CN111351893A - Method for detecting content of guanidine ions in guanidine hydrochloride sample by using ion chromatography - Google Patents
Method for detecting content of guanidine ions in guanidine hydrochloride sample by using ion chromatography Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical analysis, and relates to a method for detecting the content of guanidine ions in a guanidine hydrochloride sample by using ion chromatography. Preparing a standard working solution by using a guanidine hydrochloride standard sample, establishing a standard curve by using the response peak area of the guanidine ion standard sample as a vertical coordinate and using the guanidine ion content as a horizontal coordinate according to the response of guanidine ions in a cation system, and substituting the response peak area of the guanidine ions in the sample into the standard curve to calculate the guanidine ion content in the sample. The method has the advantages of simple operation, rapid detection, no need of complex pretreatment, no toxicity and harm in the detection process, high accuracy and good reproducibility.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, and relates to a method for detecting the content of guanidine ions in a guanidine hydrochloride sample by using ion chromatography.
Background
Guanidine hydrochloride is a white or yellowish block, is used as an intermediate of medicines, pesticides, dyes and other organic compounds, is an important raw material for preparing sulfonamides and folic acid, and can also be used as an antistatic agent for synthetic fibers.
The existing detection method comprises picric acid precipitation method and nuclear magnetic carbon spectrum quantification, but picric acid, also named 2, 4, 6-trinitrophenol, belongs to explosive, is possibly exploded by heating, open fire, friction and impact, belongs to an easy-explosion reagent in dangerous chemicals, is difficult to purchase, and is extremely dangerous. The nuclear magnetic carbon spectrum has more quantitative interference items and overlong detection time.
At present, the ion chromatography does not find a related guanidine hydrochloride detection method, and high performance liquid chromatography detection is proposed by some people, so the ion chromatography is used as a branch of the liquid chromatography, and the ion chromatography detection is tried, and the difficulty lies in that the peak time of guanidine ions and potassium ions is close, specific instrument conditions are required, and certain difficulty is relatively existed.
Disclosure of Invention
Aiming at the problems of the existing detection method, researches show that guanidine hydrochloride exists in the form of guanidine ions and chloride ions in an aqueous solution, so that a sample can be detected by using an ion chromatography. The method has the advantages of simple operation, rapid detection, no need of complex pretreatment, no toxicity and harm in the detection process, high accuracy and good reproducibility.
The invention relates to a method for detecting the content of guanidine ions in a guanidine hydrochloride sample by using ion chromatography, which comprises the following steps:
1) drawing an ion chromatography standard curve: preparing a high-grade pure guanidine hydrochloride sample into a 1000ppm guanidine ion standard stock solution, diluting by 10 times to prepare a 100ppm standard working solution, respectively preparing 2ppm, 5ppm, 10ppm, 20ppm, 40ppm and 100ppm standard solutions, injecting by using an automatic sample injector, carrying out quantitative analysis by an external standard method, carrying out linear regression analysis on the chromatographic peak area of a target compound and the corresponding concentration to obtain a standard curve linear regression equation, wherein the correlation coefficient of the curve is more than or equal to 0.9999. The ion chromatography is used for detecting the content of ppm level, if a small-concentration standard working solution is directly prepared, the weighing error is increased due to the over-small sample weighing, and the calibration curve is influenced.
2) Measuring the content of guanidine ions in a guanidine hydrochloride sample: selecting proper sample weighing amount according to the purity range of a measured sample, using primary water to perform constant volume to a 100mL volumetric flask, filtering the prepared sample solution into a sample feeding bottle by using a filter membrane of 0.45 mu m, using an automatic sample feeder to perform sample feeding, measuring the peak area of a target object, using an external standard method to perform quantification, introducing into a unitary linear regression equation, and calculating the content of guanidine ions in the sample to be measured.
Preferably, the sample weights are generally: the weight of a pure guanidine hydrochloride product or a sample with the content of more than 30 percent is about 0.01g, the weight of a sample with the content of less than 30 percent can be increased by 0.02g, and the weight of waste residues and waste materials with ppm level can be increased to 0.1g and is accurate to 0.0001.
The conductivity of the primary water is less than or equal to 0.01mS/m, wherein the content of suspended matters, particles and ions is the lowest, the requirement of the ion chromatographic column packing is met, meanwhile, the background conductivity value in the detection process is reduced, and the signal-to-noise ratio is improved.
The retention time of the guanidine ions is the peak-off time, the peak-off time is deviated due to different instruments or detection conditions, and the guanidine hydrochloride standard substance is used for rebuilding a standard curve every other one month or two months according to the column efficiency of the chromatographic column, so that the peak-off time of the guanidine ions is determined.
In the process of drawing an ion chromatography standard curve and measuring the content of guanidine ions in a guanidine hydrochloride sample, the column temperature is 25-35 ℃, the flow rate is 0.6-1.0mL/min, the sample amount is 25 mu L, the analysis time is 25min or more, and the leacheate can be 12-16mmol/L methane sulfonic acid aqueous solution.
Preferably, the suppressor current is set in accordance with the eluent concentration, typically in the order of three times the value of the eluent concentration (where the eluent concentration is in mmol/L and the current is in mA).
Preferably, during the assay: the column temperature is 30 ℃, the flow rate is 1.0mL/min, and the leacheate is 16mmol/L methane sulfonic acid aqueous solution.
The column temperature is an optimal value, the service life of the chromatographic column is prolonged, and the optimal temperature of the column effect is maintained; the concentration of the leacheate affects the ion peak time, the 16mmol/L methane sulfonic acid leacheate is optimal, under the concentration of the leacheate, guanidine ions and potassium ions can be separated, and the detection time is saved.
Preferably, in the ion chromatography system adopted in the invention, the protection column is a CG12A protection column with the size of 4 × 50mm, the analytical column is a CS12A cation exchange column with the size of 4 × 250mm, the suppressor is a CERS500 with the size of 4mm, the ion chromatography system further comprises an automatic sample injector, an ion chromatography pump, a six-way valve, a conductivity detector, a data processing system and other conventional configurations, and under the preferable conditions, a standard curve linear regression equation y is 0.1239x-0.0017, and the correlation coefficient of the curve is 1.
The method for detecting the guanidine ions in the guanidine hydrochloride sample is simple and rapid, and a large number of experiments prove that the method has high precision and the accuracy of standard addition recovery, and the test result is accurate and reliable.
Drawings
FIG. 1 standard graph of guanidine ion in example 1;
FIG. 2 is a graph of the chromatographic response of guanidine ion in example 1;
FIG. 3 standard graph of guanidine ion in example 3;
FIG. 4 standard graph of guanidine ion in example 4;
FIG. 5 chromatogram response of guanidine ion in example 4;
FIG. 6 is a graph showing a guanidine ion chromatographic response of a 5ppm guanidine ion standard solution in an experimental example (16 mmol/L methanesulfonic acid aqueous solution as a leacheate, 47mA of suppressor current);
FIG. 7 is a graph showing a guanidine ion chromatographic response of a 5ppm guanidine ion standard solution in an experimental example (eluent was 12mmol/L methanesulfonic acid aqueous solution, and suppressor current was 36 mA).
Detailed Description
The present invention will be described in further detail with reference to the following examples, but it should not be construed that the scope of the above subject matter is limited to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention, and the following embodiments are all completed by adopting the conventional prior art except for the specific description.
Example 1
The existing guanidine hydrochloride solid sample needs to detect the guanidine ion content.
The ion chromatography conditions employed were: the device comprises an automatic sample injector, an ion chromatographic pump, a six-way valve, a protective column CG12A, a size of 4 x 50mm, an analytical column CS12A cation exchange column, a size of 4 x 250mm, a suppressor model of CERS500, a size of 4mm, a conductivity detector, a data processing system, a column temperature of 30 ℃, a flow rate of 1.0mL/min, a suppressor current of 47mA, a sample injection amount of 25 muL, an analysis time of 25min and a leacheate of 16mmol/L methane sulfonic acid aqueous solution.
The method adopts an ion chromatograph to carry out detection and quantitative analysis by an external standard method, and comprises the following specific steps:
(1) preparing a guanidine ion standard stock solution:
0.8181g of guanidine hydrochloride standard sample (molecular weight 95.53, purity 99%) is accurately weighed by an analytical balance to be 0.0001g, and the volume is determined in a 500mL volumetric flask by using primary water to prepare 1000mg/L mother solution (calculated according to guanidine ions, molecular weight 59, if no special indication exists, the same is applied below);
(2) preparing a guanidine ion standard working solution:
transferring 10.00mL of standard stock solution into a 100mL volumetric flask by using a pipette, shaking the solution to a constant volume, and then naming the solution A, transferring 10.00mL of solution A into 25mL,50mL and 100mL volumetric flasks respectively to prepare B, C, D, E solutions with four different concentrations, namely 40mg/L, 20mg/L, 10mg/L and 5mg/L, and transferring the solution D10.00mL into a 50mL volumetric flask to obtain solution F.
(3) Drawing of standard curve
Shaking the standard solutions A, B, C, D, E, F evenly, injecting 25 μ L of the solutions by using an ion chromatography autosampler to obtain peak areas of 12.3818 μ s min, 4.9933 μ s min, 2.4714 μ s min, 1.2333 μ s min, 0.6061 μ s min and 0.2445 μ s min, drawing a guanidine ion standard solution concentration-peak area standard curve, and obtaining a regression equation of the standard curve as follows: 0.1239x-0.0017, R2＝1
In the formula: y is peak area in mus min;
x is the concentration of guanidine ions, and the unit is mg/L;
r: a linear correlation coefficient.
(4) Preparing guanidine hydrochloride sample solution
Accurately weighing 6 parts of 0.01g guanidine hydrochloride sample, accurately weighing the guanidine hydrochloride sample to 0.0001g, fixing the volume in a 100mL volumetric flask, and filtering by using a 0.45 mu m water-phase filter membrane to prepare 6 parts of solution to be detected. The same chromatographic conditions were used for quantitative loop injection at 25 μ L on the same ion chromatograph, while the peak area was recorded.
(5) Calculation of the content of guanidine ions
The calculation formula is as follows:
in the formula:
x: mass fraction of guanidine ions, unit%;
a: peak area, in μ s min;
v: the volume is determined by unit mL;
m: sample weight in g
The experimental data and the detection results are detailed in table 1:
TABLE 1
Precision and spiking recovery tests were performed on example 1:
(1) and (3) precision experiment:
taking the standard working solution of 10.004mg/L prepared in the example, adopting the same instrument, carrying out parallel sample injection for 6 times under the same condition, wherein the detection result is shown in Table 2:
TABLE 2
(2) And (3) standard addition recovery test:
0.8181g of guanidine hydrochloride standard sample (molecular weight 95.53, purity 99%) is accurately weighed by an analytical balance to be 0.0001g, primary water is used for fixing volume in a 500mL volumetric flask to prepare 1000mg/L mother solution, 10.00mL is moved in a 100mL volumetric flask, after the constant volume is shaken up, 10.00mL and 10.00mL are respectively moved in three 100mL volumetric flasks, solutions corresponding to 1mg, 2mg and 3mg of the standard sample are respectively added, after the constant volume is shaken up, the same instrument is adopted, sample injection detection is carried out under the same instrument condition, the standard addition recovery rate of guanidine ions is calculated according to the detection peak area, and the calculation result is shown in Table 3:
TABLE 3
The experimental data show that the method for detecting guanidine ions in the guanidine hydrochloride sample is simple and rapid, the precision degree and the accuracy of standard addition recovery of the method are high, and the test result is accurate and reliable.
Example 2
A batch of guanidine hydrochloride solid samples different from the samples of example 1 were tested for their guanidine ion content:
the ion chromatography conditions employed were: the device comprises an automatic sample injector, an ion chromatographic pump, a six-way valve, a protective column CG12A, a size of 4 x 50mm, an analytical column CS12A cation exchange column, a size of 4 x 250mm, a suppressor model of CERS500, a size of 4mm, a conductivity detector, a data processing system, a column temperature of 30 ℃, a flow rate of 1.0mL/min, a suppressor current of 47mA, a sample injection amount of 25 muL, an analysis time of 25min and a leacheate of 16mmol/L methane sulfonic acid aqueous solution.
The method adopts an ion chromatograph to carry out detection and quantitative analysis by an external standard method, and comprises the following specific steps:
(1) preparing a guanidine ion standard stock solution;
(2) preparing a guanidine ion standard working solution;
(3) drawing a standard curve;
the above steps (1) to (3) are the same as in example 1.
(4) Preparing guanidine hydrochloride sample solution
Accurately weighing 6 parts of 0.01g guanidine hydrochloride sample, accurately weighing the guanidine hydrochloride sample to 0.0001g, fixing the volume in a 100mL volumetric flask, and filtering by using a 0.45 mu m water-phase filter membrane to prepare 6 parts of solution to be detected. The same chromatographic conditions were used for quantitative loop injection at 25 μ L on the same ion chromatograph, while the peak area was recorded.
(5) Calculation of the content of guanidine ions
The calculation formula is as follows:
in the formula:
x: mass fraction of guanidine ions, unit%;
a: peak area, in μ s min;
v: the volume is determined by unit mL;
m: sample weight in g
The experimental data and the test results are detailed in table 4:
TABLE 4
Example 3
The same guanidine hydrochloride solid sample of example 2 was selected and its guanidine ion content was measured:
the ion chromatography conditions employed were: the device comprises an automatic sample injector, an ion chromatographic pump, a six-way valve, a protective column CG12A, a size of 4 x 50mm, an analytical column CS12A cation exchange column, a size of 4 x 250mm, a suppressor model of CERS500, a size of 4mm, a conductivity detector, a data processing system, a column temperature of 30 ℃, a flow rate of 1.0mL/min, a suppressor current of 36mA, a sample injection amount of 25 muL, an analysis time of 25min and a leacheate of 12mmol/L methane sulfonic acid aqueous solution.
(1) Preparing a guanidine ion standard stock solution:
0.8010g of guanidine hydrochloride standard sample (molecular weight 95.53, purity 99%) is accurately weighed by an analytical balance to be 0.0001g, and the volume is determined in a 500mL volumetric flask by using primary water to prepare 1000mg/L mother solution (calculated according to guanidine ions, molecular weight 59, if no special indication exists, the same is applied below);
(2) preparing a guanidine ion standard working solution:
transferring 10.00mL of standard stock solution into a 100mL volumetric flask by using a pipette, shaking the solution to a constant volume, then naming the solution A, transferring 10.00mL of solution A into 25mL,50mL and 100mL volumetric flasks respectively, preparing B, C, D, E solutions with four different concentrations of 40mg/L, 20mg/L, 10mg/L and 5mg/L, taking solution D10.00mL, and fixing the volume into the 100mL volumetric flask to obtain solution F.
(3) Drawing of standard curve
Shaking the standard solution A, B, C, D, E, F uniformly, injecting 25 μ L of the solution by using an ion chromatography autosampler to obtain peak areas of 11.6646 μ s min, 4.4996 μ s min, 2.1587 μ s min, 0.9977 μ s min, 0.5827 μ s min and 0.1008 μ s min, respectively, drawing a guanidine ion standard solution concentration-peak area standard curve, and obtaining a regression equation of the standard curve as shown in fig. 3: 0.1196x-0.1027, R2＝0.9996；
In the formula: y is peak area in mus min;
x is the concentration of guanidine ions, and the unit is mg/L;
R2: a linear correlation coefficient.
(4) Preparing guanidine hydrochloride sample solution
Accurately weighing 6 parts of 0.01g guanidine hydrochloride sample, accurately weighing the guanidine hydrochloride sample to 0.0001g, fixing the volume in a 100mL volumetric flask, and filtering by using a 0.45 mu m water-phase filter membrane to prepare 6 parts of solution to be detected. The same chromatographic conditions were used for quantitative loop injection at 25 μ L on the same ion chromatograph, while the peak area was recorded.
(5) Calculation of the content of guanidine ions
The calculation formula is as follows:
in the formula:
x: mass fraction of guanidine ions, unit%;
a: peak area, in μ s min;
v: the volume is determined by unit mL;
m: sample weight in g
The experimental data and the test results are detailed in table 5:
TABLE 5
Example 4
The same guanidine hydrochloride solid sample of example 2 was selected and its guanidine ion content was measured:
the ion chromatography conditions employed were: the device comprises an automatic sample injector, an ion chromatographic pump, a six-way valve, a protective column CG12A, a size of 4 x 50mm, an analytical column CS12A cation exchange column, a size of 4 x 250mm, a suppressor model of CERS500, a size of 4mm, a conductivity detector, a data processing system, a column temperature of 30 ℃, a flow rate of 0.8mL/min, a suppressor current of 36mA, a sample injection amount of 25 muL, an analysis time of 25min and a leacheate of 12mmol/L methane sulfonic acid aqueous solution.
(1) Preparing a guanidine ion standard stock solution:
0.8010g of guanidine hydrochloride standard sample (molecular weight 95.53, purity 99%) is accurately weighed by an analytical balance to be 0.0001g, and the volume is determined in a 500mL volumetric flask by using primary water to prepare 1000mg/L mother solution (calculated according to guanidine ions, molecular weight 59, if no special indication exists, the same is applied below);
(2) preparing a guanidine ion standard working solution:
transferring 10.00mL of standard stock solution into a 100mL volumetric flask by using a pipette, shaking the solution to a constant volume, then naming the solution A, transferring 10.00mL of solution A into 25mL,50mL and 100mL volumetric flasks respectively, preparing B, C, D, E solutions with four different concentrations of 40mg/L, 20mg/L, 10mg/L and 5mg/L, taking solution D10.00mL, and fixing the volume into the 100mL volumetric flask to obtain solution F.
(3) Drawing of standard curve
Shaking the standard solution A, B, C, D, E, F uniformly, injecting 25 μ L of the solution by using an ion chromatography autosampler to obtain peak areas of 11.6646 μ s min, 4.4996 μ s min, 2.1587 μ s min, 0.9977 μ s min, 0.5827 μ s min and 0.1008 μ s min, respectively, drawing a guanidine ion standard solution concentration-peak area standard curve, and obtaining a regression equation of the standard curve as shown in fig. 3: 0.1237x-0.036, R2＝0.9997
In the formula: y is peak area in mus min;
x is the concentration of guanidine ions, and the unit is mg/L;
R2: a linear correlation coefficient.
(4) Preparing guanidine hydrochloride sample solution
Accurately weighing 6 parts of 0.01g guanidine hydrochloride sample, accurately weighing the guanidine hydrochloride sample to 0.0001g, fixing the volume in a 100mL volumetric flask, and filtering by using a 0.45 mu m water-phase filter membrane to prepare 6 parts of solution to be detected. The same chromatographic conditions were used for quantitative loop injection at 25 μ L on the same ion chromatograph, while the peak area was recorded.
(5) Calculation of the content of guanidine ions
The calculation formula is as follows:
in the formula:
x: mass fraction of guanidine ions, unit%;
a: peak area, in μ s min;
v: the volume is determined by unit mL;
m: sample weight in g
The experimental data and the test results are detailed in table 6:
TABLE 6
Examples of the experiments
The same guanidine ion standard solution with the content of 5ppm is used for carrying out tests by using leachates with different concentrations respectively, and the adopted ion chromatographic conditions are as follows: an automatic sample injector, an ion chromatographic pump, a six-way valve, a protective column CG12A, the size of 4 x 50mm, an analytical column CS12A cation exchange column, the size of 4 x 250mm, the model of a suppressor CERS500, the size of 4mm, a conductivity detector, a data processing system, the column temperature of 30 ℃, the flow rate of 1.0mL/min, the sample injection amount of 25 muL,
① the leacheate is 16mmol/L methane sulfonic acid water solution, and the suppressor current is 47 mA;
② the leacheate is 12mmol/L methane sulfonic acid water solution, and the suppressor current is 36 mA;
the peak effect is shown in figures 6 and 7, wherein figure 6 is a peak appearance diagram of 16mmol/L methane sulfonic acid leacheate, figure 7 is a peak appearance diagram of 12mmol/L methane sulfonic acid leacheate, according to the comparison of the graphs, the peak types, the peak appearance time, the peak broadening and the peak areas of the two spectrograms are different, and the specific data are shown in table 7.
TABLE 7
According to the peak characteristics of the ion chromatography, the lower the concentration of the leacheate, the longer the peak-off time and the larger the peak broadening, the best peak type of the leacheate with the concentration of 16mmol/L can be obtained according to data comparison, the peak-off time is proper, and the concentration of the leacheate is preferably considered within the allowable range of an instrument. If the conditions of the apparatus do not allow, the concentration of 12-16mmol/L can be selected to be suitable for the apparatus.
Claims (8)
1. A method for detecting the content of guanidine ions in a guanidine hydrochloride sample by using ion chromatography is characterized by comprising the following steps:
1) drawing an ion chromatography standard curve: respectively preparing standard solutions of 2ppm, 5ppm, 10ppm, 20ppm, 40ppm and 100ppm of superior pure guanidine hydrochloride, injecting the samples by using an automatic sample injector, carrying out quantitative analysis by an external standard method, and carrying out linear regression analysis on the chromatographic peak area of a target compound and the corresponding concentration to obtain a standard curve linear regression equation;
2) measuring the content of guanidine ions in a guanidine hydrochloride sample: according to the purity range of a measured sample, selecting a sample weighing amount, using primary water to fix the volume to 100mL, injecting a sample solution prepared by using an automatic sample injector, measuring to obtain the peak area of a target object, using an external standard method to quantify, substituting into a standard curve linear regression equation, and calculating the content of guanidine ions in the sample to be measured;
in the processes of drawing an ion chromatography standard curve in the step 1) and measuring the content of guanidine ions in a guanidine hydrochloride sample in the step 2), the column temperature is 25-35 ℃, the flow rate is 0.6-1.0mL/min, the sample injection amount is 25 mu L, the analysis time is 25min or more, and the eluent can be a methane sulfonic acid aqueous solution of 12-16 mmol/L.
2. The method for detecting the content of the guanidine ions in the guanidine hydrochloride sample by using the ion chromatography as claimed in claim 1, wherein in the determination process: the column temperature was 30 ℃ and the flow rate was 1.0 mL/min.
3. The method for detecting the content of guanidine ions in a guanidine hydrochloride sample by using ion chromatography as claimed in claim 1, wherein the eluent is 16mmol/L methane sulfonic acid aqueous solution.
4. The method for detecting the content of guanidine ions in a guanidine hydrochloride sample by using ion chromatography as claimed in claim 1, wherein the weighing in step 2) is as follows: weighing 0.01g of guanidine hydrochloride pure product or sample with the content of more than 30%, weighing 0.02g of guanidine hydrochloride pure product or sample with the content of less than 30%, and weighing 0.1g of guanidine hydrochloride pure product or sample with the content of less than 30%.
5. The method for detecting the content of guanidine ions in a guanidine hydrochloride sample by using ion chromatography as claimed in claim 1, wherein the sample solution in the step 2) is filtered by using a 0.45 μm filter membrane.
6. The method for detecting the content of guanidine ions in a guanidine hydrochloride sample by using ion chromatography as claimed in claim 1, wherein the adopted ion chromatography system comprises a protective column selected from CG12A protective column with the size of 4 × 50mm, and an analytical column adopts CS12A cation exchange column with the size of 4 × 250 mm.
7. The method for detecting the content of guanidine ions in a guanidine hydrochloride sample by using ion chromatography as claimed in claim 6, wherein the ion chromatography system further comprises: the suppressor model is CERS500, size 4 mm.
8. The method for detecting the content of guanidine ions in a guanidine hydrochloride sample by using ion chromatography as claimed in claim 1, wherein the suppressor current is set according to the concentration of the leacheate, wherein the concentration of the leacheate is in units of mmol/L, and the current is in units of mA, and is set according to three times the numerical value of the concentration of the leacheate.
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| CN115266998A (en) * | 2022-08-03 | 2022-11-01 | 成都普康唯新生物科技有限公司 | Method for detecting content of sodium ions in sodium salt molecules |
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