CN107389807A - A kind of assay method of the carboxylic acid concentration of L thiazolidines 4 - Google Patents
A kind of assay method of the carboxylic acid concentration of L thiazolidines 4 Download PDFInfo
- Publication number
- CN107389807A CN107389807A CN201710432935.0A CN201710432935A CN107389807A CN 107389807 A CN107389807 A CN 107389807A CN 201710432935 A CN201710432935 A CN 201710432935A CN 107389807 A CN107389807 A CN 107389807A
- Authority
- CN
- China
- Prior art keywords
- sample
- measure
- standard
- thiazolidines
- carboxylic acid
- 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.)
- Pending
Links
Classifications
-
- 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
- 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
Landscapes
- 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 Analysing Biological Materials (AREA)
Abstract
The invention discloses a kind of assay method of the carboxylic acid concentration of L thiazolidines 4, including the preparation of sample collection, sample treatment, standard liquid and measure, the making of standard curve and measure；The gas phase condition of gas chromatograph is arranged to use HP INWWAX capillary chromatographic columns in the determination step, and column temperature is 115 degree, and temperature of vaporization chamber is 167 degree, and detection room temperature is 234 degree, carrier gas flux 12ml/min.Result detection data of the present invention are accurate, meet national requirements, time-saving and efficiency, preparation for standard liquid, using the method after the improvement of the present invention, the usage amount of standard liquid is reduced, for ensureing that the preci-sion and accuracy of sample measure serves good facilitation.
Description
Technical field
Present invention relates particularly to a kind of assay method of L- thiazolidines -4- carboxylic acid concentrations.
Background technology
Pidotimod is the Immunopromoter developed by Italian Poli chemical industrial companies, can be promoted non-specific
Property immune response, and can promote specific immune response；It is mainly used in preventing and treating children's recurrent respiratory infection, uropoiesis
System infections, allergic rhinitis and asthma, it may also be used for have caused by a variety of virus infection, malignant tumour and other chronic diseases
Body's immunity is low.
L- thiazolidinyl -4- carboxylic acids are the important intermediates for synthesizing Pidotimod, up to the present, are not yet recorded in document
The analyzing detecting method of L- thiazolidinyl -4- carboxylic acids, but the analysis of L- thiazolidinyl -4- carboxylic acids is detected to reaction controlling and yield
Raising plays the role of quality that is important, while also directly affecting finished product Pidotimod, so it is effective to establish a kind of stabilization
Analyzing detecting method to L- thiazolidinyl -4- carboxylic acids carry out quality control be very important.
The content of the invention
Goal of the invention：In order to solve the deficiencies in the prior art, the invention provides a kind of L- thiazolidines -4- carboxylic acid concentrations'
Assay method.
Technical scheme：A kind of assay method of L- thiazolidines -4- carboxylic acid concentrations, including sample collection, sample treatment, standard
The preparation of solution and measure, the making of standard curve and measure；Wherein：
The standard liquid is formulated as accurately weighing 0.18g L- thiazolidine -4- carboxylic acids in 10ml volumetric flasks, adds solution
Imbibition constant volume, dense standard liquid is configured to, draws 0,10,20,30, the 40 and 50 dense standard liquids of μ l respectively and parsed in 1ml in bottle, is made into successively
0th, 146,292,436,581 and 727 μ g/ml standard series；
The gas phase condition of gas chromatograph is arranged to use HP-INWWAX capillary chromatographic columns, post in the determination step
Temperature is 115 degree, and temperature of vaporization chamber is 167 degree, and detection room temperature is 234 degree, carrier gas flux 12ml/min.
As optimization：The sample collection includes short time sampling, sampling, personal sampling and blank sample are adopted for a long time
Sample；The short time is sampled as, in sampled point, silicone tube or activated carbon tube both ends being opened, with 220mL/min flow collections 18min
Air sample；The long-time is sampled as, in sampled point, silicone tube both ends being opened, with 50mL/min flow collection 1~3h air
Sample；The personal sampling is in sampled point, opens silicone tube both ends, is worn on the shirtfront top of sample objects, approaches as far as possible
Breathing zone, with 50mL/min flow collection 1~3h air samples；The blank sample is sampled as bringing silicone tube to sampled point,
In addition to samplers sample air sample is not connected to, remaining operates same sample.
As optimization：The sample handling procedure is to pour into the front and rear section silica gel for adopting sample in solvent desorption bottle respectively,
1ml stripping liquid acetic acid is added, after closing, shakes 1min, desorbs 40min, stripping liquid is for measure.
As optimization：The Specification Curve of Increasing step is conditioning instrumentation operating condition, under insulation, sample introduction 0.1ml, is surveyed
Fixed each standard series, each concentration replication 3 times, it is bent to draw standard with peak height or peak area average to corresponding formic acid concn
Line.
As optimization：The determination step includes sample measure and reference substance measure；It is empty that the reference substance is determined as measure
White control stripping liquid, obtains peak height or peak area value；The sample is determined as determines sample with the similarity condition of bioassay standard series
Product stripping liquid, after the sample peak height or peak area value measured subtracts blank control peak height or peak area value, sample is obtained by standard curve
The concentration of formic acid in product.
Beneficial effect：Result detection data of the present invention are accurate, meet national requirements, time-saving and efficiency, for standard liquid
Prepare, using the method after the improvement of the present invention, the usage amount of standard liquid is reduced, the precision for ensureing sample measure
Good facilitation is served with the degree of accuracy.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, so that the technology of this area
Personnel can be better understood from advantages and features of the invention, so as to make apparent boundary to protection scope of the present invention
It is fixed.Embodiment described in the invention is only part of the embodiment of the present invention, rather than whole embodiments, based on the present invention
In embodiment, the every other implementation that those of ordinary skill in the art are obtained on the premise of creative work is not made
Example, belongs to the scope of protection of the invention.
Embodiment
A kind of assay method of L- thiazolidines -4- carboxylic acid concentrations, including sample collection, sample treatment, standard liquid are matched somebody with somebody
System and measure, the making of standard curve and measure；Wherein：
The standard liquid is formulated as accurately weighing 0.18g L- thiazolidine -4- carboxylic acids in 10ml volumetric flasks, adds solution
Imbibition constant volume, dense standard liquid is configured to, draws 0,10,20,30, the 40 and 50 dense standard liquids of μ l respectively and parsed in 1ml in bottle, is made into successively
0th, 146,292,436,581 and 727 μ g/ml standard series；
The gas phase condition of gas chromatograph is arranged to use HP-INWWAX capillary chromatographic columns, post in the determination step
Temperature is 115 degree, and temperature of vaporization chamber is 167 degree, and detection room temperature is 234 degree, carrier gas flux 12ml/min.
The sample collection includes short time sampling, for a long time sampling, personal sampling and blank sample sampling；It is described in short-term
Between be sampled as in sampled point, silicone tube or activated carbon tube both ends are opened, with 220mL/min flow collection 18min air samples；Institute
State and be sampled as, in sampled point, silicone tube both ends being opened, with 50mL/min flow collection 1~3h air samples for a long time；Described
Sampler body is in sampled point, opens silicone tube both ends, is worn on the shirtfront top of sample objects, as far as possible close to breathing zone, with
50mL/min flow collection 1~3h air samples；The blank sample is sampled as bringing silicone tube to sampled point, except being not connected to adopt
Outside sample device collection air sample, remaining operates same sample.
The sample handling procedure adds 1ml solutions for the front and rear section silica gel for adopting sample is poured into solvent desorption bottle respectively
Imbibition acetic acid, after closing, 1min is shaken, desorb 40min, stripping liquid is for measure.
The Specification Curve of Increasing step is conditioning instrumentation operating condition, under insulation, sample introduction 0.1ml, determines each standard
Series, each concentration replication 3 times, standard curve is drawn to corresponding formic acid concn with peak height or peak area average.
The determination step includes sample measure and reference substance measure；The reference substance is determined as measure blank control desorption
Liquid, obtain peak height or peak area value；The sample is determined as the similarity condition determination sample stripping liquid with bioassay standard series, surveys
Sample peak height or peak area value subtract blank control peak height or peak area value after, the dense of formic acid in sample is obtained by standard curve
Degree.
Result detection data of the present invention are accurate, meet national requirements, time-saving and efficiency, the preparation for standard liquid, use
Method after the improvement of the present invention, the usage amount of standard liquid is reduced, the preci-sion and accuracy for ensureing sample measure
Serve good facilitation.
Claims (5)
- A kind of 1. assay method of L- thiazolidines -4- carboxylic acid concentrations, it is characterised in that：Including sample collection, sample treatment, standard The preparation of solution and measure, the making of standard curve and measure；Wherein：The standard liquid is formulated as accurately weighing 0.18g L- thiazolidine -4- carboxylic acids in 10ml volumetric flasks, adds stripping liquid Constant volume, dense standard liquid is configured to, draws 0,10,20,30, the 40 and 50 dense standard liquids of μ l respectively and parsed in 1ml in bottle, be made into 0 successively, 146th, 292,436,581 and 727 μ g/ml standard series；The gas phase condition of gas chromatograph is arranged to use HP-INWWAX capillary chromatographic columns in the determination step, and column temperature is 115 degree, temperature of vaporization chamber is 167 degree, and detection room temperature is 234 degree, carrier gas flux 12ml/min.
- 2. the assay method of L- thiazolidines -4- carboxylic acid concentrations according to claim 1, it is characterised in that：The sample is adopted Collection includes short time sampling, for a long time sampling, personal sampling and blank sample sampling；The short time is sampled as in sampled point, Silicone tube or activated carbon tube both ends are opened, with 220mL/min flow collection 18min air samples；The long-time is sampled as Sampled point, silicone tube both ends are opened, with 50mL/min flow collection 1~3h air samples；The personal sampling be in sampled point, Open silicone tube both ends, be worn on the shirtfront top of sample objects, as far as possible close to breathing zone, with 50mL/min flow collections 1~ 3h air samples；The blank sample is sampled as bringing silicone tube to sampled point, in addition to samplers sample air sample is not connected to, Remaining operates same sample.
- 3. the assay method of L- thiazolidines -4- carboxylic acid concentrations according to claim 1, it is characterised in that：At the sample Reason step adds 1ml stripping liquid acetic acid, after closing, shaken for the front and rear section silica gel for adopting sample is poured into solvent desorption bottle respectively 1min is shaken, desorbs 40min, stripping liquid is for measure.
- 4. the assay method of L- thiazolidines -4- carboxylic acid concentrations according to claim 1, it is characterised in that：The standard is bent Line plot step is conditioning instrumentation operating condition, and under insulation, sample introduction 0.1ml determines each standard series, and each concentration repeats to survey It is fixed 3 times, standard curve is drawn to corresponding formic acid concn with peak height or peak area average.
- 5. the assay method of L- thiazolidines -4- carboxylic acid concentrations according to claim 1, it is characterised in that：The measure step Suddenly sample measure and reference substance measure are included；The reference substance is determined as measure blank control stripping liquid, obtains peak height or peak face Product value；The sample is determined as the similarity condition determination sample stripping liquid with bioassay standard series, the sample peak height or peak measured After area value subtracts blank control peak height or peak area value, the concentration of formic acid in sample is obtained by standard curve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710432935.0A CN107389807A (en) | 2017-06-09 | 2017-06-09 | A kind of assay method of the carboxylic acid concentration of L thiazolidines 4 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710432935.0A CN107389807A (en) | 2017-06-09 | 2017-06-09 | A kind of assay method of the carboxylic acid concentration of L thiazolidines 4 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107389807A true CN107389807A (en) | 2017-11-24 |
Family
ID=60333290
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710432935.0A Pending CN107389807A (en) | 2017-06-09 | 2017-06-09 | A kind of assay method of the carboxylic acid concentration of L thiazolidines 4 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107389807A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103226142A (en) * | 2012-01-30 | 2013-07-31 | 南京长澳医药科技有限公司 | Method for detecting leucogen concentration in blood plasma |
| CN104655736A (en) * | 2013-11-18 | 2015-05-27 | 山东新时代药业有限公司 | Analysis and detection method of L-thiazolidinyl-4-carboxylic acid |
| CN105467045A (en) * | 2016-01-06 | 2016-04-06 | 福建农林大学 | Method for quickly detecting L-thiazolidine-4-carboxylic acid in lentinula edodes |
-
2017
- 2017-06-09 CN CN201710432935.0A patent/CN107389807A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103226142A (en) * | 2012-01-30 | 2013-07-31 | 南京长澳医药科技有限公司 | Method for detecting leucogen concentration in blood plasma |
| CN104655736A (en) * | 2013-11-18 | 2015-05-27 | 山东新时代药业有限公司 | Analysis and detection method of L-thiazolidinyl-4-carboxylic acid |
| CN105467045A (en) * | 2016-01-06 | 2016-04-06 | 福建农林大学 | Method for quickly detecting L-thiazolidine-4-carboxylic acid in lentinula edodes |
Non-Patent Citations (1)
| Title |
|---|
| HO-SANG SHIN 等: "Determination of thiazolidine-4-carboxylates in urine by chloroformate derivatization and gas chromatography-electron impact mass spectrometry", 《JOURNAL OF MASS SPECTROMETRY》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103713056B (en) | Method for simultaneously analyzing and detecting residual veterinary drug compositions in animal tissue | |
| CN101647829B (en) | Quality control method of ginkgolide injection | |
| CN105181853A (en) | Method for determining ethanol and isopropyl benzene contents of air and waste gas | |
| CN103454369A (en) | Method for detecting sodium valproate content of blood through high performance liquid chromatography | |
| CN103743843A (en) | Method for detecting chloroacetic acid in air in workplace | |
| CN104569194A (en) | Ion chromatographic measurement method for ammonia content in flue gas of electronic cigarette | |
| CN104122349B (en) | Cr (III) and Cr (VI) extraction and isolation and analytical approach in a kind of cigarette smoke | |
| CN204214826U (en) | A kind of aflatoxin B1 immune affinity column | |
| CN110057959A (en) | A kind of analysis method of the high effective liquid chromatography for measuring Febustat intermediate in relation to substance | |
| CN109632997A (en) | The extraction and measuring method of regallity glycosides B in a kind of lily medicinal material | |
| CN107389807A (en) | A kind of assay method of the carboxylic acid concentration of L thiazolidines 4 | |
| CN106338559B (en) | A kind of gas-chromatography detection method of chlorine disinfection by-product dichloro acetamide | |
| CN110487927A (en) | The measuring method of methanol in a kind of exhaust of solid pollution source | |
| CN104634904B (en) | Concentration of aniline assay method in a kind of workplace aromatic amine | |
| CN103884789B (en) | Method for rapidly determining polysaccharide peptide in lucid ganoderma product | |
| CN102636582B (en) | Method for determining content of diminazene and antipyrine in diminazene particle | |
| CN104764826A (en) | Method for determining content of cotinine in urine | |
| CN104569174A (en) | Method for determining concentration of formic acid in carboxylic acids in working place | |
| Liu et al. | On-site solid phase extraction and HPLC determination of chloramphenicol in surface water and sewage | |
| Hurst et al. | Determination of clovoxamine concentration in human plasma by electron capture gas chromatography. | |
| CN111579684B (en) | Method for measuring content of total capsaicin in capsule wall material of capsule | |
| CN114113409A (en) | High performance liquid chromatography detection method for berberine intermediate | |
| CN104569245A (en) | Method for measuring concentration of cyclohexylamine in aliphatic amines of workplace | |
| CN104569250A (en) | Method for determining concentration of pyridine in heterocyclic compound of workplace | |
| CN104764812A (en) | Detection method for determining alcohol compounds through gas chromatography |
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 | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 226000 Third Floor, Science and Technology Venture Center, No. 52 Central Road, Nantong Development Zone, Jiangsu Province Applicant after: Jiangsu tajie testing technology Limited by Share Ltd Address before: 226000 Third Floor, Science and Technology Venture Center, No. 52 Central Road, Nantong Development Zone, Jiangsu Province Applicant before: Jiangsu Taijie Inspection Technology Co., Ltd. |
|
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171124 |