CN108107125A - A kind of content assaying method of Beta-methyl monomethyl glutarate - Google Patents
A kind of content assaying method of Beta-methyl monomethyl glutarate Download PDFInfo
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- CN108107125A CN108107125A CN201711353439.2A CN201711353439A CN108107125A CN 108107125 A CN108107125 A CN 108107125A CN 201711353439 A CN201711353439 A CN 201711353439A CN 108107125 A CN108107125 A CN 108107125A
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- beta
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- monomethyl glutarate
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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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
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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Abstract
The invention discloses a kind of content assaying methods of β methylglutaric acids mono-methyl, and using gas chromatograph, content is calculated with external standard method.By the assay method of the present invention, the content of β methylglutaric acid mono-methyls can be accurately measured, excludes the influence of a variety of acidic materials such as β methylglutaric acids in sample, specificity is strong, and error is small.
Description
Technical field
The present invention relates to a kind of content assaying method of Beta-methyl monomethyl glutarate.
Background technology
Beta-methyl monomethyl glutarate, the entitled Monomethyl β-methylglutarate of English, molecular formula are
C7H12O4, molecular weight 160.1678, CAS registration numbers are 27151-65-1, for organic synthesis.In the prior art, Beta-methyl
The assay method of monomethyl glutarate is：Precision weighs 0.2g samples, is dissolved with 10ml neutral alcohols, using 1% phenolphthalein as instruction
Liquid is titrated to pink with 0.1mol/L NaOH titrating solutions.
Content=(C drops × V drop × 0.16)/G × 100%
The concentration (mol/L) of C drops --- -- NaOH titrating solutions
V drops --- -- consume the volume (ml) of NaOH titrating solutions
G----- sample qualities (g)
The content 95.00~100.00% of Beta-methyl monomethyl glutarate is qualification.
Using more than assay method, cannot judge containing a variety of acidic materials such as Beta-methyl glutaric acids in sample, it should
Method specificity is not strong, and assay result is inaccurate.In addition it is big using titration, error by hand.
How using a kind of content assaying method of new Beta-methyl monomethyl glutarate, improve and measure accuracy, reduce
Error is the technical problem to be solved in the invention.
The content of the invention
The present invention provides a kind of assay side of Beta-methyl monomethyl glutarate aiming at above-mentioned defect
Method.By the assay method of the present invention, the content of Beta-methyl monomethyl glutarate can be accurately measured, excludes Beta-methyl in sample
The influence of a variety of acidic materials such as glutaric acid, specificity is strong, and error is small.
A kind of content assaying method technical solution of Beta-methyl monomethyl glutarate of the present invention is, using gas-chromatography
Instrument calculates content with external standard method.
The gas chromatograph is furnished with shunting/non split stream injector, controlled sequence heating post case, hydrogen flame detector；
High pure nitrogen 99.9999% is carrier gas；Hydrogen, air are auxiliary gas.
Chromatographic column is that capillary column its specification is 50m*0.32mm*0.25 μm, and interior painting stationary phase is SE-54.
GC conditions：Detector temperature：260 DEG C, gasify room temperature：240 DEG C, column temperature：100 DEG C, constant temperature 1min, with
The speed of 10 DEG C/min rises to 200 DEG C, then rises to 250 DEG C with the speed of 5 DEG C/min, nebulizer gas pressure：0.06Mpa.
Precision measures 200 μ l of standard items, puts in 1ml measuring bottles, ethanol solution is added to be diluted to scale, shake up, and filters；With
Sample introduction needle takes above-mentioned 0.2 μ L of solution injections gas chromatograph, records chromatogram；Precision measures 200 μ l of sample, puts in 1ml measuring bottles,
Ethanol solution is added to be diluted to scale, is shaken up, is filtered；Above-mentioned 0.2 μ L of solution injections gas chromatograph, record are taken with sample introduction needle
Chromatogram calculates content with external standard method；
Formula：ωSample=ωMark*ASample/AMark
In formula：ωMarkThe percentage composition of Beta-methyl monomethyl glutarate in-standard substance
ASampleThe average peak area of Beta-methyl monomethyl glutarate in-sample
AMarkThe average peak area of Beta-methyl monomethyl glutarate in-standard substance.
Beneficial effects of the present invention are：By the assay method of the present invention, Beta-methyl glutaric acid list first can be accurately measured
The content of ester excludes the influence of a variety of acidic materials such as Beta-methyl glutaric acid in sample, and specificity is strong, and error is small.
Description of the drawings：
Fig. 1 show standard items collection of illustrative plates 1；
Fig. 2 show standard items collection of illustrative plates 2；
It is sample collection of illustrative plates 1 described in Fig. 3；
Fig. 4 show sample collection of illustrative plates 2.
Specific embodiment：
For a better understanding of the present invention, below with specific example come the technical solution that the present invention will be described in detail, but this
Invention is not limited thereto.
Embodiment 1
Assay：Detect the content of Beta-methyl monomethyl glutarate in sample
1st, instrument：Good fortune founds gas chromatograph, equipped with shunting/non split stream injector, controlled sequence heating post case, hydrogen flame inspection
Survey device；High pure nitrogen 99.9999% is carrier gas；Hydrogen, air are auxiliary gas；It is equipped with corresponding chromatographic work station；Chromatographic column is hair
Its specification of capillary column is 50m*0.32mm*0.25 μm, and interior painting stationary phase is SE-54.
2nd, reagent：
Absolute ethyl alcohol (analysis is pure) dilution
3rd, GC conditions：Detector temperature：260 DEG C, gasify room temperature：240 DEG C, column temperature：100 DEG C, constant temperature 1min,
200 DEG C are risen to the speed of 10 DEG C/min, then rises to 250 DEG C with the speed of 5 DEG C/min, nebulizer gas pressure：0.06Mpa.
4th, assay method
4.1 standard items are prepared：Precision measures 200 μ l of standard items, puts in 1ml volumetric flasks, ethanol solution is added to be diluted to
Scale shakes up, filtering.
With sample introduction needle above-mentioned 0.2 μ L of solution injections good fortune is taken to found gas chromatograph, record chromatogram, it is parallel to be illustrated twice
Book attached drawing standard items collection of illustrative plates 1 shown in FIG. 1 and standard items collection of illustrative plates 2 shown in Fig. 2.
4.2 sample preparation：Precision measures 200 μ l of sample, puts in 1ml measuring bottles, ethanol solution is added to be diluted to scale, shake
It is even, filtering.
With sample introduction needle above-mentioned 0.2 μ L of solution injection good fortune is taken to found gas chromatograph, records chromatogram, it is parallel twice, said
Bright book attached drawing sample collection of illustrative plates 1 shown in Fig. 3 and sample collection of illustrative plates 2 shown in Fig. 4.Content is calculated with external standard method.
Formula：ωSample=ωMark*ASample/AMark
In formula：ωMark--- the percentage composition of Beta-methyl monomethyl glutarate in standard substance
ASample--- the average peak area of Beta-methyl monomethyl glutarate in sample
AMark--- the average peak area of Beta-methyl monomethyl glutarate in standard substance.
Claims (5)
1. a kind of content assaying method of Beta-methyl monomethyl glutarate, which is characterized in that using gas chromatograph, use external standard method
Calculate content.
2. the content assaying method of a kind of Beta-methyl monomethyl glutarate according to claim 1, which is characterized in that described
Gas chromatograph equipped with shunting/non split stream injector, controlled sequence heating post case, hydrogen flame detector；High pure nitrogen
99.9999% is carrier gas；Hydrogen, air are auxiliary gas.
A kind of 3. content assaying method of Beta-methyl monomethyl glutarate according to claim 1, which is characterized in that chromatography
Column is that capillary column its specification is 50m*0.32mm*0.25 μm, and interior painting stationary phase is SE-54.
A kind of 4. content assaying method of Beta-methyl monomethyl glutarate according to claim 1, which is characterized in that gas phase
Chromatographic condition：Detector temperature：260 DEG C, gasify room temperature：240 DEG C, column temperature：100 DEG C, constant temperature 1min, with the speed of 10 DEG C/min
Degree rises to 200 DEG C, then rises to 250 DEG C with the speed of 5 DEG C/min, nebulizer gas pressure：0.06Mpa.
5. the content assaying method of a kind of Beta-methyl monomethyl glutarate according to claim 1, which is characterized in that accurate
200 μ l of sample are measured, puts in 1ml measuring bottles, ethanol solution is added to be diluted to scale, shake up, are filtered；It is taken with sample introduction needle above-mentioned molten
0.2 μ L of liquid inject gas chromatograph, record chromatogram, and content is calculated with external standard method；
Formula：ωSample=ωMark*ASample/AMark
In formula：ωMarkThe percentage composition of Beta-methyl monomethyl glutarate in-standard substance
ASampleThe average peak area of Beta-methyl monomethyl glutarate in-sample
AMarkThe average peak area of Beta-methyl monomethyl glutarate in-standard substance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711353439.2A CN108107125A (en) | 2017-12-15 | 2017-12-15 | A kind of content assaying method of Beta-methyl monomethyl glutarate |
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| CN201711353439.2A CN108107125A (en) | 2017-12-15 | 2017-12-15 | A kind of content assaying method of Beta-methyl monomethyl glutarate |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003299495A (en) * | 2002-04-10 | 2003-10-21 | Sumitomo Chem Co Ltd | Method for producing optically active monoester of 3- methylglutaric acid |
| JP2016124939A (en) * | 2014-12-26 | 2016-07-11 | 大成化工株式会社 | Polyvinyl chloride-based sheet for medicine packaging |
| CN107337592A (en) * | 2017-07-03 | 2017-11-10 | 辽宁科技学院 | Utilize the method for β methylglutaric acid mono-methyl musk ambrette ketone |
-
2017
- 2017-12-15 CN CN201711353439.2A patent/CN108107125A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003299495A (en) * | 2002-04-10 | 2003-10-21 | Sumitomo Chem Co Ltd | Method for producing optically active monoester of 3- methylglutaric acid |
| JP2016124939A (en) * | 2014-12-26 | 2016-07-11 | 大成化工株式会社 | Polyvinyl chloride-based sheet for medicine packaging |
| CN107337592A (en) * | 2017-07-03 | 2017-11-10 | 辽宁科技学院 | Utilize the method for β methylglutaric acid mono-methyl musk ambrette ketone |
Non-Patent Citations (2)
| Title |
|---|
| SCHAFER W 等: "Multiple-injection high-throughput ga s chromatography analysis", 《J.SEP.SCI》 * |
| 孙志忠 等: "β-甲基戊二酸的合成工艺优化", 《化学研究与应用》 * |
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Application publication date: 20180601 |