CN112683641A - Method for detecting residual amount of aluminum in spiramycin - Google Patents
Method for detecting residual amount of aluminum in spiramycin Download PDFInfo
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- CN112683641A CN112683641A CN202011439476.7A CN202011439476A CN112683641A CN 112683641 A CN112683641 A CN 112683641A CN 202011439476 A CN202011439476 A CN 202011439476A CN 112683641 A CN112683641 A CN 112683641A
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Abstract
The invention discloses a method for detecting residual quantity of aluminum in spiramycin, which comprises the following steps: taking a proper amount of aluminum element standard solution, and adding a nitric acid solution for dilution to prepare a linear stock solution; taking a proper amount of linear stock solution, and adding a nitric acid solution for dilution to prepare a linear solution; taking a proper amount of spiramycin, digesting the spiramycin by using nitric acid, and dissolving the spiramycin by using a nitric acid solution to prepare a test solution; taking a proper amount of spiramycin, digesting the spiramycin by using nitric acid, adding a linear stock solution, and dissolving the spiramycin by using a nitric acid solution to prepare a test solution; measuring the linear solution in an inductively coupled plasma emission spectrometer, recording a spectrogram, and performing linear regression by taking the sample injection concentration as a horizontal coordinate and the peak area as a vertical coordinate to obtain a regression equation; and (5) sequentially measuring the sample solution and the added standard sample solution according to the steps (2) and (3).
Description
Technical Field
The invention relates to the field of detection of elemental impurities, and particularly relates to a method for detecting residual quantity of aluminum in spiramycin.
Background
Plasma emission spectrometry is an emission spectrometry technique in which a plasma torch is used as an excitation light source in a spectroscopic analysis technique. Among them, the emission spectrum analysis method using Inductively Coupled Plasma (ICP) as an excitation light source, abbreviated as ICP-OES, is one of the analysis techniques studied deeply and applied widely and effectively in spectrum analysis. The temperature of the inductively coupled plasma flame moment can reach 6000-8000K, when a sample is introduced into the atomizer through the sample injector and is carried into the flame moment by argon carrier gas, components in the sample are atomized, ionized and excited, and energy is emitted in a light form. When atoms of different elements are excited or ionized, characteristic spectrums with different wavelengths are emitted, so that qualitative analysis can be performed according to the wavelength of characteristic light; when the content of the elements is different, the intensity of the emitted characteristic light is different, and therefore quantitative analysis can be carried out.
Spiramycin is a macrolide antibiotic in white or off-white powder; is bitter in taste; it is slightly hygroscopic. The molecular formula of the spiramycin is C43H74N2O14And the molecular weight is 743.05.
Relevant researches show that the spiramycin has stable character, stronger antibacterial activity and pharmacokinetic property and has a lasting Post-Antibiotic Effect (PAE). The antibacterial agent mainly plays a role in inhibiting bacteria by inhibiting the synthesis of bacterial protein, has a wide antibacterial spectrum, and comprises various gram-positive bacteria and gram-negative bacteria and also comprises some parasites. It can enhance phagocytosis of phagocytes, has side effects obviously lower than those of erythromycin, and is highly sensitive to some gram-positive bacteria (such as streptococcus, staphylococcus, pneumococcus, etc.) and some gram-negative bacteria (such as meningococcus, etc.). In addition, the spiramycin also has better curative effect on penicillin-resistant pathogenic bacteria, so that the spiramycin still has good clinical application and popularization value for treating some infectious diseases. In particular, the spiramycin is a more effective medicament for treating recessive sporozoon diarrhea of an increasing number of AIDS patients.
At present, aluminum element impurities are introduced by using raw and auxiliary materials, process equipment and process water in the production process of spiramycin. If the aluminum content in the spiramycin is too high, unknown side effects can be caused, and the treatment effect of the spiramycin is seriously influenced. Therefore, the benefits of patients are effectively maintained, and the safety, effectiveness and controllable quality of the medicine are ensured, so that a detection method capable of detecting the aluminum content in the spiramycin is required to be disclosed on the basis of the prior art.
Disclosure of Invention
The invention aims to provide a method for detecting the residual quantity of aluminum in spiramycin, which solves one or more of the problems in the prior art.
The invention provides a method for detecting residual quantity of aluminum in spiramycin, which comprises the following steps:
taking a proper amount of aluminum element standard solution, and adding a nitric acid solution for dilution to prepare a linear stock solution; taking a proper amount of linear stock solution, and adding a nitric acid solution for dilution to prepare a linear solution;
taking a proper amount of spiramycin, digesting the spiramycin by using nitric acid, and dissolving the spiramycin by using a nitric acid solution to prepare a test solution;
taking a proper amount of spiramycin, digesting the spiramycin by using nitric acid, adding a linear stock solution, and dissolving the spiramycin by using a nitric acid solution to prepare a test solution;
measuring the linear solution in an inductively coupled plasma emission spectrometer, recording a spectrogram, and performing linear regression by taking the sample injection concentration as a horizontal coordinate and the peak area as a vertical coordinate to obtain a regression equation;
and (5) sequentially measuring the sample solution and the added standard sample solution according to the steps (2) and (3).
In certain embodiments, step (1) is specifically:
measuring an aluminum element standard solution into a volumetric flask, and diluting with a nitric acid solution to obtain a linear stock solution I with the aluminum element concentration of 25 ug/ml; respectively taking 1.0ml, 2.0ml and 4.0ml of linear stock solution, putting the linear stock solution into a volumetric flask, and diluting the linear stock solution with nitric acid solution to obtain linear solutions (namely, linear solutions) (namely, 0.5ug/ml, 1.0ug/ml and 2.0 ug/ml) of aluminum element.
In certain embodiments, the mass fraction of the nitric acid solution in step (1) is 2%.
In certain embodiments, step (2) is specifically:
weighing spiramycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, transferring the spiramycin into a volumetric flask after the digestion is finished and the nitrate is driven, and continuously adding a nitric acid solution for dilution to obtain a test solution.
In certain embodiments, the mass fraction of the nitric acid solution in step (2) is 2%.
In certain embodiments, step (3) is specifically:
weighing spiramycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, transferring the solution into a volumetric flask after nitrate removal, adding linear stock solution, finally adding nitric acid solution for dilution, shaking up and preparing 3 parts in parallel, wherein the solution is used as a sample solution added with a standard sample solution of (fifth), (sixth) and (seventh); weighing spiramycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, transferring the solution into a volumetric flask after the nitrate removal is finished, adding linear stock solution, finally adding nitric acid solution for dilution, shaking up and preparing 6 parts in parallel as a solution (r, ninx, r) for the sample to be added,
(ii) a Weighing spiramycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, transferring the solution into a volumetric flask after the digestion is finished and the nitrate is removed, adding a linear stock solution, finally adding a nitric acid solution for dilution, shaking up and preparing 3 parts in parallel to be used as a solution for adding a standard test sample
。
In certain embodiments, the mass fraction of the nitric acid solution in step (3) is 2%.
In certain embodiments, step (4) is specifically:
respectively measuring a nitric acid solution with the mass fraction of 2% and linear solutions II, III and IV, and performing linear regression by taking the sample injection concentration (ug/ml) as a horizontal coordinate and the response value as a vertical coordinate to obtain a linear equation.
In certain embodiments, the inductively coupled plasma emission spectrometer of step (4) is of the type PE Avio200, wavelength 396.153nm, pump flow rate of 1.5ml/min, argon gas as the gas used, plasma gas flow rate of 12L/min, auxiliary gas flow rate of 0.4L/min, atomization gas flow rate of 0.7L/min, power of 1300W, and radial direction of view.
In certain embodiments, step (5) further comprises performing a reproducible intermediate precision and recovery assay on the spiked test sample solution.
In certain embodiments, the reproducibility and intermediate precision measurements in step (5) are specifically: and precisely weighing 6 parts of spiramycin, performing microwave digestion, respectively placing the spiramycin into 50ml measuring flasks, respectively adding 2ml of linear stock solution, adding 2% nitric acid solution for dilution, shaking up to be used as a sample solution, and calculating repeatability and precision.
In certain embodiments, the determination of recovery in step (5) is specifically: precisely weighing 9 parts of spiramycin, respectively placing the spiramycin into 50ml measuring flasks after microwave digestion, respectively adding 1.6ml, 2.0ml and 2.4ml of linear stock solutions into each three parts of spiramycin, adding 2% nitric acid solution for dilution, shaking up the spiramycin to serve as a sample solution, and calculating the recovery rate under three concentrations.
Wherein: digestion, also called wet digestion, is a method of destroying organic substances or reducing substances in a sample by using acid liquor or alkali liquor under the condition of heating.
Has the advantages that: the method realizes the high-efficiency determination of the residual quantity of aluminum in the spiramycin, and has simple operation and good sensitivity.
Drawings
FIG. 1 is a spectrum of a linear solution;
FIG. 2 is a linear solution line graph;
FIG. 3 is a spectrum of a test solution.
Detailed Description
The present invention is described in detail with reference to the embodiments shown in the drawings, but it should be understood that these embodiments are not intended to limit the present invention, and those skilled in the art should understand that functional, methodological, or structural equivalents or substitutions made by these embodiments are within the scope of the present invention.
Unless otherwise specified in the specification, analytical grade is used for the components and raw materials in each embodiment of the invention. In addition, "g" and "mg" in each example are the weight units "g" and "mg", respectively; "ml" is the volume unit "ml".
Laboratory apparatus and reagent
An experimental instrument: the model of an inductively coupled plasma emission spectrometer (ICP) is PE Avio 200;
reagent: standard solution of aluminum element, spiramycin and nitric acid;
detection conditions are as follows: the wavelength was 396.153nm, the pump flow rate was 1.5ml/min, the gas used was argon, the plasma gas flow rate was 12L/min, the auxiliary gas flow rate was 0.4L/min, the atomization gas flow rate was 0.7L/min, the power was 1300W, and the observation direction was radial.
A detection step:
measuring commercially available element standard liquid Al (2.5ml) into a volumetric flask of 250ml, and diluting the volumetric flask to a scale by using a 2% nitric acid solution to obtain a linear stock solution (I) with the Al of 25 ug/ml; respectively taking 1.0ml, 2.0ml and 4.0ml of linear stock solution, putting the linear stock solution into a 50ml volumetric flask, diluting the linear stock solution to a scale by using 2% nitric acid solution to obtain linear solutions (namely 0.5ug/ml, 1.0ug/ml and 2.0 ug/ml) of Al;
weighing 200mg (180-220 mg) of spiramycin in a polytetrafluoroethylene tank, adding 5ml of nitric acid for digestion, transferring the mixture into a 50ml volumetric flask after the digestion is finished and the nitrate is removed, and adding 2% nitric acid solution to a constant volume to reach a scale to be used as a test solution;
weighing 200mg (180 mg-220 mg) of spiramycin in a polytetrafluoroethylene tank, adding 5ml of nitric acid for digestion, transferring the solution into a 50ml volumetric flask after the nitrate removal is finished, adding 1.6ml of linear stock solution, adding 2% nitric acid solution for constant volume to scale, shaking up, and preparing three parts in parallel as standard sample adding solutions (fifthl, sixty and seventy); weighing 200mg (180 mg-220 mg) of spiramycin in a polytetrafluoroethylene tank, adding 5ml of nitric acid for digestion, transferring the mixture into a 50ml volumetric flask after the digestion is finished and the nitrate is removed, adding 2.0ml of linear stock solution, adding 2 percent nitric acid solution to a constant volume to scale, shaking up and preparing six parts in parallel as solution for adding a standard sample (III, ninu, R),
(ii) a Weighing 200mg (180-220 mg) of spiramycin in a polytetrafluoroethylene tank, adding 5ml of nitric acid for digestion, transferring to 50ml of capacity after the digestion is finished and nitrate is removedAdding 2.4ml of linear stock solution into a bottle, adding 2% nitric acid solution to a constant volume to scale, shaking up, and preparing three parts in parallel as a solution for adding a standard test sample
；
Step (4), linear measurement: respectively measuring a 2% nitric acid solution and linear solutions (namely, the second solution, the third solution and the fourth solution), performing linear regression by taking the injection concentration (ug/ml) as an abscissa and the response value as an ordinate to obtain a linear equation of y which is 40530x-12.3 and a correlation coefficient of 1.000;
step (5), testing the test solution: and sampling the sample solution, substituting the obtained response value into a linear equation, and calculating the concentration of the aluminum element in the sample solution. In FIG. 1, the response of Al element at a wavelength of 396.153nm, in FIG. 2, the corresponding linear curve is shown, and in FIG. 3, the response of Al element in the test solution at the corresponding wavelength is shown. And substituting the response value of the Al element in the test solution into the linear curve to obtain the content of the Al element in the test solution. Therefore, the detection method can realize high-efficiency and reliable quantitative analysis on the Al element contained in the spiramycin, and has high sensitivity.
And (3) repeatability determination: taking solution of labeled test article (ninthly, R),
Separately, the samples were injected, the response values were recorded, and the RSD was calculated, the results are shown in table 1 (reproducibility measurement results).
TABLE 1
Intermediate precision measurement: another laboratory technician, prepare six test solutions of the parallel standard, inject sample separately, record the response value, calculate RSD, the result is shown in Table 2 (intermediate precision measurement result).
TABLE 2
And (3) accuracy determination: taking three concentrations of standard sample solution, three parts of each concentration, low concentration solution, middle concentration solution, high concentration solution and high concentration solution
And respectively injecting samples and recording response values.
Accuracy is shown by the recovery (%) of the sample addition (measured amount-sample introduced amount)/added amount x 100%. The results of the sample recovery of aluminum are shown in Table 3.
TABLE 3
In summary, the following steps: the method realizes the high-efficiency determination of the residual quantity of aluminum in the spiramycin, and has simple operation and good sensitivity.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these should be considered as within the scope of the present invention.
Claims (9)
1. A method for detecting the residual amount of aluminum in spiramycin is characterized by comprising the following steps:
taking a proper amount of aluminum element standard solution, and adding a nitric acid solution for dilution to prepare a linear stock solution; taking a proper amount of linear stock solution, and adding a nitric acid solution for dilution to prepare a linear solution;
taking a proper amount of spiramycin, digesting the spiramycin by using nitric acid, and dissolving the spiramycin by using a nitric acid solution to prepare a test solution;
taking a proper amount of spiramycin, digesting the spiramycin by using nitric acid, adding a linear stock solution, and dissolving the spiramycin by using a nitric acid solution to prepare a test solution;
measuring the linear solution in an inductively coupled plasma emission spectrometer, recording a spectrogram, and performing linear regression by taking the sample injection concentration as a horizontal coordinate and the peak area as a vertical coordinate to obtain a regression equation;
and (5) sequentially measuring the sample solution and the added standard sample solution according to the steps (2) and (3).
2. The detection method according to claim 1, wherein the step (1) is specifically:
measuring an aluminum element standard solution into a volumetric flask, and diluting with a nitric acid solution to obtain a linear stock solution I with the aluminum element concentration of 25 ug/ml; respectively taking 1.0ml, 2.0ml and 4.0ml of linear stock solution, putting the linear stock solution into a volumetric flask, and diluting the linear stock solution with nitric acid solution to obtain linear solutions (namely, linear solutions) (namely, 0.5ug/ml, 1.0ug/ml and 2.0 ug/ml) of aluminum element.
3. The detection method according to claim 2, wherein the mass fraction of the nitric acid solution in the step (1) is 2%.
4. The detection method according to claim 1, wherein the step (2) is specifically:
weighing spiramycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, transferring the spiramycin into a volumetric flask after the digestion is finished and the nitrate is driven, and continuously adding a nitric acid solution for dilution to obtain a test solution.
5. The detection method according to claim 4, wherein the mass fraction of the nitric acid solution in the step (2) is 2%.
6. The detection method according to claim 1, wherein the step (3) is specifically:
weighing spiramycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, transferring the solution into a volumetric flask after nitrate removal, adding linear stock solution, finally adding nitric acid solution for dilution, shaking up and preparing 3 parts in parallel, wherein the solution is used as a sample solution added with a standard sample solution of (fifth), (sixth) and (seventh); weighing spiramycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, transferring the solution into a volumetric flask after the nitrate removal is finished, adding linear stock solution, finally adding nitric acid solution for dilution, shaking up and preparing 6 parts in parallel as a solution (r, ninx, r) for the sample to be added,
Weighing spiramycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, transferring the solution into a volumetric flask after the digestion is finished and the nitrate is removed, adding a linear stock solution, finally adding a nitric acid solution for dilution, shaking up and preparing 3 parts in parallel to be used as a solution for adding a standard test sample
7. The detection method according to claim 6, wherein the mass fraction of the nitric acid solution in the step (3) is 2%.
8. The detection method according to claim 1, wherein the step (4) is specifically:
respectively measuring a nitric acid solution with the mass fraction of 2% and linear solutions II, III and IV, and performing linear regression by taking the sample injection concentration (ug/ml) as a horizontal coordinate and the response value as a vertical coordinate to obtain a linear equation.
9. The detection method according to claim 1, wherein the inductively coupled plasma emission spectrometer of step (4) is of a type PE Avio200, a wavelength of 396.153nm, a pump flow rate of 1.5ml/min, argon is used as a gas, a plasma gas flow rate of 12L/min, an auxiliary gas flow rate of 0.4L/min, an atomization gas flow rate of 0.7L/min, a power of 1300W, and a radial direction is observed.
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Application publication date: 20210420 |