CN112763479A - Method for detecting residual amounts of Cd, Pb, As, Hg, Co, V and Ni in mitomycin - Google Patents
Method for detecting residual amounts of Cd, Pb, As, Hg, Co, V and Ni in mitomycin Download PDFInfo
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- 229930192392 Mitomycin Natural products 0.000 title claims abstract description 54
- NWIBSHFKIJFRCO-WUDYKRTCSA-N Mytomycin Chemical compound C1N2C(C(C(C)=C(N)C3=O)=O)=C3[C@@H](COC(N)=O)[C@@]2(OC)[C@@H]2[C@H]1N2 NWIBSHFKIJFRCO-WUDYKRTCSA-N 0.000 title claims abstract description 54
- 229960004857 mitomycin Drugs 0.000 title claims abstract description 54
- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 26
- 229910052745 lead Inorganic materials 0.000 title claims abstract description 26
- 229910052753 mercury Inorganic materials 0.000 title claims abstract description 26
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 26
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 26
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 67
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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Abstract
The invention discloses a method for detecting residual amounts of Cd, Pb, As, Hg, Co, V and Ni in mitomycin, which comprises the following steps: step (1), preparing a linear stock solution and a linear solution; step (2), taking a proper amount of mitomycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, and adding a nitric acid solution for dissolution to prepare a test sample solution; step (3), putting a proper amount of mitomycin into a polytetrafluoroethylene tank, adding nitric acid for digestion, adding a linear stock solution, and finally dissolving with a nitric acid solution to prepare a standard sample solution; step (4), taking a linear solution to measure in an inductively coupled plasma emission spectrometer, recording a spectrogram, and performing linear regression 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 amounts of Cd, Pb, As, Hg, Co, V and Ni in mitomycin.
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 the excitation light source, abbreviated as ICP-OES, is one of the analysis techniques studied deeply and applied widely and effectively in the 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 also different, and accordingly quantitative analysis can be performed.
Mitomycin is an antibiotic obtained from Streptomyces culture fluid, and is blue purple crystal or crystalline powder; dissolving in acetone, ethyl acetate and cyclohexanone, and slightly dissolving in water. The molecular formula of mitomycin is C15H18N4O5And the molecular weight is 334.33.
Mitomycin is an antineoplastic drug, and related researches show that mitomycin contains an active group with alkylation action, can form cross connection with purine on DNA to inhibit DNA synthesis, and can also cause DNA single-strand breakage and chromosome breakage. Mitomycin has a broad-spectrum anti-tumor effect, is a drug with nonspecific cell cycle, has an antibacterial effect, and has a stronger effect on gram-positive bacteria than on gram-negative bacteria.
At present, Cd, Pb, As, Hg, Co, V and Ni element impurities are introduced by using raw and auxiliary materials, process equipment and process water in the production process of mitomycin. If the content of Cd, Pb, As, Hg, Co, V and Ni in mitomycin is too high, unknown side effects can be caused and the treatment effect of mitomycin is seriously influenced. Therefore, the benefits of patients are effectively maintained, the safety, the effectiveness and the controllable quality of the medicines are ensured, and a detection method capable of detecting the contents of Cd, Pb, As, Hg, Co, V and Ni in mitomycin 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 Cd, Pb, As, Hg, Co, V and Ni in mitomycin, which solves one or more of the problems in the prior art.
The invention provides a method for detecting residual amounts of Cd, Pb, As, Hg, Co, V and Ni in mitomycin, which comprises the following steps:
taking a proper amount of standard solution of Cd, Pb, As, Hg, Co, V and Ni elements, and adding a nitric acid solution to dilute to prepare linear stock solution; taking a proper amount of linear stock solution, and adding a nitric acid solution for dilution to prepare a linear solution;
step (2), taking a proper amount of mitomycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, and then adding a nitric acid solution for dissolution to prepare a test sample solution;
step (3), putting a proper amount of mitomycin into a polytetrafluoroethylene tank, adding nitric acid for digestion, adding a linear stock solution, and finally dissolving with a nitric acid solution to prepare a standard sample 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 each element standard solution into a volumetric flask, and diluting with a nitric acid solution to obtain linear stock solutions (I) of Cd, Pb, As, Hg, Co, V and Ni which are respectively 10ug/ml, 25ug/ml, 75ug/ml, 15ug/ml, 25ug/ml, 50ug/ml and 100 ug/ml;
respectively taking 1.0ml, 2.0ml and 5.0ml of linear stock solution, placing the linear stock solution in a volumetric flask, and diluting with a nitric acid solution to obtain Cd of 0.2ug/ml, 0.4ug/ml and 1.0ug/ml respectively; pd is 0.5ug/ml, 1.0ug/ml and 2.5ug/ml respectively; as is 1.5ug/ml, 3.0ug/ml and 7.5ug/ml respectively; hg is respectively 0.3ug/ml, 0.6ug/ml and 1.5 ug/ml; co is 0.5ug/ml, 1.0ug/ml and 2.5ug/ml respectively; v is 1.0ug/ml, 2.0ug/ml and 5.0ug/ml respectively; ni is 2.0ug/ml, 4.0ug/ml and 10.0ug/ml respectively.
In certain embodiments, the mass fraction of the nitric acid solution in step (1) is 2%.
In certain embodiments, the mass of mitomycin in step (2) is from 45 to 50mg and the amount of nitric acid added to effect digestion is 5 ml.
In certain embodiments, the mass fraction of nitric acid in step (2) is 2%.
In certain embodiments, step (3) is specifically:
s1, weighing mitomycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, transferring to a volumetric flask, adding a linear stock solution, finally adding a nitric acid solution for dissolution and dilution, shaking up and preparing 3 parts in parallel, wherein the 3 parts are used as standard sample adding solutions of (fifth), (sixth) and (seventh);
s2, weighing mitomycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, transferring to a volumetric flask, adding linear stock solution, finally adding nitric acid solution for dissolution and dilution, shaking up and preparing 6 parts in parallel as a solution for the test object to be labeled (r, ninx, r),
S3, weighing mitomycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, transferring to a volumetric flask, adding a linear stock solution, finally adding a nitric acid solution for dissolution and dilution, shaking up and preparing 3 parts in parallel to serve as a solution for adding a standard test sample
In certain embodiments, the mass of mitomycin in step S1 is 45 to 50mg, the amount of nitric acid added to perform the digestion is 5ml, the volume of the linear stock solution is 0.8ml, and the mass fraction of nitric acid solution is 2%.
In certain embodiments, the amount of the rip mycin in step S2 is 45 to 50mg, the amount of nitric acid added for digestion is 5ml, the volume of the linear stock solution is 1.0ml, and the mass fraction of the nitric acid solution is 2%.
In certain embodiments, the mass of mitomycin in step S3 is 45 to 50mg, the amount of nitric acid added to perform the digestion is 5ml, the volume of the linear stock solution is 1.2ml, and the mass fraction of nitric acid solution is 2%.
In some embodiments, the inductively coupled plasma emission spectrometer of step (4) is of the type PE Avio 200, the 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, the power is 1300W, and the observation direction is radial.
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: precisely weighing 6 parts of mitomycin, respectively placing the mitomycin in a polytetrafluoroethylene tank, adding 5ml of nitric acid for digestion, transferring the mitomycin to a 25ml volumetric flask, adding 1.0ml of linear stock solution, dissolving the mitomycin by using 2% nitric acid solution, and fixing the volume to a scale to obtain a sample solution, and calculating the repeatability and the precision.
In certain embodiments, the determination of recovery in step (5) is specifically: precisely weighing 9 parts of mitomycin, respectively placing the mitomycin in a polytetrafluoroethylene tank, adding 5ml of nitric acid for digestion, transferring the mitomycin to a 25ml volumetric flask, adding 1.0ml of linear stock solution, dissolving the mitomycin by using 2% nitric acid solution, fixing the volume to the scale to obtain a sample solution, adding 0.8ml of linear stock solution, 1.0ml of linear stock solution and 1.2ml of linear stock solution into each three parts of the mitomycin, dissolving the mitomycin by using 2% nitric acid solution, fixing the volume to the scale, shaking up the mitomycin to obtain the sample solution, and calculating the recovery rates of the mitomycin under three concentrations.
Has the advantages that: the method realizes the high-efficiency determination of the residual amounts of Cd, Pb, As, Hg, Co, V and Ni in mitomycin, and has the advantages of simple operation and good sensitivity.
Drawings
FIG. 1 is a spectrum of a Cd linear solution;
FIG. 2 is a spectrum of a Pb linear solution;
FIG. 3 is a spectrum of As linear solution
FIG. 4 is a spectrum of a Hg linear solution;
FIG. 5 is a spectrum of a Co linear solution;
FIG. 6 is a spectrum of a V-line solution;
FIG. 7 is a spectrum of a Ni linear solution;
FIG. 8 is a linear diagram of Cd, Pb, As, Hg, Co, V, Ni linear solutions;
FIG. 9 is a spectrum of Cd in the test solution;
FIG. 10 is a graph showing the spectrum of Pb in the test solution;
FIG. 11 is a spectrum of As in the test solution;
FIG. 12 is a graph showing Hg spectra in the test solution;
FIG. 13 is a chart of Co in the test solution;
FIG. 14 is a graph showing the spectrum of V in the test solution;
FIG. 15 is a spectrum of Ni in the 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;
experimental reagent: cd. Standard solutions of Pb, As, Hg, Co, V and Ni elements, mitomycin and nitric acid;
detection conditions are as follows: the 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, the power is 1300W, and the observation direction is radial.
A detection step:
measuring commercially available standard element solutions Cd, Pb, As, Hg, Co, V and Ni into bottles with the capacity of 0.5ml, 1.25ml, 3.75ml, 0.75ml, 1.25ml, 2.5ml and 5.0ml to 50ml respectively, and diluting the bottles to scale by using a 2% nitric acid solution to obtain linear stock solutions I with the capacity of 10ug/ml, 25ug/ml, 75ug/ml, 15ug/ml, 25ug/ml, 50ug/ml and 100ug/ml respectively for Cd, Pb, As, Hg, Co, V and Ni; respectively taking 1.0ml, 2.0ml and 5.0ml of linear stock solution, placing the linear stock solution in a 50ml volumetric flask, and diluting the linear stock solution to a scale by using 2% nitric acid solution to obtain Cd of 0.2ug/ml, 0.4ug/ml and 1.0ug/ml respectively; pd is 0.5ug/ml, 1.0ug/ml and 2.5ug/ml respectively; as is 1.5ug/ml, 3.0ug/ml and 7.5ug/ml respectively; hg is respectively 0.3ug/ml, 0.6ug/ml and 1.5 ug/ml; co is 0.5ug/ml, 1.0ug/ml and 2.5ug/ml respectively; v is 1.0ug/ml, 2.0ug/ml and 5.0ug/ml respectively; ni is 2.0ug/ml, 4.0ug/ml and 10.0ug/ml of linear solutions (II), (III) and (IV) respectively;
weighing 50mg (45-50 mg) of mitomycin in a polytetrafluoroethylene tank, adding 5ml of nitric acid for digestion, transferring to a 25ml volumetric flask, adding a 2% nitric acid solution for dissolution, and fixing the volume to the standard degree to prepare a test solution;
weighing 50mg (45-50 mg) of mitomycin in a polytetrafluoroethylene tank, adding 5ml of nitric acid for digestion, transferring to a 25ml volumetric flask, adding 0.8ml of linear stock solution, adding 2% nitric acid solution for dissolving, fixing the volume to scale, shaking up, and preparing three parts in parallel as a labeled sample solution (fifth, sixth and seventh); weighing 50mg (45-50 mg) of mitomycin in a polytetrafluoroethylene tank, adding 5ml of nitric acid for digestion, transferring to a 25ml volumetric flask, adding 1.0ml of linear stock solution, adding 2% nitric acid solution for dissolution, fixing the volume to a scale, shaking up and preparing six parts in parallel as a solution for adding a standard sample (red, ninu, red, blue, green, blue),
Weighing 50mg (45-50 mg) of mitomycin in a polytetrafluoroethylene tank, adding 5ml of nitric acid for digestion, transferring to a 25ml volumetric flask, adding 1.2ml of linear stock solution, adding 2% nitric acid solution for dissolution, fixing the volume to a scale, shaking up, and preparing three parts in parallel to serve as a solution for adding a standard sample
Step (4), linear measurement: respectively measuring 2% nitric acid solution and linear solutions (II, III and IV), taking the sample injection concentration (ug/ml) as an abscissa and the response value as an ordinate, and performing linear regression to obtain a linear equation of Cd: y is 1000000x-1069.2 with a correlation coefficient of 1.000; pd: y 5613x-106.6, correlation coefficient 1.000; as: 1050x-163.8 with a correlation coefficient of 0.999; hg: y 4356x + 54.3; co: y is 38670x +54.3, and the correlation coefficient is 1.000; v: 73000x-2835.3 with a correlation coefficient of 1.000; ni: 42860x-3001.8, with a correlation coefficient of 1.000;
step (5), testing the test solution: and sampling the sample solution, substituting the obtained response values into a linear equation, and calculating the concentrations of Cd, Pb, As, Hg, Co, V and Ni elements in the sample solution. In FIGS. 1-7, the Cd, Pb, As, Hg, Co, V, Ni elements respectively respond at the wavelengths of 228.802nm, 220.353nm, 188.979nm, 194.168nm, 228.616nm, 292.464nm, 231.604nm, FIGS. 8-9 are corresponding linear curves, and FIGS. 10-15 are the responses of Cd, Pb, As, Hg, Co, V, Ni elements in the test solution at the corresponding wavelengths. The content of each element in the test solution can be obtained by substituting the response values of Cd, Pb, As, Hg, Co, V and Ni elements in the test solution into a linear curve. Therefore, the detection method can realize efficient and reliable quantitative analysis on Cd, Pb, As, Hg, Co, V and Ni elements contained in mitomycin, and has high sensitivity.
And (3) repeatability determination: taking solution of labeled test article (ninthly, R),
The samples were injected separately, the response values recorded, and the RSD calculated, the results are shown in Table 1 (repeatability measurements).
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 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%. Cd. The results of the sample recovery measurements of Pb, As, Hg, Co, V, and Ni elements are shown in tables 3-9, respectively.
TABLE 3
TABLE 4
TABLE 5
TABLE 6
TABLE 7
TABLE 8
TABLE 9
In summary, the following steps: the method realizes the high-efficiency determination of the residual amounts of Cd, Pb, As, Hg, Co, V and Ni in mitomycin, and has the advantages of 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 (10)
1. A method for detecting the residual amounts of Cd, Pb, As, Hg, Co, V and Ni in mitomycin is characterized by comprising the following steps:
taking a proper amount of standard solution of Cd, Pb, As, Hg, Co, V and Ni elements, and adding a nitric acid solution to dilute to prepare linear stock solution; taking a proper amount of linear stock solution, and adding a nitric acid solution for dilution to prepare a linear solution;
step (2), taking a proper amount of mitomycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, and adding a nitric acid solution for dissolution to prepare a test sample solution;
step (3), putting a proper amount of mitomycin into a polytetrafluoroethylene tank, adding nitric acid for digestion, adding a linear stock solution, and finally dissolving with a nitric acid solution to prepare a standard sample 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 each element standard solution into a volumetric flask, and diluting with a nitric acid solution to obtain linear stock solutions (I) of Cd, Pb, As, Hg, Co, V and Ni which are respectively 10ug/ml, 25ug/ml, 75ug/ml, 15ug/ml, 25ug/ml, 50ug/ml and 100 ug/ml;
respectively taking 1.0ml, 2.0ml and 5.0ml of linear stock solution, placing the linear stock solution in a volumetric flask, and diluting with a nitric acid solution to obtain Cd of 0.2ug/ml, 0.4ug/ml and 1.0ug/ml respectively; pd is 0.5ug/ml, 1.0ug/ml and 2.5ug/ml respectively; as is 1.5ug/ml, 3.0ug/ml and 7.5ug/ml respectively; hg is respectively 0.3ug/ml, 0.6ug/ml and 1.5 ug/ml; co is 0.5ug/ml, 1.0ug/ml and 2.5ug/ml respectively; v is 1.0ug/ml, 2.0ug/ml and 5.0ug/ml respectively; ni is 2.0ug/ml, 4.0ug/ml and 10.0ug/ml respectively.
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 mass of mitomycin in step (2) is 45 to 50mg and the amount of nitric acid added for digestion is 5 ml.
5. The detection method according to claim 4, wherein the mass fraction of nitric acid in the step (2) is 2%.
6. The detection method according to claim 1, wherein the step (3) is specifically:
s1, weighing mitomycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, transferring to a volumetric flask, adding a linear stock solution, finally adding a nitric acid solution for dissolution and dilution, shaking up and preparing 3 parts in parallel as a standard sample solution (c), (c) and (c);
s2, weighing mitomycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, transferring to a volumetric flask, adding linear stock solution, finally adding nitric acid solution for dissolution and dilution, shaking up and preparing 6 parts in parallel as a solution for adding the standard sample (r, c, r),
S3, weighing mitomycin in a polytetrafluoroethylene tank, adding nitric acid for digestion, transferring to a volumetric flask, adding linear stock solution, finally adding nitric acid solution for dissolution and dilution, shaking up and preparing 3 parts in parallel as a solution for adding a standard test sample
7. The detection method according to claim 6, wherein the mass of mitomycin in step S1 is 45-50 mg, the amount of nitric acid added for digestion is 5ml, the volume of the linear stock solution is 0.8ml, and the mass fraction of the nitric acid solution is 2%.
8. The detection method according to claim 6, wherein the mass of the rip mycin in the step S2 is 45-50 mg, the addition amount of the nitric acid for digestion is 5ml, the volume of the linear stock solution is 1.0ml, and the mass fraction of the nitric acid solution is 2%.
9. The detection method according to claim 6, wherein the mass of mitomycin in step S3 is 45-50 mg, the amount of nitric acid added for digestion is 5ml, the volume of the linear stock solution is 1.2ml, and the mass fraction of the nitric acid solution is 2%.
10. The detection method according to claim 1, wherein the inductively coupled plasma emission spectrometer of step (4) is of type PE Avio 200, the 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, the power is 1300W, and the observation direction is radial.
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Citations (3)
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| CN103018316A (en) * | 2012-12-04 | 2013-04-03 | 漳州片仔癀药业股份有限公司 | Method for detecting heavy metal elements in anti-inflammatory and analgesic bolus by inductively coupled plasma mass spectrometric method |
| CN109374807A (en) * | 2018-11-07 | 2019-02-22 | 南京明捷生物医药检测有限公司 | A kind of method of metal element A g and Rh residual content in measurement drug |
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| CN103018316A (en) * | 2012-12-04 | 2013-04-03 | 漳州片仔癀药业股份有限公司 | Method for detecting heavy metal elements in anti-inflammatory and analgesic bolus by inductively coupled plasma mass spectrometric method |
| CN109374807A (en) * | 2018-11-07 | 2019-02-22 | 南京明捷生物医药检测有限公司 | A kind of method of metal element A g and Rh residual content in measurement drug |
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