicol it is water-soluble very poor, so at present, Thiamphenicol all simply sheet and glue are being used in clinical test
Capsule, and the stability of Thiamphenicol is very poor, and product is difficult the real quality of output, at present, neither one when processing
The function of the kit without reduction pressure of the Thiamphenicol of the method for detection Thiamphenicol, and carrying well, so as to lead
Medicine inside causing is damaged, therefore invention a kind of reasonable and effective detection method and kit, is imperative.
The content of the invention
（One）The technical problem of solution
In view of the shortcomings of the prior art, the invention provides a kind of Thiamphenicol detection method and kit, possesses effective inspection
Survey Thiamphenicol and the advantages of avoid kit from suffering oppression, solve can not be good detection Thiamphenicol and reduce kit
The problem that interior medicine is damaged.
（Two）Technical scheme
To realize above-mentioned effective detection Thiamphenicol and avoiding kit from suffering oppression purpose, the present invention provides following technical side
Case：A kind of Thiamphenicol detection method, mobile phase uses dimethylformamide, methyl alcohol, biphosphate in high performance liquid chromatography
The mixed solution of potassium solution, silver nitrate solution and ethyl acetate.
Preferably, the ratio of the dimethylformamide-methanol-ethyl acetate is 34：60：20.
Preferably, the ratio of the dimethylformamide-methyl alcohol-silver nitrate solution is 25：70：15.
Preferably, the dimethylformamide-methyl alcohol-potassium dihydrogen phosphate ratio is 40：50：70.
Another technical problem to be solved by the present invention is that a kind of Thiamphenicol detection method is provided, about the detection side of material
Method is as follows：
High effective liquid chromatography for measuring：
1）The mould sample of MSM is taken, precision weighing is carried out, dimethylformamide-methyl alcohol-potassium dihydrogen phosphate is subsequently adding（40：
50：70）Dissolved, and lysate is quantitatively diluted to does not have the solution containing 0.9mg in 1ml, then precision is measured 1ml,
Measure 100ml to be placed into reagent bottle, the solution of 100ml is shaken up for comparison liquid.
2）The step of taking out 5mg 1）Solution, solution is dripped on reaction plate, and takes out acetate-methanol ratio and be
90:5 used as solvent, after the completion of launched and dried, be then placed into being inspected under ultraviolet lamp, then observe ultraviolet
The color of the solution under light lamp and step 1）In comparison liquid color it is whether identical.
3）Take out step 1）Contrast solution and step 2）Each 10mg of reference substance solution, carry out precision weighing, weighed
Cheng Hou, is then injected separately into liquid chromatograph, is analyzed detection.
4）Contrast solution 10mg is taken out, precision weighing is carried out, dimethylformamide-methyl alcohol-silver nitrate solution is subsequently adding
Its ratio is 25：70：15, reaction vessel is subsequently adding, the stirring of three minutes is carried out by the stirring rod that heat is 50 degree, so
The color and fusion degree of solution are observed afterwards, potassium dihydrogen phosphate 5mg is added into reaction bulb again after the completion of observation, carrying out two
The stirring of minute, observes the color of its reaction.
A kind of Thiamphenicol kit, including main cartridge, the bottom of the main cartridge inwall loose with interior clamp, institute
State and fixing hole is offered on interior clamp, the opposite side of the interior clamp and main cartridge has been fixedly connected with decompression cystosepiment, and two
The opposite side of individual decompression cystosepiment is fixedly connected with the two ends of relief spring, is flexibly connected on the inwall of the main cartridge limited
Position plate, offers the spacing hole corresponding with fixing hole on the limiting plate.
（Three）Beneficial effect
Compared with prior art, the invention provides a kind of Thiamphenicol detection method and kit, possess following beneficial
Effect：
1st, a kind of Thiamphenicol detection method and kit, effectively can detect to Thiamphenicol, can be mould to MSM
The water solubility of element detects effective data, while can also effective detection be made to the stability of Thiamphenicol, so that
Thiamphenicol makes the product can be with the real quality of output when processing.
2nd, a kind of Thiamphenicol detection method and kit, by the cystosepiment that depressurizes, relief spring, limiting plate and spacing
The setting in hole, makes reagent bottle when main cartridge is placed into, and will not be squeezed and broken, so as to avoid the situation of medicine damage.
Brief description of the drawings
Fig. 1 is a kind of Thiamphenicol detection method proposed by the present invention and kit cross-sectional view.
In figure：1 main cartridge, clamp, 3 fixing holes, 4 decompression cystosepiments, 5 relief springs, 6 limiting plates, 7 spacing holes in 2.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Refer to Fig. 1, a kind of Thiamphenicol detection method, mobile phase uses dimethyl formyl in high performance liquid chromatography
The mixed solution of amine, methyl alcohol, potassium dihydrogen phosphate, silver nitrate solution and ethyl acetate.Dimethylformamide-methanol-acetic acid
The ratio of ethyl ester is 34：60：20, the ratio of dimethylformamide-methyl alcohol-silver nitrate solution is 25：70：15, dimethyl formyl
Amine-methyl alcohol-potassium dihydrogen phosphate ratio is 40：50：70.
Another technical problem to be solved by the present invention is that a kind of Thiamphenicol detection method is provided, about the detection side of material
Method is as follows：
High effective liquid chromatography for measuring：
1）The mould sample of MSM is taken, precision weighing is carried out, dimethylformamide-methyl alcohol-potassium dihydrogen phosphate is subsequently adding（40：
50：70）Dissolved, and lysate is quantitatively diluted to does not have the solution containing 0.9mg in 1ml, then precision is measured 1ml,
Measure 100ml to be placed into reagent bottle, the solution of 100ml is shaken up for comparison liquid.
2）The step of taking out 5mg 1）Solution, solution is dripped on reaction plate, and takes out acetate-methanol ratio and be
90:5 used as solvent, after the completion of launched and dried, be then placed into being inspected under ultraviolet lamp, then observe ultraviolet
The color of the solution under light lamp and step 1）In comparison liquid color it is whether identical.
3）Take out step 1）Contrast solution and step 2）Each 10mg of reference substance solution, carry out precision weighing, weighed
Cheng Hou, is then injected separately into liquid chromatograph, is analyzed detection.
4）Contrast solution 10mg is taken out, precision weighing is carried out, dimethylformamide-methyl alcohol-silver nitrate solution is subsequently adding
Its ratio is 25：70：15, reaction vessel is subsequently adding, the stirring of three minutes is carried out by the stirring rod that heat is 50 degree, so
The color and fusion degree of solution are observed afterwards, potassium dihydrogen phosphate 5mg is added into reaction bulb again after the completion of observation, carrying out two
The stirring of minute, observes the color of its reaction.
A kind of Thiamphenicol kit, including main cartridge 1, the bottom of the inwall of main cartridge 1 loose with interior clamp 2, lead to
The setting of clamp 2 is crossed, reagent bottle is preferably placed, it is to avoid the problem of reagent bottle run-off the straight, on interior clamp 2
Fixing hole 3 is offered, by the setting of fixing hole 3, reagent bottle is limited to certain position, it is to avoid to shake.
The opposite side of interior clamp 2 and main cartridge 1 has been fixedly connected with decompression cystosepiment 4, and two phases of decompression cystosepiment 4
Two ends of the offside with relief spring 5 are fixedly connected, and by the setting of depressurize cystosepiment 4 and relief spring 5, are receiving kit
Can preferably be depressurized when extruding, it is to avoid kit is oppressed and causes the damaged situation of reagent bottle, is led
Limiting plate 6 is connected with the inwall of box body 1, the spacing hole 7 corresponding with fixing hole 3 is offered on limiting plate 6.
In sum, a kind of Thiamphenicol detection method and kit, effectively can detect, energy to Thiamphenicol
Enough water solubilitys to Thiamphenicol detect effective data, while effective inspection also can be made to the stability of Thiamphenicol
Survey, so that Thiamphenicol is when processing, make the product can be with the real quality of output, by the cystosepiment 4 that depressurizes, decompression bullet
The setting of spring 5, limiting plate 6 and spacing hole 7, makes reagent bottle when main cartridge 1 is placed into, and will not be squeezed and broken, so as to avoid
The situation that medicine is damaged.
It should be noted that herein, such as first and second or the like relational terms are used merely to a reality
Body or operation make a distinction with another entity or operation, and not necessarily require or imply these entities or deposited between operating
In any this actual relation or order.And, term " including ", "comprising" or its any other variant be intended to
Nonexcludability is included, so that process, method, article or equipment including a series of key elements not only will including those
Element, but also other key elements including being not expressly set out, or also include being this process, method, article or equipment
Intrinsic key element.In the absence of more restrictions, the key element limited by sentence "including a ...", it is not excluded that
Also there is other identical element in process, method, article or equipment including the key element.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding can carry out various changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (6)
1. a kind of Thiamphenicol detection method, it is characterised in that in high performance liquid chromatography mobile phase using dimethylformamide,
The mixed solution of methyl alcohol, potassium dihydrogen phosphate, silver nitrate solution and ethyl acetate.
2. a kind of Thiamphenicol detection method according to claim 1, it is characterised in that the dimethylformamide-first
The ratio of alcohol-ethyl acetate is 34：60：20.
3. a kind of Thiamphenicol detection method according to claim 1, it is characterised in that the dimethylformamide-first
The ratio of alcohol-silver nitrate solution is 25：70：15.
4. a kind of Thiamphenicol detection method according to claim 1, it is characterised in that the dimethylformamide-first
Alcohol-potassium dihydrogen phosphate ratio is 40：50：70.
5. a kind of Thiamphenicol detection method, it is characterised in that the detection method about material is as follows：
High effective liquid chromatography for measuring：
The mould sample of MSM is taken, precision weighing is carried out, dimethylformamide-methyl alcohol-potassium dihydrogen phosphate is subsequently adding（40：50：
70）Dissolved, and lysate is quantitatively diluted to does not have the solution containing 0.9mg in 1ml, then precision is measured 1ml, is being measured
100ml is placed into reagent bottle, and the solution of 100ml is shaken up for comparison liquid；
The step of taking out 5mg 1）Solution, solution is dripped on reaction plate, and it is 90 to take out acetate-methanol ratio:5 make
Be solvent, after the completion of launched and dried, be then placed into being inspected under ultraviolet lamp, then observe under ultraviolet lamp
Solution color and step 1）In comparison liquid color it is whether identical；
3）Take out step 1）Contrast solution and step 2）Each 10mg of reference substance solution, carry out precision weighing, after the completion of weighing,
Then liquid chromatograph is injected separately into, detection is analyzed；
4）Contrast solution 10mg is taken out, precision weighing is carried out, it compares to be subsequently adding dimethylformamide-methyl alcohol-silver nitrate solution
Example is 25：70：15, reaction vessel is subsequently adding, the stirring of three minutes, Ran Houguan are carried out by the stirring rod that heat is 50 degree
The color and fusion degree of solution are examined, potassium dihydrogen phosphate 5mg is added into reaction bulb again after the completion of observation, carried out two minutes
Stirring, observe its reaction color.
6. a kind of Thiamphenicol kit, including main cartridge（1）, it is characterised in that：The main cartridge（1）The bottom activity of inwall
There is interior clamp（2）, the interior clamp（2）On offer fixing hole（3）, the interior clamp（2）And main cartridge（1）It is relative
Side has been fixedly connected with decompression cystosepiment（4）, and two decompression cystosepiments（4）Opposite side and relief spring（5）Two ends
It is fixedly connected, the main cartridge（1）Inwall on be connected with limiting plate（6）, the limiting plate（6）On offer and fixation
Hole（3）Corresponding spacing hole（7）.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611112562.0A CN106706780A (en) | 2016-12-07 | 2016-12-07 | Detection method for thiamphenicol and kit |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611112562.0A CN106706780A (en) | 2016-12-07 | 2016-12-07 | Detection method for thiamphenicol and kit |
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| Publication Number | Publication Date |
|---|---|
| CN106706780A true CN106706780A (en) | 2017-05-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611112562.0A Pending CN106706780A (en) | 2016-12-07 | 2016-12-07 | Detection method for thiamphenicol and kit |
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| Country | Link |
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| CN (1) | CN106706780A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107843678A (en) * | 2017-12-06 | 2018-03-27 | 武汉生物工程学院 | A kind of method of Thiamphenicol content in thin-layer chromatography combined highly effective liquid chromatographic detection animal feed |
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2016
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| CN2238801Y (en) * | 1995-11-02 | 1996-10-30 | 王建阳 | Packing box for oral dysentery vaccine |
| CN203648477U (en) * | 2013-12-31 | 2014-06-18 | 上海碧云天生物技术有限公司 | Gel preparation kit |
| CN204676082U (en) * | 2015-05-18 | 2015-09-30 | 王军富 | Microbial detection reagent kit |
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| 国家药典委员会: "《中华人民共和国药典 2010年版 2部》", 31 January 2010, 北京：中国医药科技出版社 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107843678A (en) * | 2017-12-06 | 2018-03-27 | 武汉生物工程学院 | A kind of method of Thiamphenicol content in thin-layer chromatography combined highly effective liquid chromatographic detection animal feed |
| CN107843678B (en) * | 2017-12-06 | 2020-04-14 | 武汉生物工程学院 | Method for detecting content of thiamphenicol in animal feed by combining thin-layer chromatography with high performance liquid chromatography |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170524 |
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| RJ01 | Rejection of invention patent application after publication |