CN112697775A - Method for detecting mercury residual quantity in netilmicin sulfate - Google Patents
Method for detecting mercury residual quantity in netilmicin sulfate Download PDFInfo
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Abstract
The invention provides a method for detecting mercury residual quantity in netilmicin sulfate, which comprises 5 steps, wherein in the step (1), mercury element is taken to prepare linear stock solution and linear solution; preparing a test solution; preparing a standard-added test sample solution; measuring the linear solution in ICP, 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), and measuring the repeatability intermediate precision and the recovery rate of the added standard sample solution. The method realizes the high-efficiency determination of the residual amounts of Cd, Pb, As, Co, V and Ni in netilmicin sulfate by 5 steps, has simple operation steps and good sensitivity, and ensures the safety, effectiveness and controllable quality of the medicine.
Description
Technical Field
The invention relates to the technical field of detection of elemental impurities, in particular to a method for detecting mercury residual quantity in netilmicin sulfate.
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. The emission spectrum analysis method using Inductively Coupled Plasma (ICP) as an excitation light source, referred to as ICP-OES for short, is one of the analysis techniques that are deeply studied and widely applied 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.
Netilmicin sulfate is a semi-synthetic aminoglycoside antibiotic, in the form of white or off-white powder or loose clumps; no odor; it has hygroscopicity. The molecular formula of the netilmicin sulfate is C42H92N10O34S5, and the molecular weight is 1441.55.
Related researches show that the netilmicin has wide antibacterial effect, mainly aims at gram-negative bacilli and a few gram-positive bacilli, and still has antibacterial activity on most strains with drug resistance to aminoglycoside antibiotics. The toxicity of the ear and kidney is lower than that of gentamicin, tobramycin, kanamycin and amikacin. The clinical application is the sulfate thereof. At present, there are three dosage forms of netilmicin sulfate injection, netilmicin sulfate for injection and netilmicin sulfate eye drops.
At present, mercury element impurities can be introduced by using raw and auxiliary materials, process equipment and process water in the production process of netilmicin sulfate. If the content of mercury in the netilmicin sulfate is too high, unknown side effects can be caused, and the treatment effect of the netilmicin sulfate is seriously influenced. Therefore, it is necessary to disclose a detection method capable of detecting the mercury content in netilmicin sulfate based on the prior art.
Disclosure of Invention
The invention aims to disclose a method for detecting mercury residual quantity in netilmicin sulfate, which is used for realizing an efficient detection method for the content of residual mercury elements in the production process.
In order to achieve the aim, the invention provides a method for detecting the residual quantity of mercury in netilmicin sulfate, which comprises the following steps:
taking a proper amount of mercury element standard solution, and adding water to dilute the mercury element standard solution to prepare linear stock solution; taking a proper amount of netilmicin sulfate, adding a proper amount of linear stock solution, and adding water for dilution to prepare a linear solution;
step (2), taking a proper amount of netilmicin sulfate, and dissolving with water to prepare a test solution;
step (3), taking a proper amount of netilmicin sulfate, adding a proper amount of linear stock solution, and dissolving with water to prepare a standard sample solution;
step (4), taking the linear solution to perform measurement in ICP, recording a spectrogram, performing linear regression by taking the sample injection concentration as a horizontal coordinate and the peak area as a vertical coordinate, and obtaining a regression equation;
and (5) sequentially measuring the sample solution and the added standard sample solution according to the steps (2) and (3), and measuring the repeatability intermediate precision and the recovery rate of the added standard sample solution.
In some embodiments, the ICP is model PE Avio 200.
In some embodiments, the ICP pump flow rate is 1.5ml/min, the plasma gas flow rate is 12L/min, the auxiliary gas flow rate is 0.4L/min, the atomization gas flow rate is 0.7L/min, and the power is 1300W.
In some embodiments, the direction of observation of ICP is radial.
In some embodiments, the reproducibility determination in step (5) is in particular: precisely weighing 6 parts of netilmicin sulfate, respectively placing the netilmicin sulfate into measuring flasks, respectively adding the linear stock solutions, adding water for dilution, fixing the volume to a scale, shaking up to obtain a sample solution, and calculating the repeatability.
In some embodiments, the intermediate precision determination in step (5) is specifically: precisely weighing 6 parts of netilmicin sulfate, respectively placing the netilmicin sulfate into measuring flasks, respectively adding the linear stock solutions, adding water for dilution, fixing the volume to a scale, shaking up to obtain a sample solution, and calculating the precision.
In some embodiments, netilmicin sulfate is placed in 10ml measuring vials, and 1ml of the linear stock solution is added, respectively.
In some embodiments, the determination of recovery in step (5) is specifically: precisely weighing 9 parts of netilmicin sulfate, respectively placing the netilmicin sulfate into 10ml measuring bottles, respectively adding 0.8ml, 1.0ml and 1.2ml of linear stock solutions into each three parts of netilmicin sulfate, adding water for dilution, fixing the volume to a scale, shaking up to obtain a sample solution, and calculating the recovery rate under three concentrations.
Compared with the prior art, the invention has the beneficial effects that: the method realizes the efficient determination of the residual quantity of the mercury element in the netilmicin sulfate, has simple operation steps and good sensitivity, and ensures the safety, effectiveness and controllable quality of the medicine.
Drawings
FIG. 1 is a spectrum of a linear solution according to the present invention;
FIG. 2 is a linear plot of a linear solution according to the present invention;
FIG. 3 is a spectrum of a test solution according to the present invention.
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".
Implementation of instruments and reagents:
in this embodiment, an inductively coupled plasma emission spectrometer (ICP) is used, model PE Avio 200.
Raw materials: mercury standard solution and netilmicin sulfate.
The detection conditions are that the wavelength is 194.168nm, the pump flow rate is 1.5ml/min, the used gas is argon, the plasma gas flow rate is 12L/min, the auxiliary gas flow rate is 0.4L/min, the atomization gas flow rate is 0.7L/min, the power is 1300W, and the observation direction is radial.
The detection steps are as follows:
measuring commercial mercury element standard solution Hg0.75ml to 500ml volumetric flasks, diluting the volumetric flasks to scales with water to obtain a linear stock solution I with Hg of 1.5 ug/ml; weighing 275mg of netilmicin sulfate, weighing three parts, respectively placing the three parts into 10ml volumetric flasks, respectively adding 0.5ml, 1.0ml and 5.0ml of linear stock solutions, diluting the linear stock solutions with water to a scale to obtain linear solutions (namely, 0.075ug/ml, 0.15ug/ml and 0.75ug/ml of Hg), and then obtaining a third linear solution, a fourth linear solution and a fourth linear solution.
Weighing 275mg of netilmicin sulfate, placing the netilmicin sulfate into a 10ml volumetric flask, adding water to dissolve the netilmicin sulfate, and fixing the volume to a scale to obtain a test solution.
Weighing 275mg of netilmicin sulfate into a 10ml volumetric flask, adding 0.8ml of linear stock solution, adding water to a constant volume to scale, shaking up, and preparing three parts in parallel as standard sample adding solutions of (v), (v) and (v); weighing 275mg to 10ml of netilmicin sulfate in a volumetric flask, adding 1.0ml of linear stock solution, adding water to dissolve and fix the volume to a scale, shaking up and preparing six parts in parallel as a labeling test solution (solutions) (+, ninu, r, ⑪, ⑫ and ⑬); weighing 275mg of netilmicin sulfate into a 10ml volumetric flask, adding 1.2ml of linear stock solution, adding water to dissolve, fixing the volume to a scale, shaking up and preparing three parts in parallel as standard sample solution ⑭, ⑮ and ⑯.
Step (4), linear measurement: taking water and linear solutions to measure respectively, taking the injection concentration (ug/ml) as an abscissa and the response value as an ordinate, and performing linear regression to obtain a linear equation of y equal to 78.80x +1346.5 and a correlation coefficient of 0.999.
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 mercury element in the sample solution. As shown in fig. 1, the response of elemental mercury at a wavelength of 194.168nm, fig. 2 is a corresponding linear graph, and fig. 3 is the response of elemental mercury in the test sample solution at the corresponding wavelength. And substituting the response value of the mercury element in the test solution into the linear curve to obtain the content of the mercury element in the test solution. Therefore, the detection method can realize efficient and reliable quantitative analysis on the mercury element contained in the netilmicin sulfate, and has high sensitivity.
And (3) repeatability determination: sampling solutions of labeled test products (ninja, r, ⑪, ⑫ and ⑬), recording response values, calculating RSD, and determining repeatability as shown in Table 1.
Table 1: results of repeated measurements
Intermediate precision measurement: six portions of the parallel standard-added test sample solution are prepared again, sample introduction is carried out respectively, response values are recorded, RSD is calculated, and the intermediate precision measurement result is shown in Table 2.
Table 2: results of intermediate precision measurement
And (3) accuracy determination: taking three concentrations of sample solution to be tested, taking sample solutions with low concentration, (+ -) and (c) as solutions with medium concentration, and ⑭, ⑮ and ⑯ as solutions with high concentration, sampling separately and recording response value.
Accuracy is shown by the recovery (%) of the sample addition (measured amount-sample introduced amount)/added amount x 100%. The results of the mercury recovery measurement are shown in Table 3.
Table 3: sample recovery rate measurement result of mercury element
According to the experimental data, the method realizes the high-efficiency determination of the residual quantity of the mercury element in the netilmicin sulfate, and has the advantages of simple operation steps and good sensitivity.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. The method for detecting the residual quantity of mercury in netilmicin sulfate is characterized by comprising the following steps of:
taking a proper amount of mercury element standard solution, and adding water to dilute the mercury element standard solution to prepare linear stock solution; taking a proper amount of netilmicin sulfate, adding a proper amount of linear stock solution, and adding water for dilution to prepare a linear solution;
step (2), taking a proper amount of netilmicin sulfate, and dissolving with water to prepare a test solution;
step (3), taking a proper amount of netilmicin sulfate, adding a proper amount of linear stock solution, and dissolving with water to prepare a standard sample solution;
step (4), taking the linear solution to perform measurement in ICP, recording a spectrogram, performing linear regression by taking the sample injection concentration as a horizontal coordinate and the peak area as a vertical coordinate, and obtaining a regression equation;
and (5) sequentially measuring the sample solution and the added standard sample solution according to the steps (2) and (3), and measuring the repeatability intermediate precision and the recovery rate of the added standard sample solution.
2. The method for detecting the residual amount of mercury in netilmicin sulfate according to claim 1, wherein the ICP type is PE Avio 200.
3. The method for detecting the residual amount of mercury in netilmicin sulfate as claimed in claim 2, wherein the pump flow rate of the ICP is 1.5ml/min, the plasma gas flow rate is 12L/min, the auxiliary gas flow rate is 0.4L/min, the atomization gas flow rate is 0.7L/min, and the power is 1300W.
4. The method for detecting the residual amount of mercury in netilmicin sulfate according to claim 3, wherein the ICP is observed in a radial direction.
5. The method for detecting the residual amount of mercury in netilmicin sulfate according to claim 4, wherein the repetitive determination in the step (5) is specifically as follows: precisely weighing 6 parts of netilmicin sulfate, respectively placing the netilmicin sulfate into measuring flasks, respectively adding the linear stock solutions, adding water for dilution, fixing the volume to a scale, shaking up to obtain a sample solution, and calculating the repeatability.
6. The method for detecting the residual quantity of mercury in netilmicin sulfate according to claim 5, wherein the intermediate precision measurement in the step (5) is specifically as follows: precisely weighing 6 parts of netilmicin sulfate, respectively placing the netilmicin sulfate into measuring flasks, respectively adding the linear stock solutions, adding water for dilution, fixing the volume to a scale, shaking up to obtain a sample solution, and calculating the precision.
7. The method for detecting the residual quantity of mercury in netilmicin sulfate according to claim 5 or 6, wherein netilmicin sulfate is respectively put into 10ml measuring bottles, and 1ml of linear stock solution is respectively added.
8. The method for detecting the residual amount of mercury in netilmicin sulfate according to claim 5, wherein the determination of the recovery rate in step (5) is specifically as follows: precisely weighing 9 parts of netilmicin sulfate, respectively placing the netilmicin sulfate into 10ml measuring bottles, respectively adding 0.8ml, 1.0ml and 1.2ml of linear stock solutions into each three parts of netilmicin sulfate, adding water for dilution, fixing the volume to a scale, shaking up to obtain a sample solution, and calculating the recovery rate under three concentrations.
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Patent Citations (7)
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| CN102607933A (en) * | 2012-02-25 | 2012-07-25 | 云南农业大学 | Method for simultaneously detecting content of four heavy metal elements in tobacco leaves |
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