CN112285248A - Nitrite detection method - Google Patents
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- CN112285248A CN112285248A CN202011612711.6A CN202011612711A CN112285248A CN 112285248 A CN112285248 A CN 112285248A CN 202011612711 A CN202011612711 A CN 202011612711A CN 112285248 A CN112285248 A CN 112285248A
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Abstract
The invention discloses a nitrite detection method, which comprises the following steps: (1) preparing a reference substance and a test solution; (2) and (3) detection: the detection method specifically comprises the following steps: a chromatographic column: thermo Acclaim Trinity P1; mobile phase: potassium dihydrogen phosphate buffer-acetonitrile, volume ratio: 50-65: 35-50; flow rate: 0.4-0.5 mL/min; column temperature: 25-35 ℃; detection wavelength: 205-215 nm; (3) the nitrite content was calculated. The detection method can quickly and accurately detect the content of the nitrite in the test sample, and has good accuracy, precision, reproducibility and stability.
Description
Technical Field
The invention relates to a detection method of nitrite, in particular to a detection method capable of quickly and accurately detecting the content of nitrite.
Background
Nitrite is a generic name of inorganic compounds, widely exists in human environment, is a common nitrogen-containing compound, and is easy to react with amide and the like in an acid environment to generate a strong carcinogen, namely nitrosamine substances. In 7 months in 2018, EMA announces that in known valsartan, a trace amount of genotoxic impurity Nitrosodimethylamine (NDMA) is found, and then FDA publishes a series of genotoxic impurities which are nitrosamine impurities. Nitrite, in turn, acts as a precursor compound for nitrosamines and, therefore, requires source control.
At present, the commonly used detection method of nitrite is diazo coupling spectrophotometry, and the principle of the method is that the nitrite is diazotized with sulfanilamide and then is mixed with hydrochloric acid under the pH value of less than 1.7NThe- (2-naphthalene) -ethylenediamine produces coupling reaction to produce purple azo dye, and the method has the defects of complex sample preparation, influence on detection if the color of a substrate to be detected exists, poor specificity and the like. In addition, the detection of nitrite by ion chromatography has been reported, but the method is expensive in equipment, disadvantageous in popularization of the method, and cannot be used as a conventional means for detecting nitrite.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a nitrite detection method with good accuracy, precision, reproducibility and stability.
The technical scheme is as follows: the detection method of nitrite comprises the following steps:
(1) preparing a reference substance and a test solution;
(2) and (3) detection: the detection method is concretely as follows,
mobile phase: potassium dihydrogen phosphate buffer-acetonitrile, volume ratio: 50-65: 35-50; flow rate: 0.4-0.5 mL/min; column temperature: 25-35 ℃; detection wavelength: 205-215 nm;
(3) the nitrite content was calculated.
Furthermore, the concentration of the reference solution in the step (1) is 10-20 mug/mL, and the concentration of the test solution is 3-10 mg/mL.
Preparing a solvent: and adding 1000mL of acetonitrile into 1000mL of water, shaking up, and performing ultrasonic treatment to obtain the product.
The preparation method of the reference solution comprises the following steps: precisely measuring 5-10 mL of nitrous acid standard ion solution (100 mu g/mL), placing the nitrous acid standard ion solution into a 50mL measuring flask, diluting the nitrous acid standard ion solution to a scale with a solvent, and shaking up to be used as a reference solution (10-20 mu g/mL).
The preparation method of the test solution comprises the following steps: the sample is about 150-500 mg, precisely weighed, placed in a 50mL measuring flask, dissolved by adding a solvent, added to the scale, and shaken up to be used as a sample solution (3-10 mg/mL).
Further, the chromatographic column used in the step (2) is a multimode surface chemical bonding phase chromatographic column, the column length is 30-250 mm, and the granularity of a chromatographic column filler is 1.6-5 μm; the column used was more specifically Thermo Acclaim Trinity P1, column length 150mm, column diameter 3mm, column packing particle size 3 μm.
The preferable chromatographic column can synchronously separate the medicine components and the counter ions thereof, has unique triple surface chemistry, can realize the functions of reverse phase, cation exchange and anion exchange, and achieves the rapid and effective separation of all the components. In addition, hydrophilic ions and ionizable analytes can be effectively retained without an ion-pairing reagent, with low column loss.
Further, the concentration of the potassium dihydrogen phosphate buffer solution in the mobile phase in the step (2) is 10-30 mmol/L.
Further, the volume ratio of the potassium dihydrogen phosphate to the acetonitrile in the mobile phase in the step (2) is 55-65: 35-45.
Further, the sample volumes of the reference solution and the test solution detected in the step (2) are respectively 10-20 muL.
Further, the detector detected in step (2) is an ultraviolet detector.
Further, the detection mode detected in step (2) is a HILIC mode.
Further, the calculation method of the nitrite content in the step (3) is an external standard method.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages:
(1) a brand-new detection method related to the nitrite is established, and the content of the nitrite can be rapidly and accurately determined;
(2) the method is simple and convenient to operate, the content of nitrite can be effectively detected, and the method has the advantages of high sensitivity (the detection limit is 0.9ng and the quantification limit is 3 ng), high accuracy (the linear range is 0.3-20 mug/mL, the r value is greater than 0.999, the recovery rate of the LOQ-150% level is 94% -101% and the RSD is less than 5%), high precision (the RSD is less than 5%), high reproducibility (the RSD is less than 5%) and high stability (a reference product and a test product are stable within 24 hours at room temperature);
(3) has strong adaptability and can be used for the quality control of nitrite in various test samples.
Drawings
FIG. 1 is an HPLC chromatogram of a nitrite control;
FIG. 2 is yet another HPLC chromatogram of a nitrite control;
FIG. 3 is yet another HPLC chromatogram of a nitrite control;
FIG. 4 is an HPLC chromatogram of a nitrite test sample;
FIG. 5 is an HPLC chromatogram of a nitrite spiked test sample;
FIG. 6 is an HPLC chromatogram of the nitrite control of comparative example 1.
Detailed Description
The technical solution of the present invention is further explained below with reference to the examples and the accompanying drawings.
Example 1
(1) Laboratory apparatus and conditions
Thermo U3000 high performance liquid chromatograph, TCC-3000 RS ultraviolet detector
A chromatographic column: thermo Acclaim Trinity P1 (3.0 mm. times.150 mm, 3 μm);
mobile phase: 10mM potassium dihydrogen phosphate buffer-acetonitrile = 55: 45;
flow rate: 0.5 mL/min;
the column temperature is 25 ℃;
sample introduction amount: 10 mu L of the solution;
detection wavelength of the ultraviolet detector: 205 nm.
(2) Experimental procedure
Precisely measuring 10mL of nitrous acid standard ion solution (100. mu.g/mL), placing in a 50mL measuring flask, diluting to scale with solvent, shaking, using as a reference solution (20. mu.g/mL), precisely measuring 10. mu.L of the reference solution, injecting into a liquid chromatograph, and recording chromatogram, wherein the result is shown in FIG. 1.
As can be seen from fig. 1, the nitrite chromatographic peak shape and the separation degree were good using the detection method of the present application.
Example 2
(1) Laboratory apparatus and conditions
Thermo U3000 high performance liquid chromatograph, TCC-3000 RS ultraviolet detector;
a chromatographic column: thermo Acclaim Trinity P1 (3.0 mm. times.150 mm, 3 μm);
mobile phase: 10mM potassium dihydrogen phosphate buffer-acetonitrile = 65: 35;
flow rate: 0.4 mL/min;
column temperature: 35 ℃;
sample introduction amount: 20 mu L of the solution;
detection wavelength of the ultraviolet detector: 215 nm.
(2) Experimental procedure
Precisely measuring 10mL of nitrous acid standard ion solution (100. mu.g/mL), placing in a 100mL measuring flask, diluting with solvent to scale, shaking, using as a reference solution (10. mu.g/mL), precisely measuring 20. mu.L of the reference solution, injecting into a liquid chromatograph, and recording chromatogram, wherein the result is shown in FIG. 2.
As can be seen from fig. 2, the nitrite chromatographic peak shape and the separation degree were good using the detection method of the present application.
Example 3
(1) Laboratory apparatus and conditions
Thermo U3000 high performance liquid chromatograph, TCC-3000 RS ultraviolet detector;
a chromatographic column: thermo Acclaim Trinity P1 (3.0 mm. times.150 mm, 3 μm);
mobile phase: 10mM potassium dihydrogen phosphate buffer-acetonitrile = 60: 40;
flow rate: 0.5 mL/min;
the column temperature is 30 ℃;
sample introduction amount: 20 mu L of the solution;
detection wavelength of the ultraviolet detector: 210 nm.
The experimental steps are as follows: 10mL of a nitrous acid standard ion solution (100. mu.g/mL) was precisely measured, placed in a 100mL measuring flask, diluted to the scale with a solvent, and shaken up to obtain a control solution (10. mu.g/mL).
Taking an unknown sample of about 150mg, precisely weighing, placing in a 50mL measuring flask, adding a solvent to dissolve, adding the solvent to the scale, and shaking up to obtain a sample solution.
Taking an unknown sample of about 150mg, precisely weighing, placing in a 50mL measuring flask, adding a solvent to dissolve, precisely weighing 5mL of nitrite ion reference product mother liquor, placing in the 50mL measuring flask, adding the solvent to a scale, shaking up, and taking as a solution for adding a standard test sample.
Precisely measuring 20 μ L of the reference solution, injecting into liquid chromatograph, and recording chromatogram, the result is shown in FIG. 3.
Precisely measuring 20 μ L of the test solution, injecting into a liquid chromatograph, and recording chromatogram, the result is shown in FIG. 4.
Precisely measuring 20 μ L of the sample solution, injecting into a liquid chromatograph, and recording chromatogram, with the result shown in FIG. 5.
As can be seen from FIGS. 3 to 5, the chromatographic peak shape and the separation degree of nitrite were good by using the detection method of the present application.
Example 4: stability verification
The standard sample solution is prepared according to the method in the embodiment 3, high performance liquid detection is carried out, HPLC chromatograms are respectively measured for 0h, 2h, 4h, 8h, 12h and 24h, the relative retention time of a nitrite chromatographic peak and the RSD value of a relative peak area are calculated, and the result is shown in tables 1-2.
TABLE 1 stability verification-relative peak area and its RSD value
TABLE 2 stability verification-relative Retention time and its RSD value
As can be seen from tables 1-2, the relative retention time of the chromatographic peak of nitrite in the test sample, the relative peak area and the RSD value of the peak area are all less than 5% within 24h, which meets the quality control requirement of high performance liquid chromatography, and shows that the test sample treated by the detection method of the application is stable within 24h at room temperature.
Example 5: precision verification
Taking about 500mg of an unknown sample, preparing a 10mg/mL test solution according to the method in the embodiment 3, carrying out high performance liquid detection, respectively and continuously feeding samples 6 to determine an HPLC chromatogram on different high performance liquid instruments, and calculating the relative retention time and the relative peak area of a nitrite chromatographic peak, wherein the results are shown in tables 3-6.
TABLE 3 precision verification-relative Peak area and its RSD value (Instrument one)
TABLE 4 precision verification-relative retention time and its RSD value (Instrument one)
TABLE 5 precision verification-relative Peak area and its RSD value (second Instrument)
TABLE 6 precision verification-relative retention time and its RSD value (second instrument)
As can be seen from tables 3-6, the relative retention time of the nitrite chromatographic peak in the test sample, the relative peak area and the RSD value of the peak area are all less than 5%, which meet the quality control requirement of the high performance liquid chromatography, and indicate that the detection method of the application has good precision.
Example 6: repeatability verification
A test solution is prepared according to the method in the embodiment 3, 6 parts of the test solution are precisely absorbed, high performance liquid detection is carried out, the relative retention time and the relative peak area of the nitrite chromatographic peak are calculated, and the results are shown in tables 7-8.
TABLE 7 repeatability verification-relative peak area and its RSD value
TABLE 8 repeatability verification-relative retention time and its RSD value
As can be seen from tables 7 to 8, the relative retention time of the nitrite chromatographic peak, the relative peak area and the RSD value of the peak area in the test sample are all less than 5%, and the detection method meets the quality control requirement of the high performance liquid chromatography, and shows that the detection method has good repeatability.
Example 7: linear verification
A proper amount of nitrite standard solution is precisely sucked and added into volumetric flasks with different volumes, the solutions are diluted into a series of solutions with gradient concentration by using a solvent, the determination is carried out according to the chromatographic conditions in the example 1, the concentration (mu g/mL) of the reference solution is taken as an abscissa (X), the peak area is taken as an ordinate (Y), and a standard curve of the nitrite is drawn, and the result is shown in a table 9.
TABLE 9 Standard Curve
TABLE 10 detection and quantitation limits
| Signal-to-noise ratio (S/N) | Detection limit (ng) | Signal-to-noise ratio (S/N) | Quantitative limit (ng) |
| 3.2 | 0.9 | 12.8 | 3 |
As can be seen from tables 9 to 10, the linear coefficients of nitrite are all greater than 0.999, which meets the quality control requirement of high performance liquid chromatography, and shows that the linear relation of nitrite is good in the detection method of the present application.
Example 8: accuracy verification
250mg of a test sample is precisely weighed to obtain 9 parts, 9 parts of 5mg/mL test sample solution is prepared according to the method in the embodiment 3, 3 levels of LOQ concentration (3%), 100% and 150% of reference solution with known content are respectively added, HPLC chromatogram is respectively measured, and the recovery rate of nitrite and RSD value are calculated, and the results are shown in Table 11.
TABLE 11 accuracy verification
As can be seen from Table 11, the recovery rates of the test samples at different concentration levels are 94% -101%, and the RSD is less than 5%, which meets the quality control requirements of high performance liquid chromatography, and shows that the detection method of the application has good accuracy.
Comparative example 1
Precisely measuring 10mL of nitrous acid standard ion solution (100 mu g/mL), placing the nitrous acid standard ion solution into a 100mL measuring flask, diluting the nitrous acid standard ion solution to a scale with a solvent, shaking the nitrous acid standard ion solution to be uniform, using the nitrous acid standard ion solution as a reference solution (10 mu g/mL), precisely measuring 20 mu L of the reference solution, injecting the reference solution into a liquid chromatograph, and performing chromatographic conditions as follows: the chromatographic column is Agilent ZORBAX Eclipse Plus-C18250 mM X4.6 mM, 5 μm, the column temperature is 40 ℃, the detection wavelength is 220nm, the mobile phase is 20mM potassium dihydrogen phosphate buffer-acetonitrile = 80: 20, and the flow rate is 1.0 mL/min; the results are shown in FIG. 6.
As can be seen from FIG. 6, when the detection method of the comparative example is adopted for detection, no nitrite is reserved, which indicates that the detection method of the present application is obtained through screening optimization.
Claims (9)
1. A method for detecting nitrite, the method comprising the steps of:
(1) preparing a reference substance and a test solution;
(2) and (3) detection: the detection method is concretely as follows,
a chromatographic column: thermo Acclaim Trinity P1; mobile phase: potassium dihydrogen phosphate buffer-acetonitrile, volume ratio: 50-65: 35-50; flow rate: 0.4-0.5 mL/min; column temperature: 25-35 ℃; detection wavelength: 205-215 nm;
(3) the nitrite content was calculated.
2. The detection method according to claim 1, wherein the concentration of the control solution in step (1) is 10 to 20 μ g/mL, and the concentration of the test solution is 3 to 10 mg/mL.
3. The detection method according to claim 1, wherein the detection in step (2) is carried out using a column length of 150mm, a column diameter of 3mm, and a column packing particle size of 3 μm.
4. The detection method according to claim 1, wherein the concentration of the potassium dihydrogen phosphate buffer solution in the mobile phase in the step (2) is 10-30 mmol/L.
5. The detection method according to claim 1, wherein the volume ratio of the potassium dihydrogen phosphate to the acetonitrile in the mobile phase in the step (2) is 55-65: 35-45.
6. The detection method according to claim 1, characterized in that the sample volumes of the control solution and the test solution detected in the step (2) are 10-20 μ L respectively.
7. The detection method according to claim 1, wherein the detector detected in step (2) is an ultraviolet detector.
8. The detection method according to claim 1, wherein the detection mode detected in step (2) is a HILIC mode.
9. The method according to claim 1, wherein the nitrite content in step (3) is calculated by an external standard method.
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| CN115128188A (en) * | 2022-07-11 | 2022-09-30 | 天津力生制药股份有限公司 | Detection method for nitrite in metronidazole and metronidazole tablets |
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| CN108918511A (en) * | 2018-05-21 | 2018-11-30 | 上海紫燕食品有限公司 | A kind of detection method of nitrite |
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