CN117825306A - Quantitative detection method for potassium ions in medicines - Google Patents
Quantitative detection method for potassium ions in medicines Download PDFInfo
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- CN117825306A CN117825306A CN202311835819.5A CN202311835819A CN117825306A CN 117825306 A CN117825306 A CN 117825306A CN 202311835819 A CN202311835819 A CN 202311835819A CN 117825306 A CN117825306 A CN 117825306A
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- 229910001414 potassium ion Inorganic materials 0.000 title claims abstract description 113
- 238000001514 detection method Methods 0.000 title claims abstract description 61
- 239000003814 drug Substances 0.000 title claims abstract description 45
- 229940079593 drug Drugs 0.000 title claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 90
- 238000002347 injection Methods 0.000 claims abstract description 53
- 239000007924 injection Substances 0.000 claims abstract description 53
- 238000002835 absorbance Methods 0.000 claims abstract description 45
- 239000012488 sample solution Substances 0.000 claims abstract description 45
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000012086 standard solution Substances 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000010790 dilution Methods 0.000 claims description 34
- 239000012895 dilution Substances 0.000 claims description 34
- 239000010093 guan-xin-ning Substances 0.000 claims description 9
- 238000012797 qualification Methods 0.000 claims description 3
- 239000000825 pharmaceutical preparation Substances 0.000 claims 8
- 229940127557 pharmaceutical product Drugs 0.000 claims 8
- 238000012360 testing method Methods 0.000 abstract description 19
- 239000000523 sample Substances 0.000 abstract description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 18
- 229910052700 potassium Inorganic materials 0.000 description 14
- 239000013558 reference substance Substances 0.000 description 14
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 13
- 239000011591 potassium Substances 0.000 description 13
- 238000007865 diluting Methods 0.000 description 10
- 230000009286 beneficial effect Effects 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 9
- 238000005507 spraying Methods 0.000 description 9
- 239000012085 test solution Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 8
- 229960000583 acetic acid Drugs 0.000 description 7
- 230000029087 digestion Effects 0.000 description 6
- 239000012088 reference solution Substances 0.000 description 6
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 5
- 239000011550 stock solution Substances 0.000 description 5
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 4
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 4
- 239000008098 formaldehyde solution Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- -1 sodium tetraphenylborate Chemical compound 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000012490 blank solution Substances 0.000 description 3
- 239000012362 glacial acetic acid Substances 0.000 description 3
- 239000003112 inhibitor Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004380 ashing Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000005048 flame photometry Methods 0.000 description 2
- 238000000673 graphite furnace atomic absorption spectrometry Methods 0.000 description 2
- 230000005283 ground state Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 description 2
- 235000011151 potassium sulphates Nutrition 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- FMGBNISRFNDECK-CZSBRECXSA-N Coronatine Chemical compound CC[C@H]1C[C@]1(C(O)=O)NC(=O)C1=C[C@H](CC)C[C@@H]2C(=O)CC[C@H]12 FMGBNISRFNDECK-CZSBRECXSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 244000088401 Pyrus pyrifolia Species 0.000 description 1
- 235000001630 Pyrus pyrifolia var culta Nutrition 0.000 description 1
- 238000000184 acid digestion Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- FMGBNISRFNDECK-UHFFFAOYSA-N coronatine Natural products CCC1CC1(C(O)=O)NC(=O)C1=CC(CC)CC2C(=O)CCC12 FMGBNISRFNDECK-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 239000002158 endotoxin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
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- 239000012467 final product Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000010253 intravenous injection Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000120 microwave digestion Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000003109 potassium Chemical class 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a quantitative detection method of potassium ions in medicines, which relates to the technical field of injection detection and comprises the following steps: mixing a medicine to be tested, water and cesium chloride solution to obtain a sample solution; preparing standard solutions with different potassium ion concentrations; respectively detecting the absorbance of each group of standard solution, and drawing a standard curve by taking the absorbance as an ordinate and the potassium ion concentration as an abscissa; detecting the absorbance of the solution of the test sample, and finding the corresponding potassium ion concentration according to the absorbance and a standard curve; calculating to obtain the concentration of potassium ions in the medicine to be detected; the method mainly solves the technical problem that the detection of potassium ions in the existing medicines cannot be accurately and quantitatively detected.
Description
Technical Field
The invention relates to the technical field of injection detection, in particular to a quantitative detection method of potassium ions in medicines.
Background
In the injection, potassium ions may be carried in or side reaction products of raw materials during the production process, degradation products during storage, and the like. Intravenous injection of potassium ion-containing medicines can cause discomfort to patients and also can cause infusion reaction of patients with low endotoxin threshold and weak and sensitive patients, so that the potassium ion content needs to be controlled.
The existing detection of potassium ions in the Guanxin injection adopts a colorimetric method, the method can only carry out content limit detection on potassium ions, cannot carry out accurate quantitative detection, cannot accurately control the content of potassium ions in the product, and has risks in product stability. Therefore, development of a quantitative detection method for potassium ions in medicines is urgently needed.
Disclosure of Invention
The invention aims to solve the technical problem of providing a quantitative detection method for potassium ions in medicines, which mainly solves the technical problem that the detection of potassium ions in the existing medicines, such as Guanxin injection, cannot be accurately and quantitatively detected.
The technical scheme for solving the technical problems is as follows:
the invention provides a quantitative detection method of potassium ions in a medicine, which comprises the following steps: s1, taking a medicine to be detected, water and cesium chloride solution, and mixing to obtain a sample solution; s2, preparing a series of standard solutions with different potassium ion concentrations; s3, detecting the absorbance of each group of standard solutions, and drawing a standard curve by taking the absorbance of each group of standard solutions as an ordinate and the potassium ion concentration of each group of standard solutions as an abscissa; s4, detecting the absorbance of the sample solution, and finding out the corresponding potassium ion concentration according to the standard curve according to the absorbance of the sample solution to obtain the potassium ion concentration in the sample solution; s5, calculating according to a formula I to obtain the concentration of potassium ions in the medicine to be detected, wherein the formula I is as follows: concentration of potassium ions in the test drug = concentration of potassium ions in the test sample solution/{ (volume of test drug/volume of solution after first dilution) × (volume of solution after first dilution for second dilution/volume of test sample solution) }.
The absorbance detection method can use flame photometry, and can also use other methods such as graphite furnace atomic absorption spectrometry, etc.
The beneficial effects of the invention are as follows: according to the invention, the standard curve is drawn by using the absorbance of the standard solution and the concentration of potassium ions, so that the concentration of potassium ions in a medicine to be detected is detected, and the cesium chloride solution is added as an ionization inhibitor to provide enough electrons to enable ionization balance to move towards the direction of generating potassium atoms so as to reduce ionization of potassium ions, so that the accurate quantitative detection of the concentration of potassium ions in the Guanxin injection can be realized, the method is simple and convenient to operate, and the quantitative detection efficiency of potassium ions in the Guanxin injection is improved.
Further, the mass fraction of cesium chloride in the cesium chloride solution is 2-3%, and the amount of the cesium chloride solution is 1ml.
The invention has the further beneficial effects that: reducing ionization of potassium ions by adding cesium chloride solution in this concentration interval as an ionization inhibitor to provide sufficient electrons to shift the ionization equilibrium in the direction of generating potassium ground state atoms; if the mass fraction is too low, potassium ion ionization cannot be completely eliminated, and if the addition amount is too high, raw material waste is easily caused.
Wherein, the treatment method of the sample solution is direct dilution. The direct dilution treatment method is adopted, the operation is simple and convenient, and the quantitative detection result is stable and accurate. Compared with the digestion dilution treatment method or the carbonization dilution treatment method, the operation steps are complicated, and the final detection result is interfered due to insufficient digestion or carbonization treatment, so that the detection result is inaccurate.
Further, in the test solution, the dilution factor of the drug to be tested is 125-160 times.
The invention has the further beneficial effects that: the potassium ion content in the Guanxin injection can be accurately detected by adopting the sample solution with the dilution factor, if the dilution factor is too low, the absorption value is easily too high, the numerical fluctuation is large, and the detection result is inaccurate; if the dilution factor is too high, the detection result is easily high in a deficiency way. The medicine to be tested can be diluted for multiple times as required before being mixed with cesium chloride solution, so that the situation that the corresponding potassium ion concentration cannot be found on a standard curve according to absorbance due to overhigh potassium ion concentration in an original solution is avoided, the accuracy can be further improved, and after the coronatine solution to be tested is diluted for multiple times, the formula I is changed into: concentration of potassium ions in the test drug = concentration of potassium ions in the test sample solution/{ (volume of test drug/volume of solution after first dilution) × (volume of solution after first dilution for second dilution/volume of solution after second dilution) × (volume of solution after nth dilution for preparation of test sample solution/volume of test sample solution) }.
Further, the concentration of potassium ions in the standard curve solution is in the range of 0-8. Mu.g/ml. Each group of standard curve solutions comprises the cesium chloride solution and a reference solution only containing potassium ions.
Further, the concentration of potassium ions in the control solution used for preparing the series of standard curve solutions is 45-55 mug/mL.
The invention has the further beneficial effects that: the reference substance solution in the potassium ion concentration interval is convenient for preparing subsequent standard solutions, complicated operation caused by the fact that a large amount of reference substance solution is required to be added due to the fact that the concentration is too low is avoided, and operation difficulty is not increased due to the fact that the added reference substance solution is small in volume due to the fact that the concentration is too high.
The invention has the further beneficial effects that: the concentration range can meet the requirement of system applicability, and the accuracy of the detection result is ensured; the control solution containing only potassium ions is used to avoid the influence of other ions, while cesium chloride solution is used to prevent ionization of potassium ions.
Further, in the above S4, the detection wavelength at the time of detecting absorbance was 769.9nm.
The invention has the further beneficial effects that: the detection wavelength can ensure the highest detection sensitivity, thereby improving the accuracy of the result.
Further, the medicine to be detected is a Guanxinning injection.
Further, the step of judging the qualification is further included after the step S5, when the medicine to be detected is a Guanxin injection, the Guanxin injection to be detected is unqualified when the concentration of potassium ions in the Guanxin injection to be detected exceeds 1000 mug/mL, and when the concentration of potassium ions in the Guanxin injection to be detected is not more than 1000 mug/mL, the Guanxin injection to be detected is qualified.
The invention has the further beneficial effects that: when the concentration of potassium ions in the injection to be tested exceeds 1000 mug/mL, the potassium ions contained in the injection are excessive, so that the injection can cause discomfort of a patient, and the injection is failed, and otherwise, the injection is qualified.
Further, the fitting degree of the standard curve is greater than 0.995.
The invention has the further beneficial effects that: the accuracy of the detection result can be ensured only by exceeding the standard curve of the fitting degree, so that the error is reduced.
Further, the above detection limit was 0.055. Mu.g/mL.
The invention has the further beneficial effects that: when the concentration of potassium ions in the Guanxinning injection is lower than the detection limit, accurate quantitative detection cannot be realized.
Drawings
FIG. 1 is a standard chart of example 1 of the present invention.
FIG. 2 is a graph of the standard curve of example 3 of the present invention.
FIG. 3 is a graph of the standard curve of example 4 of the present invention.
FIG. 4 is a graph of the standard curve of example 6 of the present invention.
Detailed Description
The principles and features of the present invention are described below with examples given for the purpose of illustration only and are not intended to limit the scope of the invention. The specific techniques or conditions are not identified in the examples and are described in the literature in this field or are carried out in accordance with the product specifications. The reagents or apparatus used were conventional products commercially available through regular channels, with no manufacturer noted.
The apparatus and tools used in examples 1-5 of the present invention include: pipette, volumetric flask, atomic absorption spectrophotometer.
The embodiment relates to a quantitative detection method of potassium ions in medicines, which comprises the following steps: s1, taking a medicine to be detected, water and cesium chloride solution, and mixing to obtain a sample solution; s2, preparing a series of standard solutions with different potassium ion concentrations; s3, detecting the absorbance of each group of standard solutions, and drawing a standard curve by taking the absorbance of each group of standard solutions as an ordinate and the potassium ion concentration of each group of standard solutions as an abscissa; s4, detecting the absorbance of the sample solution, and finding out the corresponding potassium ion concentration according to the standard curve according to the absorbance of the sample solution to obtain the potassium ion concentration in the sample solution; s5, calculating according to a formula I to obtain the concentration of potassium ions in the medicine to be detected, wherein the formula I is as follows: concentration of potassium ions in the test drug = concentration of potassium ions in the test sample solution/{ (volume of test drug/volume of solution after first dilution) × (volume of solution after first dilution for second dilution/volume of test sample solution) }.
The absorbance detection method can use flame photometry, and can also use other methods such as graphite furnace atomic absorption spectrometry, etc.
The standard curve is drawn by using the absorbance of the standard solution and the concentration of potassium ions, so that the concentration of potassium ions in a medicine to be detected is detected, and the cesium chloride solution is added as an ionization inhibitor to provide enough electrons to enable ionization balance to move towards the direction of generating potassium ground state atoms, so that ionization of potassium ions is reduced, accurate quantitative detection of the concentration of potassium ions in the Guanxin injection can be realized, and the method is simple and convenient to operate, and improves the quantitative detection efficiency of potassium ions in the Guanxin injection. The following is a specific explanation of the medicine to be tested as a Guanxinning injection.
Example 1
The embodiment relates to a quantitative detection method of potassium ions in medicines, which comprises the following steps:
preparation of 2.5% cesium chloride solution: taking 2.5g of cesium chloride, placing into a 100mL measuring flask, adding water to dilute to a scale, and shaking uniformly to obtain the cesium chloride.
Preparing a reference substance solution: precisely measuring 5mL of potassium unitary element standard solution, placing the solution into a 100mL measuring flask, adding water for dilution to a scale, and shaking uniformly to obtain a reference substance solution with the concentration of 50 mug/mL.
Preparing a test solution: precisely measuring 2mL of the Guanxin injection to be measured, placing the injection in a 25mL measuring flask, adding water to dilute the injection to a scale, and shaking the injection uniformly; then 2mL of the sample solution is precisely measured, placed in a 25mL measuring flask, 1mL of 2.5% cesium chloride solution is added, diluted to a scale with water, and shaken well to obtain the sample solution.
Drawing a standard curve: precisely measuring 0,0.5,1,2,3 and 4mL of the reference solution respectively, placing the reference solution into a 25mL measuring flask, adding 1mL of 2.5% cesium chloride solution, and diluting with water to obtain a solution containing 0,1,2,4,6,8 mug of potassium respectively per 1mL. And sequentially spraying flame, measuring absorbance, drawing a standard curve by taking absorbance as an ordinate and concentration as an abscissa, wherein the fitting degree in a standard curve equation is more than 0.995.
Measurement conditions of the sample solution: the detection wavelength was 769.9nm, and flame method (FIG. 1) was used.
And (3) measuring: precisely sucking the sample solution, spraying flame, detecting absorbance, reading the content of potassium ions in the sample solution from a standard curve according to the detected absorbance, and according to the formula I: and (3) calculating the concentration of potassium ions in the to-be-detected Guanxin injection=the concentration of potassium ions in the to-be-detected sample solution (mug/mL)/{ (2/25) × (2/25) }, and detecting 5 batches of samples to obtain the Guanxin injection with potassium ion contents of 525.7 mug/mL, 522.2 mug/mL, 564.7 mug/mL, 795.7 mug/mL and 489.9 mug/mL respectively.
Example 2: acid digestion control
The embodiment relates to a quantitative detection method of potassium ions in medicines, which comprises the following steps:
preparation of 2.5% cesium chloride solution: taking 2.5g of cesium chloride, placing into a 100mL measuring flask, adding water to dilute to a scale, and shaking uniformly to obtain the cesium chloride.
Preparing a reference substance solution: precisely measuring 5mL of potassium unitary element standard solution, placing the solution into a 100mL measuring flask, adding water for dilution to a scale, and shaking uniformly to obtain a reference substance solution with the concentration of 50 mug/mL.
Preparing a test solution: precisely measuring 3ml of Guanxin injection, placing into a tetrafluoroethylene digestion tank, adding 4ml of nitric acid, uniformly mixing, covering an inner cover, screwing an outer cover, placing into a proper microwave digestion furnace, carrying out digestion, taking out the digestion, placing the digestion on an electric plate of the inner tank, slowly heating to be full of reddish brown steam at 120 ℃, continuously slowly concentrating to be 2-3 ml, transferring the concentrated solution into a 25ml measuring flask by using water, adding 1ml of 2.5% cesium chloride solution, diluting to a scale by using water, and shaking uniformly to obtain the injection.
Drawing a standard curve: precisely measuring 0,0.5,1,2,3 and 4mL of the reference solution respectively, placing the reference solution into a 25mL measuring flask, adding 1mL of 2.5% cesium chloride solution, and diluting with water to obtain a solution containing 0,1,2,4,6,8 mug of potassium respectively per 1mL. And sequentially spraying flame, measuring absorbance, drawing a standard curve by taking absorbance as an ordinate and concentration as an abscissa, wherein the fitting degree in a standard curve equation is more than 0.995.
Measurement conditions of the sample solution: the detection wavelength is 769.9nm, and a flame method is adopted.
And (3) measuring: precisely sucking the sample solution, spraying flame, detecting absorbance, reading the content of potassium ions in the sample solution from a standard curve according to the detected absorbance, and according to the formula I: and calculating the concentration of potassium ions in the to-be-detected Guanxin injection=the concentration of potassium ions in the to-be-detected sample solution (mug/mL)/(3/25), and obtaining the medicine.
The results show that: the absorbance of the test solution is larger than 1.3, the numerical fluctuation is large, and the normal detection cannot be carried out.
Example 3: charring control
The embodiment relates to a quantitative detection method of potassium ions in medicines, which comprises the following steps:
preparation of 2.5% cesium chloride solution: taking 2.5g of cesium chloride, placing into a 100mL measuring flask, adding water to dilute to a scale, and shaking uniformly to obtain the cesium chloride.
Preparing a reference substance solution: precisely measuring 5mL of potassium unitary element standard solution, placing the solution into a 100mL measuring flask, adding water for dilution to a scale, and shaking uniformly to obtain a reference substance solution with the concentration of 50 mug/mL.
Preparing a test solution (1): taking 2ml of Guanxinning injection, evaporating to dryness, burning with small fire until charring, burning at 550 ℃ until completely ashing, adding 2ml of dilute acetic acid to dissolve, placing into a 25ml measuring flask, adding water to dilute to scale, and mixing uniformly; filtering, precisely weighing 1ml, placing in a 10ml measuring flask, adding 1ml of 2.5% cesium chloride solution, diluting to scale with water, and shaking.
Preparing a test solution (2): precisely measuring 2ml of GUANXINNING injection, placing in a 25ml measuring flask, diluting with water to scale, and shaking; then 1ml of the solution is precisely measured, placed in a 10ml measuring flask, 1ml of 2.5% cesium chloride solution is added, diluted to the scale with water and shaken well.
Preparation of a standard curve: precisely measuring 0,0.5,1,2,3 and 4ml of the reference substance solution respectively, placing in a 25ml measuring flask, adding 1ml of 2.5% cesium chloride solution, diluting with water to obtain a solution containing 0,1,2,4,6,8 mug of potassium per 1ml, sequentially spraying flame, measuring absorbance, carrying out quadratic least square fitting regression by taking absorbance Y as an ordinate and concentration X (mug/ml) as an abscissa, and drawing a standard curve. The fitness in the standard curve equation is greater than 0.995 (fig. 2).
Measurement conditions of the sample solution: the detection wavelength is 769.9nm, and a flame method is adopted.
And (3) measuring: precisely sucking the sample solution, spraying flame, detecting absorbance, reading the content of potassium ions in the sample solution from a standard curve according to the detected absorbance, and according to the formula I: the concentration of potassium ions in the Guanxin injection to be detected=the concentration of potassium ions in the test solution (mug/mL)/{ (2/25) × (1/10) }, and the potassium ion content of the test solution (1) of the Guanxin injection is 408.3 mug/mL, 300.4 mug/mL, 253.7 mug/mL, 451.6 mug/mL and 348.6 mug/mL respectively; the potassium ion content of the sample solution (2) was 534.2. Mu.g/mL, 516.2. Mu.g/mL, 547.8. Mu.g/mL, 762.2. Mu.g/mL, 488.1. Mu.g/mL, respectively. It can be seen that the potassium ion content of the carbonized diluted Guanxin injection is generally lower than that of the directly diluted Guanxin injection.
The test result of the comparative accuracy experiment shows that the recovery rate of the solution of the standard-added test sample subjected to carbonization dilution treatment is lower than 80 percent and exceeds the qualified range, and the recovery rate of the solution of the standard-added test sample subjected to direct dilution treatment is within the qualified range. The sample subjected to carbonization and dilution treatment cannot be completely carbonized and dissolved, so that the detection result is low.
Example 4: dilution fold control
The embodiment relates to a quantitative detection method of potassium ions in medicines, which comprises the following steps:
preparation of 2.5% cesium chloride solution: taking 2.5g of cesium chloride, placing into a 100mL measuring flask, adding water to dilute to a scale, and shaking uniformly to obtain the cesium chloride.
Preparing a reference substance solution: precisely measuring 5mL of potassium unitary element standard solution, placing the solution into a 100mL measuring flask, adding water for dilution to a scale, and shaking uniformly to obtain a reference substance solution with the concentration of 50 mug/mL.
Preparing a test solution: precisely measuring 2ml of GUANXINNING injection, placing in a 50ml measuring flask, diluting with water to scale, and shaking; then 2ml of the solution is precisely measured, placed in a 50ml measuring flask, 1ml of 2.5% cesium chloride solution is added, diluted to the scale with water and shaken well.
Preparing a labeled test sample solution: precisely measuring 2ml of GUANXINNING injection, placing in a 50ml measuring flask, diluting with water to scale, and shaking; then 2ml of the sample is precisely measured, placed in a 50ml measuring flask, 2ml of the reference stock solution is added, 1ml of 2.5% cesium chloride solution is added, diluted to scale with water, and shaken well.
Preparation of a standard curve: 1.0ml, 2.0ml, 3.0ml, 4.0ml and 5.0ml of potassium reference solution are precisely measured, respectively placed in 50ml measuring bottles, 1ml of 2.5% cesium chloride solution is added, and water is used for dilution to scale, so as to prepare a series of potassium standard solutions. And (3) sequentially spraying flame, measuring absorbance, taking absorbance Y as an ordinate and concentration X (mug/ml) as an abscissa, carrying out quadratic equation least square fitting regression, and drawing a standard curve. The fitness in the standard curve equation is greater than 0.995 (fig. 3).
Measurement conditions of the sample solution: the detection wavelength is 769.9nm, and a flame method is adopted.
And (3) measuring: precisely sucking the sample solution, spraying flame, detecting absorbance, reading the content of potassium ions in the sample solution from a standard curve according to the detected absorbance, and according to the formula I: the concentration of potassium ions in the Guanxin injection to be detected=the concentration of potassium ions in the solution of the test sample (mug/mL)/{ (2/50) × (1/50) } is calculated, and the potassium ion content of the Guanxin injection is 1192.8 mug/mL and 786.1 mug/mL respectively; the recovery rates were 125.7% and 128.7%, respectively. Too large dilution results in higher detection results and recovery rates of greater than 120%.
Example 5: other methods control
Instrument and appliance: electronic balance, acidometer, electric stove, high temperature box resistance furnace, electric heating thermostated drying oven, crucible tongs, scale tube (1 mL, 2mL, 10 mL), pipette (1 mL, 2mL, 10 mL), volumetric flask (25 mL, 100mL, 1000 mL), 10mL Navigator.
Reagent and solution: disodium ethylenediamine tetraacetate, sodium tetraphenylborate, formaldehyde solution, potassium sulfate and dilute acetic acid.
Preparing dilute acetic acid: and (3) taking 6mL of glacial acetic acid, adding water to dilute the glacial acetic acid to 100mL, and shaking the glacial acetic acid evenly to obtain the product.
Preparing alkaline formaldehyde solution: and (3) taking a proper amount of formaldehyde solution, and adjusting the pH to 8.0-9.0 by using 0.1mol/L sodium hydroxide solution.
Standard potassium ion solution was prepared: taking a proper amount of potassium sulfate, grinding, drying to constant weight at 110 ℃, precisely weighing 2.23g, placing into a 1000mL measuring flask, adding a proper amount of water to dissolve and dilute to scale, and shaking uniformly to obtain a stock solution. Before use, the stock solution is precisely measured for 10mL, put into a 100mL measuring flask, diluted to a scale by adding water, and shaken uniformly to obtain the product (each 1mL corresponds to 100 mug of K). And (3) injection: the standard potassium ion stock solution is stored in a refrigerator in a refrigerating way.
Preparation of 3% sodium tetraphenylborate solution: taking 3g of sodium tetraphenylborate, and adding water to dissolve the sodium tetraphenylborate into 100mL to obtain the product.
Preparing a 3% disodium ethylenediamine tetraacetate solution: taking 3g of disodium ethylenediamine tetraacetate, and adding water to dissolve the disodium ethylenediamine tetraacetate into 100mL to obtain the product.
And (3) measuring: taking 2mL of the Guanxinning injection to be detected, evaporating to dryness, burning with small fire until charring, burning at 500-600 ℃ until completely ashing, adding 2mL of dilute acetic acid to dissolve, placing into a 25mL measuring flask, adding water to dilute to scale, and uniformly mixing to obtain the sample solution. 2 tubes of a 10mL Nashi colorimetric tube are taken, 0.8mL of standard potassium ion solution, 0.6mL of alkaline formaldehyde solution, 2 drops of 3% ethylenediamine tetraacetic acid disodium salt solution and 0.5mL of 3% tetraphenylboron sodium solution are precisely added into the tube A, water is added for dilution into 10mL, 1mL of sample solution is precisely added into the tube B, the tube A and the tube B are simultaneously operated according to a law, shaking is carried out, the tube A and the tube B are simultaneously placed on black paper, and perspective is carried out from top to bottom.
Results: the turbidity developed in the b tube was not much stronger than in the a tube.
The concentration of potassium ions cannot be accurately and quantitatively detected in the comparative example, and only whether the comparison is qualified or not can be performed.
Example 6: detection limit
Preparation of 2.5% cesium chloride solution: weighing cesium chloride 2.5g, placing into a 100ml measuring flask, dissolving with water, diluting to scale, and shaking to obtain the final product.
Preparing a blank solution: precisely weighing 2ml of 2.5% cesium chloride solution, placing in a 50ml measuring flask, diluting with water to scale, and shaking.
Preparing a reference substance solution: precisely measuring 5ml of potassium unitary element standard solution, placing into a 100ml measuring flask, adding water to dilute to scale, and shaking to obtain reference substance solution with concentration of 50 mug/ml.
Standard curve solutions were prepared: each of 0,0.5,1,2,3 and 4ml of the control stock solution was precisely measured and placed in a 25ml measuring flask, 1ml of a 2.5% cesium chloride solution was added, and the mixture was diluted with water to prepare a solution containing 0,1,2,4,6,8. Mu.g of potassium per 1ml (FIG. 4).
System applicability requirements:
and (3) taking a standard curve solution, sequentially spraying flame, measuring absorbance at the wavelength of 769.9nm, carrying out linear least square fitting regression by taking absorbance Y as an ordinate and concentration X (mug/ml) as an abscissa, and drawing a standard curve, wherein the fitting degree in a standard curve equation is larger than 0.995.
And (3) measuring: measuring a proper amount of blank solution, measuring absorbance, and measuring for 10 times in parallel, and obtaining the result according to C 1 Minimum detection limit of element calculated by=3×sd/K, C 2 Calculated quantitative limit of detection =10×sd/K (where SD is the standard deviation of absorbance of the blank solution 10 times; K is the slope of the standard curve; C) 1 Is the detection limit; c (C) 2 To be quantitativeLimit).
Results: the detection limit is 0.055 mug/ml, the quantitative limit is 0.18 mug/ml, and the detection limit is smaller than the limit, thereby meeting the regulations.
In summary, the invention provides a quantitative detection method for potassium ions in medicines, which is characterized in that the concentration of potassium ions in a Guanxin injection to be detected is detected by drawing a standard curve by using the absorbance of a standard solution and the concentration of potassium ions, so that the quantitative detection for the concentration of potassium ions in the Guanxin injection can be realized, the method is simple and convenient to operate, and the quantitative detection efficiency of potassium ions in the Guanxin injection is improved.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (10)
1. The quantitative detection method of potassium ions in the medicine is characterized by comprising the following steps:
s1, taking a medicine to be detected, water and cesium chloride solution, and mixing to obtain a sample solution;
s2, preparing a series of standard solutions with different potassium ion concentrations;
s3, detecting the absorbance of each group of standard solutions respectively, and drawing a standard curve by taking the absorbance of each group of standard solutions as an ordinate and the potassium ion concentration of each group of standard solutions as an abscissa;
s4, detecting the absorbance of the sample solution, and finding out the corresponding potassium ion concentration according to the standard curve according to the absorbance of the sample solution to obtain the potassium ion concentration in the sample solution;
s5, calculating according to a formula I to obtain the concentration of potassium ions in the medicine to be detected, wherein the formula I is as follows: concentration of potassium ions in the drug solution to be tested = concentration of potassium ions in the sample solution/{ (volume of drug to be tested/volume of solution after first dilution) × (volume of solution after first dilution for second dilution/volume of sample solution) }.
2. The quantitative detection method of potassium ions in a medicine according to claim 1, wherein the mass fraction of cesium chloride in the cesium chloride solution is 2-3%, and the dosage of the cesium chloride solution is 1ml.
3. The method for quantitative detection of potassium ions in a pharmaceutical product according to claim 1, wherein the dilution factor of the pharmaceutical product to be tested in the sample solution is 120-160 times.
4. The method for quantitatively detecting potassium ions in a pharmaceutical product according to claim 2, wherein the concentration of potassium ions in the standard curve solution is in the range of 0-8 μg/ml.
5. The method for quantitatively detecting potassium ions in a pharmaceutical product according to claim 4, wherein the concentration of potassium ions in a control solution used for preparing a series of the standard curve solutions is 45-55 μg/mL.
6. The method for quantitative detection of potassium ions in a pharmaceutical product according to claim 1, wherein in S4, the detection wavelength at the time of detecting absorbance is 769.9nm.
7. The method for quantitatively detecting potassium ions in a medicine according to claim 1, wherein the medicine to be detected is a guanxinning injection.
8. The method for quantitative determination of potassium ions in a pharmaceutical product according to claim 7, further comprising a qualification step after S5, wherein the qualification step comprises the steps of: when the medicine to be detected is a Guanxin injection, the Guanxin injection to be detected is unqualified when the concentration of potassium ions in the Guanxin injection to be detected exceeds 1000 mug/mL, and when the concentration of potassium ions in the Guanxin injection to be detected is not more than 1000 mug/mL, the Guanxin injection to be detected is qualified.
9. The method for quantitatively detecting potassium ions in a pharmaceutical product according to claim 1, wherein the fitting degree of the standard curve is greater than 0.995.
10. The method for quantitative detection of potassium ions in a pharmaceutical product according to any one of claims 1 to 9, wherein the limit of detection is 0.055 μg/mL.
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