CN113156029B - Method for measuring purity of aminoguanidine carbonate by liquid chromatography - Google Patents
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- VPIXQGUBUKFLRF-UHFFFAOYSA-N 3-(2-chloro-5,6-dihydrobenzo[b][1]benzazepin-11-yl)-N-methyl-1-propanamine Chemical compound C1CC2=CC=C(Cl)C=C2N(CCCNC)C2=CC=CC=C21 VPIXQGUBUKFLRF-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000004811 liquid chromatography Methods 0.000 title claims abstract description 11
- 239000012488 sample solution Substances 0.000 claims description 62
- 239000000523 sample Substances 0.000 claims description 51
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 39
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 25
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 25
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 25
- 239000007853 buffer solution Substances 0.000 claims description 25
- 238000001514 detection method Methods 0.000 claims description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000741 silica gel Substances 0.000 claims description 16
- 229910002027 silica gel Inorganic materials 0.000 claims description 16
- 238000004458 analytical method Methods 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 239000003643 water by type Substances 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000012086 standard solution Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 239000000337 buffer salt Substances 0.000 description 6
- 230000014759 maintenance of location Effects 0.000 description 6
- 238000000926 separation method Methods 0.000 description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000000945 filler Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000003139 buffering effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- IWUCXVSUMQZMFG-AFCXAGJDSA-N Ribavirin Chemical compound N1=C(C(=O)N)N=CN1[C@H]1[C@H](O)[C@H](O)[C@@H](CO)O1 IWUCXVSUMQZMFG-AFCXAGJDSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004366 reverse phase liquid chromatography Methods 0.000 description 1
- 229960000329 ribavirin Drugs 0.000 description 1
- HZCAHMRRMINHDJ-DBRKOABJSA-N ribavirin Natural products O[C@@H]1[C@H](O)[C@@H](CO)O[C@H]1N1N=CN=C1 HZCAHMRRMINHDJ-DBRKOABJSA-N 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/74—Optical detectors
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Abstract
The invention belongs to the field of analytical chemistry, and discloses a method for analyzing the purity of aminoguanidine carbonate by using a liquid chromatography. The method has the advantages of strong specificity, high accuracy and simple and convenient operation.
Description
Technical Field
The invention belongs to the field of analytical chemistry, relates to a method for measuring the purity of aminoguanidine carbonate by liquid chromatography, and in particular relates to a method for measuring the purity of aminoguanidine carbonate by high performance liquid chromatography.
Background
Aminoguanidine carbonate is a white fine crystalline powder. Is hardly soluble in water, insoluble in alcohol and other acids, and is unstable under heating, and gradually decomposes at a temperature exceeding 50 ℃. The chemical structural formula is as follows:
the method is mainly used for synthesizing medicines and dyes. In the pharmaceutical industry, the method is mainly used for synthesizing furguanide, azomethine, ribavirin, propionizone and the like, and can also be used as pesticides, dyes, photographic agents and hairFoam agent and explosive.
Currently, the determination method of the purity of the aminoguanidine carbonate mainly comprises an iodometry method and a spectrophotometry method, the two methods have complicated operation steps, longer analysis time and larger influence of human factors on the determination result.
Disclosure of Invention
In order to solve the problems of complicated operation steps, long analysis time and great influence of human factors on the measurement result in the existing method for measuring the purity of the aminoguanidine carbonate, the invention provides a method for measuring the purity of the aminoguanidine carbonate by using a liquid chromatography. Thereby ensuring the purity of the aminoguanidine carbonate and realizing the quality control of the product.
The technical scheme of the invention is to provide a method for measuring the purity of aminoguanidine carbonate by liquid chromatography, which is characterized by comprising the following steps:
1) Dissolving a standard sample and a sample to be tested by using a mobile phase, and respectively preparing a standard sample solution and a sample solution;
the mobile phase consists of methanol and ammonium sulfate buffer solution, and the volume ratio of the methanol to the ammonium sulfate buffer solution is as follows: 1 to 25:99 to 75, and the pH value of the ammonium sulfate buffer solution is 2 to 5;
2) Reversed phase C using silica gel 18 The chromatographic column detects the standard sample solution and the sample solution respectively, and records chromatograms of the two solutions;
the flow rate of the mobile phase in the detection process is 0.5-1.5 ml/min, the detection wavelength is 195-254 nm, and the temperature of a chromatographic column box is 25-40 ℃;
3) The purity of aminoguanidine carbonate was calculated by analysis of both chromatograms.
Further, the silica gel is reversed phase C 18 The chromatographic column is Waters Atlantis T 3 A chromatographic column.
Further, the ratio of the methanol to the ammonium sulfate buffer solution is 5:95.
Further, the concentration of the ammonium sulfate buffer solution is 0.075mol/L, and the pH value is 2.5.
Further, the flow rate of the mobile phase is 1.0ml/min, the detection wavelength is 220nm, and the temperature of a chromatographic column box is 35 ℃.
Further, a standard solution was prepared by the following method: weighing 100mg of standard sample into a 100ml volumetric flask, adding a mobile phase for dissolution, and ultrasonically dissolving to fix the volume to a scale;
sample solutions were prepared by the following method: weigh 100mg sample into 100ml volumetric flask, add mobile phase to dissolve, and sonicate to volume to scale.
Further, the sample volume in step 2) was 10. Mu.L.
The beneficial effects of the invention are as follows:
1. the invention adopts silica gel reversed phase C 18 The chromatographic column rapidly and accurately realizes the determination of the purity of the aminoguanidine carbonate, thereby realizing the control of the purity of the aminoguanidine carbonate, ensuring the quality controllability of the aminoguanidine carbonate and having practical significance.
2. The method can effectively determine the purity of the aminoguanidine carbonate, is simple and quick, has high analysis sensitivity and accurate and reliable results.
3. The invention uses mobile phase in sample preparation, and has the advantages of simple operation and economy.
Drawings
FIG. 1 is a chromatogram of a standard sample in example 1;
FIG. 2 is a chromatogram of the sample to be tested in example 1;
FIG. 3 is a chromatogram of a standard sample in example 4.
Detailed Description
The following examples are provided for further understanding of the present invention, and are preferred embodiments of the present invention, but the present invention is not limited to the scope of the present embodiment.
Example 1
The apparatus used in this example was as follows:
liquid chromatograph: waters 2695; chromatographic column: atlantis T 3 Column, chromatographic column filler particles 5 μm, column length 250mm, inner diameter 4.6mm;
the detection condition parameters of this embodiment are as follows:
detection wavelength: 220nm; mobile phase: the volume ratio of the ammonium sulfate buffer solution to the methanol is 95:5, wherein the concentration of the ammonium sulfate buffer solution is 0.075mol/L, the pH is 2.5, and phosphoric acid can be used for adjusting the pH;
chromatographic column box temperature: 35 ℃; mobile phase flow rate: 1.0ml/min.
The detection is realized by the following steps:
taking about 100mg of aminoguanidine carbonate standard sample, placing the sample into a 100ml volumetric flask, adding a mobile phase to dissolve and dilute the sample to a scale, and shaking the sample uniformly to obtain a standard sample solution.
Taking about 100mg of aminoguanidine carbonate sample, placing the aminoguanidine carbonate sample into a 100ml volumetric flask, adding a mobile phase to dissolve and dilute the aminoguanidine carbonate sample to a scale, and shaking the aminoguanidine carbonate sample uniformly to obtain a sample solution to be measured.
10 mu L of standard sample solution was taken and analyzed under the above chromatographic conditions, and the chromatogram was recorded, and the result is shown in FIG. 1.
The chromatographic peak with retention time of 13.395min in FIG. 1 is that of aminoguanidine carbonate, and the rest is that of impurities. Under the above conditions, the aminoguanidine carbonate chromatographic peak and other impurity chromatographic peaks have good separation degree, and can meet the requirements of analysis and test.
10 mu L of the sample solution to be detected is taken, analysis is carried out according to the chromatographic conditions, and a chromatogram is recorded, and the result is shown in figure 2.
The chromatographic peak with retention time of 13.349min in FIG. 2 is that of aminoguanidine carbonate, the remaining chromatographic peaks are impurity peaks, and the purity is calculated according to the external standard peak area method. The results of the above examples show that: the method can clearly separate the aminoguanidine carbonate from impurities thereof, accurately and quantitatively detect the aminoguanidine carbonate, calculate the purity of the aminoguanidine carbonate, and effectively control the product quality of the aminoguanidine carbonate.
And 3, analyzing the two chromatograms, and calculating the purity of the aminoguanidine carbonate.
In the detection process, silica gel reverse phase C can be utilized first after the standard sample solution is prepared 18 Detecting the standard sample solution by using a chromatographic column; thereafter preparing a sample solution, reversed phase C using silica gel 18 The chromatographic column detects the sample solution.
Example 2
The apparatus used in this example was as follows:
liquid chromatograph: waters 2695; chromatographic column: atlantis T 3 Column, chromatographic column filler particles 5 μm, column length 250mm, inner diameter 4.6mm;
the detection condition parameters of this embodiment are as follows:
detection wavelength: 195nm; mobile phase: the volume ratio of the ammonium sulfate buffer solution to the methanol is 75:25, wherein the concentration of the ammonium sulfate buffer solution is 0.075mol/L, the pH is 5, and phosphoric acid can be used for adjusting the pH;
chromatographic column box temperature: 25 ℃; mobile phase flow rate: 1.5ml/min.
The detection is realized by the following steps:
taking about 100mg of aminoguanidine carbonate standard sample, placing the sample into a 100ml volumetric flask, adding a mobile phase to dissolve and dilute the sample to a scale, and shaking the sample uniformly to obtain a standard sample solution.
Taking about 100mg of aminoguanidine carbonate sample, placing the aminoguanidine carbonate sample into a 100ml volumetric flask, adding a mobile phase to dissolve and dilute the aminoguanidine carbonate sample to a scale, and shaking the aminoguanidine carbonate sample uniformly to obtain a sample solution to be measured.
10 mu L of the standard sample solution was taken and analyzed under the above chromatographic conditions, and the chromatogram was recorded, and the result was similar to that of FIG. 1.
The chromatographic peak with retention time of 13.395min is that of aminoguanidine carbonate, and the rest is that of impurity. Under the above conditions, the aminoguanidine carbonate chromatographic peak and other impurity chromatographic peaks have good separation degree, and can meet the requirements of analysis and test.
10 mu L of the sample solution to be detected is taken, analysis is carried out according to the chromatographic conditions, and a chromatogram is recorded, and the result is similar to that of FIG. 2.
The chromatographic peak with retention time of 13.349min is the chromatographic peak of aminoguanidine carbonate, the rest chromatographic peaks are impurity peaks, and the purity is calculated according to an external standard peak area method. The results of the above examples show that: the method can clearly separate the aminoguanidine carbonate from impurities thereof, accurately and quantitatively detect the aminoguanidine carbonate, calculate the purity of the aminoguanidine carbonate, and effectively control the product quality of the aminoguanidine carbonate.
And 3, analyzing the two chromatograms, and calculating the purity of the aminoguanidine carbonate.
In the detection process, silica gel reverse phase C can be utilized first after the standard sample solution is prepared 18 Detecting the standard sample solution by using a chromatographic column; thereafter preparing a sample solution, reversed phase C using silica gel 18 The chromatographic column detects the sample solution.
Example 3
The apparatus used in this example was as follows:
liquid chromatograph: waters 2695; chromatographic column: atlantis T 3 Column, chromatographic column filler particles 5 μm, column length 250mm, inner diameter 4.6mm;
the detection condition parameters of this embodiment are as follows:
detection wavelength: 254nm; mobile phase: the volume ratio of the ammonium sulfate buffer solution to the methanol is 99:1, wherein the concentration of the ammonium sulfate buffer solution is 0.075mol/L, the pH is 2.0, and phosphoric acid can be used for adjusting the pH;
chromatographic column box temperature: 40 ℃; mobile phase flow rate: 0.5ml/min.
The detection is realized by the following steps:
taking about 100mg of aminoguanidine carbonate standard sample, placing the sample into a 100ml volumetric flask, adding a mobile phase to dissolve and dilute the sample to a scale, and shaking the sample uniformly to obtain a standard sample solution.
Taking about 100mg of aminoguanidine carbonate sample, placing the aminoguanidine carbonate sample into a 100ml volumetric flask, adding a mobile phase to dissolve and dilute the aminoguanidine carbonate sample to a scale, and shaking the aminoguanidine carbonate sample uniformly to obtain a sample solution to be measured.
10 mu L of the standard sample solution was taken and analyzed under the above chromatographic conditions, and the chromatogram was recorded, and the result was similar to that of FIG. 1.
The chromatographic peak with retention time of 13.395min in FIG. 1 is that of aminoguanidine carbonate, and the rest is that of impurities. Under the above conditions, the aminoguanidine carbonate chromatographic peak and other impurity chromatographic peaks have good separation degree, and can meet the requirements of analysis and test.
10 mu L of the sample solution to be detected is taken, analysis is carried out according to the chromatographic conditions, and a chromatogram is recorded, and the result is similar to that of FIG. 2.
The chromatographic peak with retention time of 13.349min in FIG. 2 is that of aminoguanidine carbonate, the remaining chromatographic peaks are impurity peaks, and the purity is calculated according to the external standard peak area method. The results of the above examples show that: the method can clearly separate the aminoguanidine carbonate from impurities thereof, accurately and quantitatively detect the aminoguanidine carbonate, calculate the purity of the aminoguanidine carbonate, and effectively control the product quality of the aminoguanidine carbonate.
And 3, analyzing the two chromatograms, and calculating the purity of the aminoguanidine carbonate.
In the detection process, silica gel reverse phase C can be utilized first after the standard sample solution is prepared 18 Detecting the standard sample solution by using a chromatographic column; thereafter preparing a sample solution, reversed phase C using silica gel 18 The chromatographic column detects the sample solution.
Example 4
The apparatus used in this example was as follows:
liquid chromatograph: waters 2695; chromatographic column: a lichromher 100Diol reverse phase chromatography column;
the detection condition parameters of this embodiment are as follows:
detection wavelength: 190nm; mobile phase: the volume ratio of the ammonium sulfate buffer solution to the methanol is 70:30, wherein the concentration of the ammonium sulfate buffer solution is 0.075mol/L, the pH is 6.0, and phosphoric acid can be used for adjusting the pH;
chromatographic column box temperature: 20 ℃; mobile phase flow rate: 1.6ml/min.
The detection is realized by the following steps:
taking about 100mg of aminoguanidine carbonate standard sample, placing the sample into a 100ml volumetric flask, adding a mobile phase to dissolve and dilute the sample to a scale, and shaking the sample uniformly to obtain a standard sample solution.
Taking about 100mg of aminoguanidine carbonate sample, placing the aminoguanidine carbonate sample into a 100ml volumetric flask, adding a mobile phase to dissolve and dilute the aminoguanidine carbonate sample to a scale, and shaking the aminoguanidine carbonate sample uniformly to obtain a sample solution to be measured.
10 μl of the standard sample solution was taken and analyzed under the above chromatographic conditions, and the chromatogram was recorded, and the result is shown in FIG. 3.
In fig. 3, the standard sample has poor separation of chromatographic peaks of various substances, more impurity peaks which are not concerned appear, the main peak is trailing, the detection result is 79.61%, and the difference from the actual result is 99.0% is large.
The method for establishing the liquid chromatography for detecting the purity of the aminoguanidine carbonate mainly comprises the aspects of chromatographic column selection, mobile phase pH value determination, sample solution concentration determination and the like. Extensive research has been conducted on the model or parameters that each work ultimately determines, and an unsuitable parameter may result in undesirable chromatographic peak separations or peak shapes. For example, in the development of the method, the choice of buffer salt and the buffer capacity of the buffer salt are related to the concentration of the buffer salt and the pH of the buffer salt solution. The greater the buffer salt concentration, the greater the buffering capacity; the closer the pH of the buffer salt solution is to its pka, the more buffering capacity is. The method for measuring the purity of the aminoguanidine carbonate is finally obtained through repeated test verification, and the method is high in accuracy, simple, feasible, good in repeatability and suitable for quality control of industrial production of the aminoguanidine carbonate.
Claims (4)
1. A method for determining the purity of aminoguanidine carbonate by liquid chromatography, comprising the steps of:
1) Dissolving a standard sample and a sample to be tested by using a mobile phase, and respectively preparing a standard sample solution and a sample solution;
the mobile phase consists of methanol and ammonium sulfate buffer solution, and the volume ratio of the methanol to the ammonium sulfate buffer solution is as follows: 5:95, wherein the pH value of the ammonium sulfate buffer solution is 2.5, and the concentration of the ammonium sulfate buffer solution is 0.075mol/L;
2) Detecting a standard sample solution and a sample solution by using a silica gel reversed-phase C18 chromatographic column respectively, and recording chromatograms of the two solutions;
the flow rate of the mobile phase in the detection process is 1ml/min, the detection wavelength is 220nm, and the temperature of a chromatographic column box is 35 ℃;
3) Calculating the purity of the aminoguanidine carbonate by analyzing the two chromatograms;
or alternatively, the process may be performed,
1) Dissolving a standard sample and a sample to be tested by using a mobile phase, and respectively preparing a standard sample solution and a sample solution;
the mobile phase consists of methanol and ammonium sulfate buffer solution, and the volume ratio of the methanol to the ammonium sulfate buffer solution is as follows: 25:75, wherein the pH value of the ammonium sulfate buffer solution is 5, and the concentration of the ammonium sulfate buffer solution is 0.075mol/L;
2) Detecting a standard sample solution and a sample solution by using a silica gel reversed-phase C18 chromatographic column respectively, and recording chromatograms of the two solutions;
the flow rate of the mobile phase in the detection process is 1.5ml/min, the detection wavelength is 195nm, and the temperature of a chromatographic column box is 25 ℃;
3) Calculating the purity of the aminoguanidine carbonate by analyzing the two chromatograms;
or alternatively, the process may be performed,
1) Dissolving a standard sample and a sample to be tested by using a mobile phase, and respectively preparing a standard sample solution and a sample solution;
the mobile phase consists of methanol and ammonium sulfate buffer solution, and the volume ratio of the methanol to the ammonium sulfate buffer solution is as follows: 1:99, wherein the pH value of the ammonium sulfate buffer solution is 2.0, and the concentration of the ammonium sulfate buffer solution is 0.075mol/L;
2) Detecting a standard sample solution and a sample solution by using a silica gel reversed-phase C18 chromatographic column respectively, and recording chromatograms of the two solutions;
the flow rate of the mobile phase in the detection process is 0.5ml/min, the detection wavelength is 254nm, and the temperature of a chromatographic column box is 40 ℃;
3) The purity of aminoguanidine carbonate was calculated by analysis of both chromatograms.
2. The method for determining the purity of aminoguanidine carbonate by liquid chromatography according to claim 1, wherein:
the silica gel reversed phase C18 chromatographic column in the step 2) is a Waters Atlantis T3 chromatographic column.
3. The method for determining the purity of aminoguanidine carbonate by liquid chromatography according to claim 1, wherein:
the standard solution was prepared by the following method: weighing 100mg of standard sample into a 100ml volumetric flask, adding a mobile phase for dissolution, and ultrasonically dissolving to fix the volume to a scale;
sample solutions were prepared by the following method: weigh 100mg sample into 100ml volumetric flask, add mobile phase to dissolve, and sonicate to volume to scale.
4. The method for determining the purity of aminoguanidine carbonate by liquid chromatography according to claim 1, wherein: the sample volume in step 2) was 10. Mu.L.
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