CN107300564A - Application of the Dimetridazole as internal standard compound in hydrogen nuclear magnetic resonance technology - Google Patents
Application of the Dimetridazole as internal standard compound in hydrogen nuclear magnetic resonance technology Download PDFInfo
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- CN107300564A CN107300564A CN201710709732.1A CN201710709732A CN107300564A CN 107300564 A CN107300564 A CN 107300564A CN 201710709732 A CN201710709732 A CN 201710709732A CN 107300564 A CN107300564 A CN 107300564A
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- dimetridazole
- internal standard
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
Abstract
Application the invention discloses Dimetridazole as internal standard compound in hydrogen nuclear magnetic resonance technology.Application of the Dimetridazole as internal standard compound in hydrogen nuclear magnetic resonance technology, including it is following 1) at least one of 3)：1) to the structure elucidation of testing compound；2) to the qualitative analysis of testing compound；3) to the quantitative analysis of testing compound.The present invention is using high-purity Dimetridazole as internal standard, and its hydrogen spectrum is simple, quantitative peak wider range, can be dissolved in a variety of deuterated reagents, and have the advantages that traceability.
Description
Technical field
A kind of application the present invention relates to Dimetridazole as internal standard compound in hydrogen nuclear magnetic resonance technology, belongs to analytical chemistry
With stoichiometry field.
Background technology
Dimetridazole alias Dimetridazole, dimetridazole etc., English name：Dimetridazole,CAS：551-92-8.
Molecular formula C5H7N3O2.Relative molecular weight 141.13, is a kind of micro-yellow powder, 138-139 DEG C of fusing point.Be dissolved in chloroform, ethanol,
Diluted alkaline and diluted acid, water insoluble, ether.It is tasteless.Condition of storage：2-8℃.It is livestock and poultry growth accelerator and the efficient, wide spectrum of low toxicity
Antiprotozoal agent.Molecular structural formula is as shown in Equation 1.
Hydrogen nuclear magnetic resonance method have high sensitivity, pinpoint accuracy, it is quick, direct the features such as, be widely used in organising
The structure elucidation of compound and qualitative analysis.In recent years, nuclear magnetic resonance technique is ground in the purity testing of compound, standard substance definite value
Study carefully etc. and to have a clear superiority, it is used for the face that the basis of quantitative analysis is different atomic nucleus resonance absorbing peaks in each chemical environment
Product is directly proportional to produce the nuclear number at respective resonant peak.Therefore, to the measure of purity, it is desirable to have the material of known purity is made
For internal standard.If the internal standard selected is the certified reference material that international unit is traceable to by pedestal method, it is possible to will be tested
The value of thing is directly traced to the source to international unit.Quantitative nuclear-magnetism Par value calculation formula is as follows：
In above formula：PNMRThe purity of-the measured object measured using nuclear magnetic resonance method；
Ix- sample specifies the integral area at peak；
Istd- internal standard compound specifies the integral area at peak；
nstd- internal standard compound specifies the nuclear colony core number at peak；
nx- sample specifies the nuclear colony core number at peak；
MxThe molecular weight of-sample；
MstdThe molecular weight of-internal standard compound；
mstdThe quality of the internal standard compound of-addition；
mxThe sample weighting amount of-sample；
PstdThe purity of-internal standard compound.
The quantitative nuclear-magnetism internal standard species of hydrogen for being presently used for tracing to the source are not enriched.
The content of the invention
Application it is an object of the invention to provide Dimetridazole as internal standard compound in hydrogen nuclear magnetic resonance technology, the present invention is adopted
With high-purity Dimetridazole as internal standard, its hydrogen spectrum is simple, quantitative peak wider range, can be dissolved in a variety of deuterated reagents, and
And there is traceability.
Application of the Dimetridazole that the present invention is provided as internal standard compound in hydrogen nuclear magnetic resonance technology.
Application of the above-mentioned Dimetridazole as internal standard compound in hydrogen nuclear magnetic resonance technology, specifically includes following 1) -3) in
It is at least one：
1) to the structure elucidation of testing compound；
2) to the qualitative analysis of testing compound；
3) to the quantitative analysis of testing compound.
In above-mentioned application, the purity of the Dimetridazole is that 99.8% ± 0.4%, i.e. purity are 99.4~100.2%.
In the present invention, the accurate characteristics value of the Dimetridazole is according to JJF 1006-1994 national standard reference materials
Technical specification, by using accurate definite value, uniformity testing, the technical requirements such as study on the stability are obtained, high-purity in the present invention
Dimetridazole mass fraction is 99.8% ± 0.4%, under conditions of 5mg, the mass fraction characteristic magnitude of Dimetridazole
Uniformly, and the stability of more than 1 year is met.
In above-mentioned application, the applicable solvent of the Dimetridazole is deuterated solvent；
In the deuterated solvent, the chemical shift of the Dimetridazole is 2~8ppm, the feature hydrogen of the Dimetridazole
Peak wider range, can be suitably used for the quantitative study in different IPs magnetic field.
In above-mentioned application, the deuterated solvent includes deuterated methanol, deuterochloroform, deuterated acetonitrile, deuterated acetone, deuterated
At least one of dimethyl sulfoxide (DMSO) (also known as DMSO-D6) and deuterium-oxide.
In above-mentioned application, the Dimetridazole is as internal standard compound in the hydrogen nuclear magnetic resonance quantitative analysis of ethylparaben
Application.
A kind of Dimetridazole is used as the method for the hydrogen nuclear magnetic resonance quantitative analysis of internal standard compound, including following key step：
1) Dimetridazole and the testing compound are dissolved in the deuterated solvent respectively, determine hydrogen nuclear magnetic resonance
Spectrogram, respectively obtains the chemical potential at the chemical shift at the specified peak of the Dimetridazole and the specified peak of the testing compound
Move；
2) Dimetridazole and the testing compound are mixed and are dissolved in the deuterated solvent, determine hydrogen nuclear magnetic resonance
Spectrogram, according to step 1) described in Dimetridazole specified peak chemical shift and the testing compound specified peak chemistry
Displacement, obtains the integral area that Dimetridazole described in system and the testing compound each specify peak；
3) according to the quantitative nuclear-magnetism Par value calculation formula as shown in following formula I, calculate and obtain the testing compound
Purity；
In above formula I：PNMRThe purity of-the measured object measured using nuclear magnetic resonance method；
Ix- testing compound specifies the integral area at peak；
Istd- internal standard compound specifies the integral area at peak；
nstd- internal standard compound specifies the nuclear colony core number at peak；
nx- testing compound specifies the nuclear colony core number at peak；
MxThe molecular weight of-testing compound；
MstdThe molecular weight of-internal standard compound；
mstdThe quality of the internal standard compound of-addition；
mxThe sample weighting amount of-testing compound；
PstdThe purity of-internal standard compound.
The present invention is using high-purity Dimetridazole as internal standard compound, and its hydrogen spectrum is simple, quantitative peak wider range, can dissolve
In a variety of deuterated reagents, and there is traceability, can stably, accurately determine the content of determinand.
Brief description of the drawings
Fig. 1 is hydrogen nuclear magnetic resonance spectrogram of the Dimetridazole in deuterated methanol.
Fig. 2 is hydrogen nuclear magnetic resonance spectrogram of the Dimetridazole in deuterochloroform.
Fig. 3 is hydrogen nuclear magnetic resonance spectrogram of the Dimetridazole in deuterated acetonitrile.
Fig. 4 is hydrogen nuclear magnetic resonance spectrogram of the Dimetridazole in deuterated acetone.
Fig. 5 is hydrogen nuclear magnetic resonance spectrogram of the Dimetridazole in DMSO-D6.
Fig. 6 is hydrogen nuclear magnetic resonance spectrogram of the Dimetridazole in deuterium-oxide.
Fig. 7 is the hydrogen nuclear magnetic resonance spectrogram of Dimetridazole and ethylparaben in deuterochloroform.
Fig. 8 is hydrogen nuclear magnetic resonance spectrogram of the ethylparaben in deuterochloroform.
Embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
Material, reagent used etc., unless otherwise specified, are commercially obtained in following embodiments.
The application of embodiment 1, Dimetridazole as internal standard compound in hydrogen nuclear magnetic resonance technology
The opposed polarities such as deuterated methanol, deuterochloroform, deuterated acetonitrile, deuterated acetone, DMSO-D6, deuterium-oxide are primarily looked at
Deuterated solvent, shows that high-purity metronidazole is applied to above solvent by Fig. 1-6 results.In addition, feature hydrogen peak wider range, chemistry
Displacement 2-8ppm, is applicable the quantitative study in different IPs magnetic field.
By taking the quantitative nmr analysis of ethylparaben as an example, the present invention exists high-purity Dimetridazole as a kind of internal standard compound
It is applied in nmr quantitative technology.
Accurate weighing 10mg high-purities Dimetridazole is dissolved in 1mL deuterochloroform solvents altogether with 12mg ethylparabens,
It is to be measured into quartzy nuclear magnetic tube after after abundant dissolving, pipetting 0.80mL, while Dimetridazole is dissolved in respectively with ethylparaben
The ownership of chemical shift is determined in deuterochloroform as reference sample.
The factors such as nuclear-magnetism optimum experimental sampling time, sampling number, probe temperature, the quantitative nuclear-magnetism finally determined is determined
Parameter it is as follows：Nuclear-magnetism model：Avance III 400MHz, 1H NMR location parameters：90 ° of excitation pulse angle, sampling time
3.9846s, sweep length：8223.43Hz, relaxation delay 60s, add up sampling 16 times, probe temperature 293.4K, offset frequency：
2464.5137Hz, reception gain 64.00, pulse train zg30；Electronic balance：UMX2, Mettler Toledo companies of Switzerland
(scale division value：0.01mg)；Deuterated reagent：Deuterochloroform (sigma companies of the U.S.).
The hydrogen peak D (δ=4.30ppm) of Dimetridazole hydrogen peak B and ethylparaben, does not interfere with each other, and belong to same in Fig. 7
Nuclear-magnetism place.Calculated according to nuclear-magnetism Par value calculation formula is quantified as follows：
In above formula：PNMRThe purity of-the measured object measured using nuclear magnetic resonance method；
Ix- ethylparaben specifies the integral area at peak；
Istd- internal standard compound specifies the integral area at peak；
nstd- internal standard compound specifies the nuclear colony core number at peak；
nx- ethylparaben specifies the nuclear colony core number at peak；
MxThe molecular weight of-ethylparaben；
MstdThe molecular weight of-internal standard compound；
mstdThe quality of the internal standard compound of-addition；
mxThe sample weighting amount of-ethylparaben；
PstdThe purity of-internal standard compound.
Ethylparaben nuclear-magnetism quantified results are as shown in table 1.
The quantitative nuclear-magnetism of the hydrogen of table 1 spectrum determines the result (unit of ethylparaben：%)
The application effect of Dimetridazole is investigated as measured object using certified reference material ethylparaben, in table 1
Measurement result understands that the purity of ethylparaben is 99.7%, and it 0.2% is uncertainty, as a result shows to be surveyed with Dimetridazole
Fixed value 99.6% illustrates that measurement result of the present invention is accurate in the range of certificate value.
Claims (6)
1. application of the Dimetridazole as internal standard compound in hydrogen nuclear magnetic resonance technology.
2. application according to claim 1, it is characterised in that：The Dimetridazole is as internal standard compound in hydrogen nuclear magnetic resonance skill
At least one of application in art, including following 1) -3)：
1) to the structure elucidation of testing compound；
2) to the qualitative analysis of testing compound；
3) to the quantitative analysis of testing compound.
3. application according to claim 1 or 2, it is characterised in that：The purity of the Dimetridazole be 99.8% ±
0.4%.
4. the application according to any one of claim 1-3, it is characterised in that：The applicable solvent of the Dimetridazole is deuterium
For solvent；
In the deuterated solvent, the chemical shift of the Dimetridazole is 2~8ppm.
5. the application according to any one of claim 1-4, it is characterised in that：The deuterated solvent include deuterated methanol,
At least one of deuterochloroform, deuterated acetonitrile, deuterated acetone, deuterated dimethyl sulfoxide and deuterium-oxide.
6. the application according to any one of claim 1-5, it is characterised in that：The Dimetridazole is as internal standard compound in Buddhist nun
Application in the hydrogen nuclear magnetic resonance quantitative analysis of the golden ethyl ester of pool.
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Cited By (2)
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| CN108344762A (en) * | 2018-02-23 | 2018-07-31 | 中国科学院长春应用化学研究所 | The detection method of polylactic acid content in a kind of degradable plastic product |
| CN112305007A (en) * | 2020-10-30 | 2021-02-02 | 上海化工研究院有限公司 | Method for measuring deuterium isotope abundance of deuterium labeled compound by using nuclear magnetic hydrogen spectrum or deuterium spectrum |
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