CN116400002A - N, N-dimethylethanolamine detection method - Google Patents
N, N-dimethylethanolamine detection method Download PDFInfo
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- CN116400002A CN116400002A CN202310336740.1A CN202310336740A CN116400002A CN 116400002 A CN116400002 A CN 116400002A CN 202310336740 A CN202310336740 A CN 202310336740A CN 116400002 A CN116400002 A CN 116400002A
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- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000001514 detection method Methods 0.000 title claims description 10
- 238000000034 method Methods 0.000 claims abstract description 27
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- 239000003480 eluent Substances 0.000 claims abstract description 8
- 150000002500 ions Chemical class 0.000 claims abstract description 8
- 239000000945 filler Substances 0.000 claims abstract description 4
- 239000011347 resin Substances 0.000 claims abstract description 4
- 229920005989 resin Polymers 0.000 claims abstract description 4
- 238000010828 elution Methods 0.000 claims abstract description 3
- HVZUXXJWSWNELT-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene Chemical compound CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C HVZUXXJWSWNELT-UHFFFAOYSA-N 0.000 claims abstract 2
- 238000005341 cation exchange Methods 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 19
- 239000000126 substance Substances 0.000 abstract description 16
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 125000004122 cyclic group Chemical group 0.000 abstract description 8
- GCUDNJFWGVFGCM-UHFFFAOYSA-N C1CCC(C1)OCl Chemical compound C1CCC(C1)OCl GCUDNJFWGVFGCM-UHFFFAOYSA-N 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 description 28
- 239000000047 product Substances 0.000 description 20
- 239000000243 solution Substances 0.000 description 17
- 238000012360 testing method Methods 0.000 description 17
- 239000011550 stock solution Substances 0.000 description 13
- 239000013558 reference substance Substances 0.000 description 12
- 239000012488 sample solution Substances 0.000 description 11
- 238000005303 weighing Methods 0.000 description 10
- 239000003814 drug Substances 0.000 description 7
- 239000000543 intermediate Substances 0.000 description 6
- 239000000523 sample Substances 0.000 description 6
- 239000012490 blank solution Substances 0.000 description 5
- 201000000255 cycloplegia Diseases 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000010998 test method Methods 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000010790 dilution Methods 0.000 description 4
- 239000012895 dilution Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 239000012085 test solution Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- SFRUVBWDAJNXSB-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;but-1-enylbenzene Chemical compound CCC=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C SFRUVBWDAJNXSB-UHFFFAOYSA-N 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000001886 ciliary effect Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- -1 ester hydrochloride Chemical class 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 230000001738 genotoxic effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 210000003205 muscle Anatomy 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000012088 reference solution Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 229940121948 Muscarinic receptor antagonist Drugs 0.000 description 1
- 208000006550 Mydriasis Diseases 0.000 description 1
- UEEJHVSXFDXPFK-UHFFFAOYSA-O N-dimethylethanolamine Chemical compound C[NH+](C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-O 0.000 description 1
- 206010033799 Paralysis Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002164 acetylcholinergic effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000812 cholinergic antagonist Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003500 cycloplegic effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000012972 dimethylethanolamine Substances 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003747 fuel oil additive Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 231100000025 genetic toxicology Toxicity 0.000 description 1
- 231100000024 genotoxic Toxicity 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000003589 local anesthetic agent Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000002911 mydriatic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 210000001747 pupil Anatomy 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 210000005070 sphincter Anatomy 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
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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
- G01N30/96—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 using ion-exchange
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- 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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for detecting related substances of cyclopentoxy hydrochloride, and provides a method for detecting N, N-dimethylethanolamine. In the method, elution is carried out on an ion chromatograph, and a chromatographic column taking 2.5mmol/L nitric acid as eluent and sulfonic group ethyl vinyl benzene-divinylbenzene resin as a filler is adopted. The invention can effectively separate N, N-dimethylethanolamine of the cyclopentoxyde hydrochloride, has good separation degree, and can effectively control the production quality. The method can simply, rapidly and accurately separate and detect the related substances of the cyclic spray-tuitoyl hydrochloride and the substances with influenced quality, has the advantages of strong specificity, high sensitivity, good stability, good reproducibility, high precision and good peak shape, and can be used for effectively controlling the purity and quality of the cyclic spray-tuitoyl hydrochloride in actual production.
Description
Technical Field
The invention belongs to the technical field of chemical drug analysis methods, relates to a method for detecting related substances of cyclic spray tolate hydrochloride, and particularly relates to a method for detecting N, N-dimethylethanolamine.
Background
In recent years, although there is a new method of refraction, mydriatic refraction of the ciliary muscle paralyzer remains the most reliable method demonstrated over time. The ophthalmic doctor needs a medicine which has the characteristics of quick acting, complete disappearance of the regulating action, enough maximum ciliary muscle paralysis time, quick recovery of the regulating action, small side effect and the like of mydriasis and ciliary muscle paralysis, and is used as a conventional medicine for ophthalmic outpatient examination.
The cyclopentoxil hydrochloride is used as an artificially synthesized anticholinergic agent, belongs to a short-acting ciliary muscle paralysis agent, can block the action of acetylcholinergic on iris sphincter and M receptor on ciliary muscle, and can make pupil dilate and regulate paralysis (ciliary muscle paralysis). The cycloplegic hydrochloride is the most preferred ciliary muscle paralysis drug in clinic, and most patients can recover enough adjustment amplitude for reading after 6-12 hours.
The related substances (Telated substances) are known to be substances such as starting materials, reagents, intermediates, byproducts and the like brought in the production of bulk drugs, and may be degradation products, polymers or special impurities such as crystal forms which are generated during the production, storage and transportation of the preparation. The types of related substances are closely related to the synthetic route and the production process of the medicine, and the impurity spectrum of the medicine can also change according to different synthetic routes and different production processes, so that a proper analysis method is required to be established according to different synthetic routes and different production processes, and the accurate and effective detection and monitoring of the related substances of the intermediate of the cyclic spray-tuitoster hydrochloride are achieved.
N, N-dimethylethanolamine is used as related substances of the cyclospray ester hydrochloride, and is also called N, N-dimethyl-2-hydroxy ethylamine and 2-dimethyl amino ethanol, and has a genotoxicity warning structure. Can be used as local anesthetic, textile auxiliary agent, fuel oil additive, ion exchange resin, etc. and is widely applied to the production and life of people. However, as a genotoxic impurity, very low concentrations of N, N-dimethylethanolamine can damage DNA, severely threatening the patient's life safety. Therefore, accurate determination of the N, N-dimethylethanolamine content is critical. However, since N, N-dimethylethanolamine does not have an ultraviolet absorption peak, it is not suitable for liquid phase ultraviolet spectrum detection analysis; in addition, in the process of forming hydrochloride of the cyclic spray ester, N, N-dimethylethanolamine also forms hydrochloride, so that the boiling point is increased, the method is not suitable for detection by gas chromatography, and no means for effectively detecting and analyzing the impurity is specially available at present.
Disclosure of Invention
The invention provides a method for detecting N, N-dimethylethanolamine in order to make up for the defects of the prior art.
The invention is realized by the following technical scheme: the detection method of N, N-dimethylethanolamine is characterized in that elution is carried out on an ion chromatograph, and 2.5mmol/L nitric acid is adopted as eluent; a chromatographic column using sulfonic acid group-containing ethylvinylbenzene-divinylbenzene resin as a filler (Metrosep C4 cation exchange column).
Further, ion chromatography employs a conductivity detector.
Further, the concentration of the eluent is: 2.25 to 2.75mmol/L.
Further, the column temperature is 35-45 ℃.
Further, mobile phase flow rate: 0.8-1.0 mL/min.
Compared with the prior art, the invention has the advantages and positive effects that:
the invention can effectively separate N, N-dimethylethanolamine of the cyclopentoxyde hydrochloride, has good separation degree, and can effectively control the production quality. The method can simply, rapidly and accurately separate and detect the related substances of the cyclic spray-tuitoyl hydrochloride and the substances with influenced quality, has the advantages of strong specificity, high sensitivity, good stability, good reproducibility, high precision and good peak shape, and can be used for effectively controlling the purity and quality of the cyclic spray-tuitoyl hydrochloride in actual production.
Drawings
FIG. 1 is a chromatogram of a blank solution of example 1;
FIG. 2 is a chromatogram of the control solution of example 1;
FIG. 3 is a chromatogram of a sample of cycloparaffin hydrochloride of example 1;
FIG. 4 is a chromatogram of the control solution of example 2;
FIG. 5 is a chromatogram of a sample solution of cycloparaffin hydrochloride of example 2;
FIG. 6 is a chromatogram of the control solution of example 3;
FIG. 7 is a chromatogram of a sample solution of cycloparaffin hydrochloride of example 3;
FIG. 8 is a chromatogram of the control solution of example 4;
FIG. 9 is a chromatogram of a sample solution of cycloparaffin hydrochloride of example 4;
FIG. 10 is a chromatogram of the control solution of example 5;
FIG. 11 is a chromatogram of a sample solution of cycloparaffin hydrochloride of example 5;
FIG. 12 is a chromatogram of the control solution of example 6;
FIG. 13 is a chromatogram of a sample solution of cycloparaffin hydrochloride of example 6;
FIG. 14 is a chromatogram of the control solution of example 7;
FIG. 15 is a chromatogram of a sample solution of cycloparaffin hydrochloride of example 7.
Detailed Description
In order that the above objects, features and advantages of the invention will be more clearly understood, a further description of the invention will be provided with reference to specific examples. It should be noted that, in the case of no conflict, the embodiments of the present application and the features in the embodiments may be combined with each other.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as described herein, and therefore the present invention is not limited to the specific embodiments of the disclosure that follow.
Example 1
(1) Detection conditions
Instrument: a swiss universal 930 ion chromatograph, conductivity detector;
chromatographic column: a sulfonic group-containing ethylvinylbenzene-divinylbenzene resin was used as a filler (Metrosep C4 cation exchange column 150 mm. Times.4.0 mm);
eluent: 2.5mmol/L nitric acid;
flow rate: 0.9mL/min
Column temperature: 40 ℃;
sample injection amount: 20. Mu.L;
(2) Detection step
Preparation of a blank solution: 2.5mmol/L nitric acid was taken as a blank solution.
Preparation of a control solution: taking about 0.25g of N, N-Dimethylethanolamine (DMEA), precisely weighing, placing into a 25mL measuring flask, adding a solvent for dissolution and dilution to scale, shaking uniformly, precisely weighing 1mL, placing into a 100mL volumetric flask, adding a solvent for dilution to scale, and shaking uniformly to obtain the N, N-dimethylethanolamine.
Preparation of test solution: about 25mg of the product is taken, precisely weighed, placed in a 25mL measuring flask, dissolved by adding a solvent, diluted to a scale and uniformly shaken to obtain the product.
Respectively precisely measuring 20 μl of blank solution, reference solution and sample solution, injecting into ion chromatograph, and recording chromatograms (see fig. 1, 2 and 3); the results show that: in FIG. 2, N, N-dimethylethanolamine peaked at 8.812min and the blank solution had no interference with the assay.
Example 2
A similar test procedure was followed as in example 1, wherein the flow rate was 0.8mL/min. The reference substance has a pattern shown in figure 4 and the sample has a pattern shown in figure 5.N, N-dimethylethanolamine was excellent in peak form at 10.085 min.
Example 3
A similar test procedure was followed as in example 1, wherein the flow rate was 1.0mL/min. The reference substance has a pattern shown in figure 6 and the sample has a chromatogram shown in figure 7.N, N-dimethylethanolamine was excellent in peak form at 8.010 min.
Example 4
A similar assay as in example 1 was performed, wherein the column temperature was 35 ℃. The reference substance has a pattern shown in figure 8 and the sample has a pattern shown in figure 9.N, N-dimethylethanolamine was excellent in peak form at 9.383 min.
Example 5
A similar test procedure was followed as in example 1, wherein the column temperature was 45 ℃. The chromatogram of the reference substance is shown in figure 10, and the chromatogram of the test substance is shown in figure 11.N, N-dimethylethanolamine was excellent in peak form at 8.662 min.
Example 6
A similar test procedure was followed as in example 1, wherein the eluent was 2.25mmol/L nitric acid. The reference substance is shown in figure 12 and the test sample is shown in figure 13.N, N-dimethylethanolamine was excellent in peak form at 9.457 min.
Example 7
A similar test procedure was followed as in example 1, wherein the eluent was 2.75mmol/L nitric acid. The reference solution has a chromatogram of FIG. 14 and a chromatogram of the sample solution of FIG. 15.N, N-dimethylethanolamine is in 8.072min, and the peak type is good.
The above test illustrates: the method can quantitatively detect the N, N-dimethylethanolamine in the cyclopentoxy hydrochloride, and provides a better basis for controlling the quality of the product.
The reagents used in the present invention are all commercially available.
In order to further verify the feasibility of the practical application of the present invention, the present invention also performed the following verification test. The cyclic spray ester hydrochloride product to be tested in the following test is referred to as the "product". The other reagents are all commercial reagents, and the purity is chromatographic purity and analytical purity.
Linear test
Solvent: 2.5mmol/L nitric acid
Control stock solution: taking about 0.25g of N, N-dimethylethanolamine reference substance, precisely weighing, putting into a 25mL measuring flask, adding a solvent to dissolve and dilute to a scale, and shaking uniformly to obtain the N, N-dimethylethanolamine reference substance.
Preparation of a linear solution: taking 1mL of reference substance stock solution, placing the reference substance stock solution into a 100mL measuring flask, adding a solvent to dilute to a scale, shaking uniformly, precisely measuring 0.5mL, 0.8mL, 1mL, 1.2mL and 1.5mL, respectively placing the reference substance stock solution into the 100mL measuring flask, adding the solvent to dilute to the scale, shaking uniformly, and respectively taking the reference substance stock solution as linear solutions (1), (2), (3), (4) and (5).
And precisely measuring 20 mu L of each linear relation solution, respectively injecting into an ion chromatograph, and recording a chromatogram.
TABLE 2 Linear test results
From the test results, the N, N-dimethylethanolamine has good linear relation in the concentration range of 0.06466-1.61658 mug/mL, the linear relation equation y= 0.06661x-0.00006, the correlation coefficient R is 0.9997, the Y-axis intercept is less than 25% of the 100% response value, and the response factor RSD is 6.0%. Where x denotes concentration C (μg/mL) and y denotes peak area.
The chromatographic values obtained in examples 1 to 7 (data directly derived from a computer connected to the chromatograph) were substituted into standard curves (linear correlation equations) with the values of the peak areas y, respectively, to obtain the corresponding concentrations x, and thus quantitative determination was performed on N, N-dimethylethanolamine.
Second, repeatability test
Control stock solution: taking about 0.25g of N, N-dimethylethanolamine, precisely weighing, placing into a 25mL measuring flask, adding a solvent to dissolve and dilute to a scale, and shaking uniformly to obtain the N, N-dimethylethanolamine.
Control solution: precisely measuring 1mL of reference substance stock solution, placing into a 100mL measuring flask, adding solvent to dilute to scale, shaking, precisely measuring 1mL, placing into a 100mL measuring flask, diluting with solvent to scale, and shaking to obtain the final product.
Sample solution: about 25mg of the product is taken, precisely weighed, placed in a 25mL measuring flask, dissolved by adding a solvent, diluted to a scale, and shaken uniformly to serve as a sample solution. The formulation was repeated 6 parts.
The 20. Mu.L of the above solution was precisely measured, injected into an ion chromatograph, and the chromatogram was recorded.
TABLE 3 repeatability test results
Conclusion: the test results show that the repeated measurement of the product is 6 times, the repeated measurement results of N, N-dimethylethanolamine are 0.004%, and the RSD is 0, so that the method is proved to have good repeatability.
Third, intermediate precision test
And (3) respectively detecting N, N-dimethylethanolamine by different operators in different dates, and looking at the change of detection results. Solution formulation and process reproducibility. The results are shown in Table 5.
TABLE 4 intermediate II related substance examination intermediate precision test results
Conclusion: as shown by test results, the product is repeatedly measured by different personnel for 6 times, the average value of the measurement results of 12 times is 0.004%, and the RSD is 14.7%; the method proves that the intermediate precision is good.
Fourth, accuracy verification test
Solvent: 2.5mmol/L nitric acid
Blank test solution: taking about 50mg of the product, precisely weighing, placing into a 50mL measuring flask, adding a solvent to dissolve and dilute to a scale, and shaking uniformly to obtain the product.
Control solution: taking about 0.25g of N, N-dimethylethanolamine, precisely weighing, placing into a 25mL measuring flask, adding a solvent to dissolve and dilute to a scale, shaking uniformly, taking 1mL, placing into a 100mL measuring flask, adding a solvent to dilute to a scale, shaking uniformly, taking 1mL again, placing into a 100mL measuring flask, adding a solvent to dilute to a scale, and shaking uniformly to obtain the N, N-dimethylethanolamine.
Control stock solution i: taking about 0.25g of N, N-dimethylethanolamine, precisely weighing, placing into a 25mL measuring flask, adding a solvent to dissolve and dilute to a scale, shaking uniformly, taking 1mL, placing into a 100mL measuring flask, adding the solvent to dilute to the scale, shaking uniformly, taking 2.5mL again, placing into a 100mL measuring flask, adding the solvent to dilute to the scale, and shaking uniformly to obtain the N, N-dimethylethanolamine.
10% accuracy test solution: about 25mg of the product is taken, precisely weighed, placed in a 25mL measuring flask, 1mL of the control stock solution I is measured and placed in the same measuring flask, and the product is dissolved and diluted to a scale by adding a solvent, and is uniformly shaken, thus obtaining the product. 3 parts of the mixture are prepared by the same method.
Control stock solution ii: taking about 0.25g of N, N-dimethylethanolamine, precisely weighing, placing into a 25mL measuring flask, adding a solvent to dissolve and dilute to a scale, shaking uniformly, taking 5mL, placing into a 100mL measuring flask, adding a solvent to dilute to a scale, shaking uniformly, taking 5mL again, placing into a 100mL measuring flask, adding a solvent to dilute to a scale, and shaking uniformly to obtain the N, N-dimethylethanolamine.
100% accuracy test solution: about 25mg of the product is taken, precisely weighed, placed in a 25mL measuring flask, 1mL of the control stock solution II is measured and placed in the same measuring flask, and the product is dissolved and diluted to a scale by adding a solvent, and is uniformly shaken to obtain the product. 3 parts of the mixture are prepared by the same method.
Control stock solution iii: taking about 0.25g of N, N-dimethylethanolamine, precisely weighing, placing into a 25mL measuring flask, adding a solvent for dilution to a scale, shaking uniformly, measuring 5mL, placing into a 100mL measuring flask, adding a solvent for dilution to a scale, and shaking uniformly. And weighing 7.5mL, placing in a 100mL measuring flask, adding solvent to dilute to a scale, and shaking uniformly to obtain the product.
Sample solution with 150% accuracy: about 25mg of the product is taken, precisely weighed, placed in a 25mL measuring flask, 1mL of the control stock solution III is measured and placed in the same measuring flask, and the product is dissolved and diluted to a scale by adding a solvent, and is uniformly shaken to obtain the product. 3 parts of the mixture are prepared by the same method.
Precisely measuring 20 mu L of each solution, respectively injecting into an ion chromatograph, and recording a chromatogram. The results are shown in Table 5.
TABLE 5 recovery test results
Conclusion: according to the test results, the average recovery rate of 9 samples is 97.9 percent and is 91.81-105.99 percent, and the recovery rate RSD of 9 samples is 4.6 percent; less than 10.0%, and the accuracy of the method is good.
The present invention is not limited to the above-mentioned embodiments, and any equivalent embodiments which can be changed or modified by the technical content disclosed above can be applied to other fields, but any simple modification, equivalent changes and modification made to the above-mentioned embodiments according to the technical substance of the present invention without departing from the technical content of the present invention still belong to the protection scope of the technical solution of the present invention.
Claims (7)
1. The detection method of N, N-dimethylethanolamine is characterized in that elution is carried out on an ion chromatograph, and 2.5mmol/L nitric acid is adopted as eluent; a chromatographic column using sulfonic group ethyl vinyl benzene-divinylbenzene resin as filler.
2. The method for detecting N, N-dimethylethanolamine according to claim 1, wherein the chromatographic column is a Metrosep C4 cation exchange column.
3. The method for detecting N, N-dimethylethanolamine according to claim 1, wherein a conductivity detector is used.
4. The method for detecting N, N-dimethylethanolamine according to claim 1, wherein the concentration of the eluent is: 2.25 to 2.75mmol/L.
5. The method for detecting N, N-dimethylethanolamine according to claim 1, wherein the column temperature is 35 to 45 ℃.
6. The method for detecting N, N-dimethylethanolamine according to claim 1, wherein the flow rate: 0.8-1.0 mL/min.
7. The method for detecting N, N-dimethylethanolamine according to claim 1, wherein the sample volume of the sample to be detected in the method is 20. Mu.L.
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