CN113029987A - Method for measuring total sodium content in compound polyethylene glycol electrolyte powder - Google Patents
Method for measuring total sodium content in compound polyethylene glycol electrolyte powder Download PDFInfo
- Publication number
- CN113029987A CN113029987A CN202110342816.2A CN202110342816A CN113029987A CN 113029987 A CN113029987 A CN 113029987A CN 202110342816 A CN202110342816 A CN 202110342816A CN 113029987 A CN113029987 A CN 113029987A
- Authority
- CN
- China
- Prior art keywords
- solution
- polyethylene glycol
- placing
- shaking
- scale
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 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 title claims abstract description 56
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 56
- 239000011734 sodium Substances 0.000 title claims abstract description 56
- 239000002202 Polyethylene glycol Substances 0.000 title claims abstract description 51
- 229920001223 polyethylene glycol Polymers 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 46
- 150000001875 compounds Chemical class 0.000 title claims abstract description 38
- 239000003792 electrolyte Substances 0.000 title claims abstract description 37
- 239000000843 powder Substances 0.000 title claims abstract description 37
- 239000000243 solution Substances 0.000 claims abstract description 83
- 239000012086 standard solution Substances 0.000 claims abstract description 44
- 239000013558 reference substance Substances 0.000 claims abstract description 42
- 238000005303 weighing Methods 0.000 claims abstract description 32
- 238000002835 absorbance Methods 0.000 claims abstract description 26
- 239000012085 test solution Substances 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 22
- 239000012490 blank solution Substances 0.000 claims abstract description 20
- 239000012088 reference solution Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 65
- 239000004743 Polypropylene Substances 0.000 claims description 52
- -1 polypropylene Polymers 0.000 claims description 52
- 229920001155 polypropylene Polymers 0.000 claims description 52
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims description 43
- 229920003023 plastic Polymers 0.000 claims description 42
- 239000004033 plastic Substances 0.000 claims description 42
- 239000011550 stock solution Substances 0.000 claims description 35
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 34
- 239000000463 material Substances 0.000 claims description 26
- 239000000523 sample Substances 0.000 claims description 26
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 238000001514 detection method Methods 0.000 claims description 19
- 238000007865 diluting Methods 0.000 claims description 17
- 239000011780 sodium chloride Substances 0.000 claims description 17
- 239000012488 sample solution Substances 0.000 claims description 16
- 238000003321 atomic absorption spectrophotometry Methods 0.000 claims description 12
- 238000012360 testing method Methods 0.000 claims description 11
- 239000001103 potassium chloride Substances 0.000 claims description 10
- 235000011164 potassium chloride Nutrition 0.000 claims description 10
- 229940057838 polyethylene glycol 4000 Drugs 0.000 claims description 7
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 6
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 6
- 230000003595 spectral effect Effects 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 150000003385 sodium Chemical class 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 6
- 239000003814 drug Substances 0.000 description 9
- 229940079593 drug Drugs 0.000 description 9
- 238000011084 recovery Methods 0.000 description 6
- 238000010561 standard procedure Methods 0.000 description 6
- 229910001415 sodium ion Inorganic materials 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000003574 free electron Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 210000002429 large intestine Anatomy 0.000 description 2
- 206010010774 Constipation Diseases 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001839 endoscopy Methods 0.000 description 1
- 210000003736 gastrointestinal content Anatomy 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for measuring the total sodium content in compound polyethylene glycol electrolyte powder, which comprises the following steps: (1) preparing a reference substance solution: preparing a reference solution with the sodium concentration of 14.33494 mg/L; (2) preparation of a standard solution: precisely measuring a reference substance solution to prepare a sodium element series standard solution; (3) preparing a test solution: taking the content of the compound polyethylene glycol electrolyte powder, and preparing the concentration matched with the sodium element series standard solution; (4) preparing a blank solution: accurately weighing proper amount of polyethylene glycol, and preparing the concentration matched with the test solution; (5) and (3) respectively taking the blank solution, the standard solution and the test solution, measuring the absorbance at the wavelength of 589.0nm, describing a regression equation according to the concentration and the absorbance of the standard solution, and calculating the concentration of sodium in the test solution. The method has the advantages of simple and quick operation, high sensitivity, good repeatability, good solution stability and more accurate measured data.
Description
Technical Field
The invention relates to the technical field of chemical analysis, in particular to a method for measuring the content of total sodium in compound polyethylene glycol electrolyte powder.
Background
The compound polyethylene glycol electrolyte powder is mainly used for clearing intestinal contents and treating constipation during large intestine endoscopy and large intestine preoperative treatment, and has high market value. The product is a compound preparation, and comprises polyethylene glycol 4000, anhydrous sodium sulfate, sodium chloride, potassium chloride, and sodium bicarbonate. The total sodium content in the imported drug registration standard JX20170220 is measured by measuring the absorbance at 819.5nm by using an atomic absorption spectrophotometry (standard curve method). At least 5 parts of sodium chloride reference substance solutions with different concentrations are prepared, the concentrations are sequentially increased, and meanwhile, a blank solution is prepared. Detecting by a flame atomic absorption spectrometer, sequentially measuring the absorbance of the blank solution and the sodium chloride reference solution with each concentration, and recording the reading. The average of the 3 absorbance readings for each concentration was plotted on the ordinate versus the corresponding concentration on the abscissa, and a standard curve was plotted. And preparing a test solution, wherein the sodium concentration in the test solution is in the concentration range of a standard curve, measuring the absorbance, taking the average value of the readings for 3 times, and obtaining the corresponding concentration from the standard curve, thereby calculating the total sodium content. The flame atomic absorption spectrometer has the advantages of simple instrument, convenient operation, high sensitivity and high precision.
However, when the atomic absorption spectrophotometry is used for detection, sodium ions are very easy to ionize, sodium silicate is contained in a common glass measuring flask, and the wall of the glass vessel is easy to dissolve out the sodium ions, so that the absorbance of the solution is changed, the detection result is inaccurate, and the repeatability is poor.
Disclosure of Invention
The invention aims to provide a method for measuring the total sodium content in the compound polyethylene glycol electrolyte powder, which can effectively inhibit the ionization of sodium ions, has good linearity and repeatability and can accurately detect the total sodium content, aiming at the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for measuring the total sodium content in compound polyethylene glycol electrolyte powder, which comprises the following steps:
(1) preparing a reference substance solution: accurately weighing a sodium chloride reference substance, placing the sodium chloride reference substance in a polypropylene plastic volumetric flask, adding potassium chloride and polyethylene glycol 4000, diluting to a scale by using deionized water, preparing a reference substance solution with the sodium element concentration of 14.33494mg/L, and shaking up to obtain the sodium chloride reference substance;
(2) preparation of a standard solution: precisely measuring a plurality of reference substance solutions, respectively placing the reference substance solutions into polypropylene plastic volumetric flasks, respectively adding 3-8ml of 2% cesium chloride solution, diluting with deionized water to obtain sodium element series standard solution with concentration matched with that of the test solution, and shaking up to obtain the test solution;
(3) preparing a test solution: taking 4 bags of the contents of the compound polyethylene glycol electrolyte powder, placing the bags in a polypropylene plastic volumetric flask, adding deionized water for dilution, adding 3-8ml of 2% cesium chloride solution, then diluting the solution by using deionized water to reach the concentration matched with the sodium element series standard solution, and shaking up to obtain the compound polyethylene glycol electrolyte powder;
(4) preparing a blank solution: accurately weighing a proper amount of polyethylene glycol 4000, placing the polyethylene glycol 4000 in a polypropylene plastic volumetric flask, adding deionized water for dilution, adding 3-8ml of 2% cesium chloride solution, then diluting the solution by using the deionized water to reach a concentration matched with the solution of a test sample, and shaking up the solution to obtain the test sample;
(5) and (3) respectively taking the blank solution, the standard solution and the sample solution, measuring absorbance at a wavelength of 589.0nm according to an atomic absorption spectrophotometry, describing a regression equation according to the concentration and the absorbance of the standard solution, and calculating the concentration of sodium in the sample solution according to the regression equation.
Further, in the method for determining the total sodium content in the compound polyethylene glycol electrolyte powder, in the step (1), the preparation method of the reference solution is as follows:
weighing 0.1823g of sodium chloride reference substance precisely, placing in a 50ml polypropylene plastic volumetric flask, adding 0.0185g of potassium chloride and 40001.60g of polyethylene glycol, adding water for dissolving and diluting to scale, and shaking up; precisely measuring 1ml, placing in a 100ml polypropylene plastic volumetric flask, adding water to dilute to scale, and shaking up to obtain the product.
Further, in the method for determining the total sodium content in the compound polyethylene glycol electrolyte powder, the preparation method of the standard solution in the step (2) is as follows:
precisely measuring reference substance solutions 2ml, 3ml, 4ml, 5ml and 6ml, respectively placing into 100ml polypropylene plastic volumetric flasks, respectively adding 2% cesium chloride solution 5.0ml, adding water to dilute to scale, and shaking to obtain sodium series standard solutions 0.2867mg/L, 0.4303mg/L, 0.5737mg/L, 0.7172mg/L and 0.8606 mg/L.
Further, in the method for determining the total sodium content in the compound polyethylene glycol electrolyte powder, the preparation method of the test solution in the step (3) comprises the following steps:
taking 4 bags of the contents of the compound polyethylene glycol electrolyte powder, placing the bags in a polypropylene plastic volumetric flask, adding a proper amount of deionized water to dissolve and dilute the solution to a scale, and taking the solution as a stock solution of a test sample;
precisely measuring 1ml of the stock solution of the sample, placing the stock solution in a 20ml polypropylene plastic volumetric flask, adding deionized water to dilute the stock solution to a scale, shaking the stock solution uniformly, precisely measuring 1ml of the stock solution, placing the stock solution in a 100ml polypropylene plastic volumetric flask, adding 5ml of 2% cesium chloride solution, adding water to dilute the stock solution to a scale, and shaking the mixture uniformly to obtain the test solution.
Further, in the method for determining the total sodium content in the compound polyethylene glycol electrolyte powder, in the step (4), the preparation method of the blank solution is as follows:
precisely weighing 40000.32g of polyethylene glycol, placing the weighed materials into a 250ml polypropylene plastic volumetric flask, adding a proper amount of deionized water to dissolve the materials to a scale, shaking up, precisely weighing 1ml of the materials, placing the materials into a 100ml polypropylene plastic volumetric flask, adding 5ml of 2% cesium chloride solution, adding a proper amount of deionized water to dissolve the materials to a scale, and shaking up to obtain the product.
Further, in the method for determining the total sodium content in the compound polyethylene glycol electrolyte powder, in the steps (2), (3) and (4), the preparation method of the 2% cesium chloride solution is as follows:
precisely weighing 5.00060g of cesium chloride, placing the cesium chloride in a 250ml polypropylene volumetric flask, adding a proper amount of water to dissolve the cesium chloride, diluting the cesium chloride to a scale mark, and shaking up the cesium chloride to obtain the cesium chloride.
Further, in the method for determining the total sodium content in the compound polyethylene glycol electrolyte powder, 2-5ml of nitric acid solution with the concentration of 1% is respectively added when preparing 2% cesium chloride solution in the steps (2) and (3).
Further, in the method for determining the total sodium content in the compound polyethylene glycol electrolyte powder, in the step (5), the spectral conditions of the atomic absorption spectrophotometry are as follows:
the detection mode is as follows: flame is continuous; flame type: air-acetylene gas; detection wavelength: 589.0 nm; the width of the slit is as follows: 0.5 nm; lamp current: 5.0 mA; air flow rate: 13.50L/min; acetylene gas flow: 2.00L/min; height of the burner: 13.5 mm; lamp preheating time: and 15 min.
Further, in the method for determining the total sodium content in the compound polyethylene glycol electrolyte powder, an Agilent 240FS atomic absorption spectrophotometer is adopted in the atomic absorption spectrophotometry, and the detection wavelength is 589.0 nm.
By adopting the technical scheme, compared with the existing method for measuring the total sodium content of the JX20170220 which is the registration standard of the imported drugs, the method has the following technical effects:
(1) polypropylene measuring flasks are adopted in the preparation process of the reference solution, the standard solution, the test solution and the blank solution, so that interference caused by dissolution of sodium ions can be eliminated;
(2) adding a 2% cesium chloride solution in the preparation process of the standard solution, the test solution and the blank solution, wherein the cesium chloride ionizes to generate free electrons by itself so as to inhibit sodium ionization, so that the solution is more stable;
(3) through detection of samples in the same batch, the absorbance of the standard solution and the sample solution in the method is within the range of 0.1-0.5, the linear correlation coefficient of a standard curve can reach more than 0.999, and the absorbance of the standard solution and the sample solution in the standard method for registering the imported drugs is below 0.1, which shows that the sensitivity is low at the wavelength, so that the absorbance value is small, and the linear correlation coefficient of the standard curve can only reach more than 0.99;
(4) when the standard solution is returned, the recovery rate of the method is between 98 and 102 percent, and the recovery rate of the standard method for registering the imported drugs is rarely in the range of 98 to 102 percent;
(5) the method has the advantages of simple and quick operation, high sensitivity, good repeatability, good solution stability and more accurate measured data.
Drawings
FIG. 1 is a standard linear curve for determining the total sodium content in a compound polyethylene glycol electrolyte powder by using the method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The invention is further described with reference to the following drawings and specific examples, which are not intended to be limiting.
The present invention will be described in detail and specifically with reference to the following examples to facilitate better understanding of the present invention, but the following examples do not limit the scope of the present invention.
Example one
Provides a method for measuring the total sodium content in the compound polyethylene glycol electrolyte powder, which comprises the following steps:
(1) preparing a reference substance solution: precisely weighing 0.1823g of sodium chloride reference substance, placing in a 50ml polypropylene plastic volumetric flask, adding 0.0185g of potassium chloride and 40001.60g of polyethylene glycol, adding water to dissolve and dilute to scale, shaking up, precisely weighing 1ml, placing in a 100ml polypropylene plastic volumetric flask, adding water to dilute to scale, and shaking up to obtain the product;
(2) preparation of a standard solution: precisely measuring reference substance solutions 2ml, 3ml, 4ml, 5ml and 6ml, respectively placing into 100ml polypropylene plastic volumetric flasks, respectively adding 2% cesium chloride solution 5.0ml, adding water to dilute to scale, and shaking up to obtain sodium series standard solutions 0.2867mg/L, 0.4303mg/L, 0.5737mg/L, 0.7172mg/L and 0.8606 mg/L;
(3) preparing a test solution: taking 4 bags of the content of the sample, placing the 4 bags in a 2000ml polypropylene plastic volumetric flask, dissolving the 4 bags with a proper amount of water and diluting the solution to a scale to obtain a sample stock solution; precisely measuring 1ml of a sample stock solution, placing the sample stock solution into a 20ml polypropylene plastic volumetric flask, adding water to dilute the sample stock solution to a scale, shaking the sample stock solution uniformly, precisely measuring 1ml of the sample stock solution, placing the sample stock solution into a 100ml polypropylene plastic volumetric flask, adding 5ml of a 2% cesium chloride solution, adding water to dilute the sample stock solution to a scale, and shaking the sample stock solution uniformly to obtain the sample stock solution;
(4) preparing a blank solution: precisely weighing 40000.32g of polyethylene glycol, placing the weighed materials into a 250ml polypropylene plastic volumetric flask, adding a proper amount of water to dissolve the materials to a scale, shaking up, precisely weighing 1ml of the materials, placing the materials into a 100ml polypropylene plastic volumetric flask, adding 5ml of 2% cesium chloride solution, adding a proper amount of water to dissolve the materials to a scale, and shaking up to obtain the cesium chloride measuring instrument;
(5) setting the spectral conditions: the detection mode is as follows: flame is continuous; flame type: air-acetylene gas; detection wavelength: 589.0 nm; the width of the slit is as follows: 0.5 nm; lamp current: 5.0 mA; air flow rate: 13.50L/min; acetylene gas flow: 2.00L/min; height of the burner: 13.5 mm; lamp preheating time: 15 min;
(6) the operation method comprises the following steps: and (3) taking the blank solution, the standard solution and the sample solution, measuring the absorbance at a wavelength of 589.0nm according to an atomic absorption spectrophotometry, describing a regression equation according to the concentration and the absorbance of the standard solution, and calculating the concentration (Ck) (mg/L) of sodium in the sample solution according to the regression equation.
Example two
Provides a method for measuring the total sodium content in the compound polyethylene glycol electrolyte powder, which comprises the following steps:
(1) preparing a reference substance solution: precisely weighing 0.1823g of sodium chloride reference substance, placing in a 50ml polypropylene plastic volumetric flask, adding 0.0185g of potassium chloride and 40001.60g of polyethylene glycol, adding water to dissolve and dilute to scale, shaking up, precisely weighing 1ml, placing in a 100ml polypropylene plastic volumetric flask, adding water to dilute to scale, and shaking up to obtain the product;
(2) preparation of a standard solution: precisely measuring reference substance solutions 2ml, 3ml, 4ml, 5ml and 6ml, respectively placing into 100ml polypropylene plastic volumetric flasks, respectively adding 2% cesium chloride solution 5.0ml, adding water to dilute to scale, and shaking up to obtain sodium series standard solutions 0.2867mg/L, 0.4303mg/L, 0.5737mg/L, 0.7172mg/L and 0.8606 mg/L;
(3) preparing a test solution: taking 4 bags of the content of the sample, placing the 4 bags in a 2000ml polypropylene plastic volumetric flask, dissolving the 4 bags with a proper amount of water and diluting the solution to a scale to obtain a sample stock solution; precisely measuring 1ml of a stock solution of a sample, placing the stock solution in a 20ml polypropylene plastic volumetric flask, adding water to dilute the stock solution to a scale, shaking up, precisely measuring 1ml, placing the stock solution in a 100ml polypropylene plastic volumetric flask, respectively adding 5ml of a 2% cesium chloride solution and 4ml of a 1% nitric acid solution, adding water to dilute the stock solution to a scale, and shaking up to obtain the test solution;
(4) preparing a blank solution: precisely weighing 40000.32g of polyethylene glycol, placing the weighed materials into a 250ml polypropylene plastic volumetric flask, adding a proper amount of water to dissolve the materials to a scale, shaking up, precisely weighing 1ml of the materials, placing the materials into a 100ml polypropylene plastic volumetric flask, respectively adding 5ml of 2% cesium chloride solution and 3ml of 1% nitric acid solution, adding a proper amount of water to dissolve the materials to a scale, and shaking up to obtain the product;
(5) spectral conditions: the detection mode is as follows: flame is continuous; flame type: air-acetylene gas; detection wavelength: 589.0 nm; the width of the slit is as follows: 0.5 nm; lamp current: 5.0 mA; air flow rate: 13.50L/min; acetylene gas flow: 2.00L/min; height of the burner: 13.5 mm; lamp preheating time: 15 min;
(6) the operation method comprises the following steps: and (3) taking the blank solution, the standard solution and the sample solution, measuring the absorbance at a wavelength of 589.0nm according to an atomic absorption spectrophotometry, describing a regression equation according to the concentration and the absorbance of the standard solution, and calculating the concentration (Ck) (mg/L) of sodium in the sample solution according to the regression equation.
Verification test
In order to prove the stability, accuracy and feasibility of the method, the following comparative experimental research is carried out:
firstly, an imported drug registration standard method comprises the following steps:
(1) stock solution of test sample: precisely weighing the contents of the 4 bags of the compound polyethylene glycol electrolyte powder to be tested, placing the contents in a 2000ml measuring flask, adding a proper amount of water, ultrasonically dissolving, adding water to dilute to a scale, and shaking up to obtain a solution A; precisely measuring 250ml of the solution A, putting the solution A into a 500ml measuring flask, diluting the solution A to a scale with water, and shaking up to obtain a solution B;
(2) preparing a reference substance solution: 1.82362g of sodium chloride reference substance dried for 2 hours at 130 ℃ is precisely weighed, placed in a 100ml measuring flask, added with 0.18480g of potassium chloride and 400016.00177g of polyethylene glycol, dissolved and diluted to scale by adding water, and shaken up;
(3) preparation of a standard solution: precisely measuring reference substance solutions of 5ml, 8ml, 10ml, 12ml and 15ml, respectively placing in 50ml volumetric flasks, adding water to dilute to scale, and shaking to obtain series of standard solutions with sodium concentration of 715.2507mg/L, 1144.4011mg/L, 1430.5013mg/L, 1716.6016mg/L and 2145.7520 mg/L;
(4) preparing a test solution: precisely measuring 50ml of the solution B, placing the solution B in a 100ml measuring flask, and adding water to dilute the solution B to a scale;
(5) preparing a blank solution: precisely weighing 40003.20088g of polyethylene glycol, placing in a 100ml measuring flask, adding water to dilute to a scale, and shaking up;
(6) spectral conditions: the detection mode is as follows: flame is continuous; flame type: air-acetylene gas detection wavelength: 819.5 n; the width of the slit is as follows: 0.5 nm; lamp current: 5.0 mA; air flow rate: 13.50L/min; acetylene gas flow: 2.00L/min; height of the burner: 13.5 mm; lamp preheating time: 15 min;
(7) and (3) taking the blank solution, the standard solution and the sample solution, measuring the absorbance at a wavelength of 589.0nm according to an atomic absorption spectrophotometry, describing a regression equation according to the concentration and the absorbance of the standard solution, and calculating the concentration (Ck) (mg/L) of sodium in the sample solution according to the regression equation.
(II) the method for measuring the total sodium content in the compound polyethylene glycol electrolyte powder
(1) Stock solution of test sample: precisely weighing the contents of the 4 bags of the compound polyethylene glycol electrolyte powder to be tested, placing the contents in a 2000ml measuring flask, adding a proper amount of water, ultrasonically dissolving, adding water to dilute to a scale, and shaking up to be used as a stock solution of the to-be-tested sample;
(2) preparing a reference substance solution: taking 0.18g of sodium chloride reference substance dried for 2 hours at 130 ℃, precisely weighing, placing in a 50ml polypropylene volumetric flask, adding 0.01854g of potassium chloride and 40001.59973g of polyethylene glycol, adding water to dissolve and dilute to a scale, shaking up, precisely weighing 1ml, placing in a 100ml polypropylene volumetric flask, adding water to dilute to the scale, and shaking up to obtain the sodium chloride reference substance;
(3) preparation of 2% cesium chloride solution: accurately weighing 5.0g, placing in a 250ml polypropylene volumetric flask, adding a proper amount of water for dissolving, diluting to a scale, and shaking up to obtain the product;
(4) preparation of a standard solution: precisely measuring reference substance solutions 2ml, 3ml, 4ml, 5ml and 6ml, respectively placing in 100ml polypropylene volumetric flasks, respectively adding 2% cesium chloride solution 5.0ml, adding water to dilute to scale, shaking up, and preparing a series of standard solutions as shown in the following table 1;
(5) preparing a test solution: precisely measuring 1ml, placing in a 100ml polypropylene volumetric flask, adding water to dilute to scale, shaking up, precisely measuring 1ml, placing in a 100ml polypropylene volumetric flask, adding 5.0ml of 2% cesium chloride solution, adding water to dilute to scale, and shaking up to obtain the product;
(6) preparing a blank solution: precisely weighing 40000.32031g of polyethylene glycol, placing the weighed materials into a 250ml polypropylene volumetric flask, adding a proper amount of water to dissolve the materials, diluting the materials to a scale, shaking up, precisely weighing 1ml of the materials, placing the materials into a 100ml polypropylene volumetric flask, adding 5.0ml of 2% cesium chloride solution, and shaking up to obtain the product;
(7) spectral conditions: the detection mode is as follows: flame is continuous; flame type: air-acetylene gas; detection wavelength: 589.0 nm; the width of the slit is as follows: 0.5 nm; lamp current: 5.0 mA; air flow rate: 13.50L/min; acetylene gas flow: 2.00L/min; height of the burner: 13.5 mm; lamp preheating time: 15 min;
(8) the blank solution, the standard solution and the sample solution were taken, absorbance was measured at a wavelength of 589.0nm according to atomic absorption spectrophotometry, as shown in the following table one, a linear regression equation was plotted according to the concentration and absorbance of the standard solution, as shown in fig. 1, and then the concentration (Ck) (mg/L) of sodium in the sample solution was calculated according to the regression equation.
TABLE 1 concentration and absorbance of standard solution and its linear equation
(III) presentation of the results of the analysis
The total sodium content in each bag of compound polyethylene glycol electrolyte powder is calculated according to the following formula according to the sodium concentration (Ck) (mg/L) in the test solution measured by the method of the invention according to the method (I) of registering standard method by using imported drugs and the method (II) respectively:
m Ck/1000/1000 2000 dilution factor/4
In the formula: m-total sodium content per bag (g); ck-concentration of sodium in the test solution (mg/L).
(IV) accuracy specificity experiments
The experimental method comprises the following steps:
preparation of linear solution: taking a proper amount of sodium chloride reference substances (corresponding to 75%, 100%, 125% and the concentration of a test sample) dried for 2 hours at 105 ℃, precisely weighing, placing the reference substances in a 100ml measuring flask, adding 0.037g of potassium chloride and 40003.2g of polyethylene glycol, adding water to dissolve and dilute the reference substances to scale, shaking up, precisely weighing 1ml, placing the reference substances in a 100ml plastic volumetric flask, adding water to dilute the reference substances to scale, shaking up, precisely weighing 2ml, 3ml, 4ml, 5ml and 6ml of the reference substances, respectively placing the reference substances in a 100ml plastic volumetric flask, respectively adding 5ml of 2% cesium chloride solution, adding water to dilute the reference substances to scale, and shaking up to obtain accurate solutions with the total sodium concentration of 3 high, medium and low.
The experimental results are shown in table 2;
the results show that: the average recovery rate is 99.92%, and the RSD is 1.32%, which shows that the method has high accuracy, high specificity and good instrument precision.
Table 2 recovery data are shown in the following table:
as can be seen from the above comparative test and various detection data, compared with the method for determining the total sodium content of the imported drug registration standard JX20170220, the method has the following advantages: the interference generated by the dissolution of sodium ions can be eliminated by using the measuring flask made of polypropylene material; by adding a 2% cesium chloride solution, cesium chloride ionizes itself to give free electrons and thereby inhibit sodium ionization, making the solution more stable.
In addition, through detection of samples in the same batch, the absorbance of the standard solution and the sample solution in the method is within the range of 0.1-0.5, the linear correlation coefficient of the standard curve can reach more than 0.999, and the absorbance of the standard solution and the sample solution in the standard method for registering the imported drugs is below 0.1, which shows that the absorbance value is smaller due to low sensitivity at the wavelength, and the linear correlation coefficient of the standard curve can only reach more than 0.99. And when the standard solution is returned, the recovery rate of the method is between 98 and 102 percent, and the recovery rate of the standard method for registering the imported drugs is rarely in the range of 98 to 102 percent. In conclusion, the method is simple and quick to operate, high in sensitivity and good in repeatability, and the solution in the method is good in stability and the measured data are more accurate.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. A method for measuring the total sodium content in compound polyethylene glycol electrolyte powder is characterized by comprising the following steps:
(1) preparing a reference substance solution: accurately weighing a sodium chloride reference substance, placing the sodium chloride reference substance in a polypropylene plastic volumetric flask, adding potassium chloride and polyethylene glycol 4000, diluting to a scale by using deionized water, preparing a reference substance solution with the sodium element concentration of 14.33494mg/L, and shaking up to obtain the sodium chloride reference substance;
(2) preparation of a standard solution: precisely measuring a plurality of reference substance solutions, respectively placing the reference substance solutions into polypropylene plastic volumetric flasks, respectively adding 3-8ml of 2% cesium chloride solution, diluting with deionized water to obtain sodium element series standard solution with concentration matched with that of the test solution, and shaking up to obtain the test solution;
(3) preparing a test solution: taking 4 bags of the contents of the compound polyethylene glycol electrolyte powder, placing the bags in a polypropylene plastic volumetric flask, adding deionized water for dilution, adding 3-8ml of 2% cesium chloride solution, then diluting the solution by using deionized water to reach the concentration matched with the sodium element series standard solution, and shaking up to obtain the compound polyethylene glycol electrolyte powder;
(4) preparing a blank solution: accurately weighing a proper amount of polyethylene glycol 4000, placing the polyethylene glycol 4000 in a polypropylene plastic volumetric flask, adding deionized water for dilution, adding 3-8ml of 2% cesium chloride solution, then diluting the solution by using the deionized water to reach a concentration matched with the solution of a test sample, and shaking up the solution to obtain the test sample;
(5) and (3) respectively taking the blank solution, the standard solution and the sample solution, measuring absorbance at a wavelength of 589.0nm according to an atomic absorption spectrophotometry, describing a regression equation according to the concentration and the absorbance of the standard solution, and calculating the concentration of sodium in the sample solution according to the regression equation.
2. The method for determining the total sodium content in the compound polyethylene glycol electrolyte powder according to claim 1, wherein in the step (1), the preparation method of the reference solution comprises the following steps:
weighing 0.1823g of sodium chloride reference substance precisely, placing in a 50ml polypropylene plastic volumetric flask, adding 0.0185g of potassium chloride and 40001.60g of polyethylene glycol, adding water for dissolving and diluting to scale, and shaking up; precisely measuring 1ml, placing in a 100ml polypropylene plastic volumetric flask, adding water to dilute to scale, and shaking up to obtain the product.
3. The method for determining the total sodium content in the compound polyethylene glycol electrolyte powder according to claim 1, wherein the preparation method of the standard solution in the step (2) comprises the following steps:
precisely measuring reference substance solutions 2ml, 3ml, 4ml, 5ml and 6ml, respectively placing into 100ml polypropylene plastic volumetric flasks, respectively adding 2% cesium chloride solution 5.0ml, adding water to dilute to scale, and shaking to obtain sodium series standard solutions 0.2867mg/L, 0.4303mg/L, 0.5737mg/L, 0.7172mg/L and 0.8606 mg/L.
4. The method for determining the total sodium content in the compound polyethylene glycol electrolyte powder according to claim 1, wherein the preparation method of the test solution in the step (3) comprises the following steps:
taking 4 bags of the contents of the compound polyethylene glycol electrolyte powder, placing the bags in a polypropylene plastic volumetric flask, adding a proper amount of deionized water to dissolve and dilute the solution to a scale, and taking the solution as a stock solution of a test sample;
precisely measuring 1ml of the stock solution of the sample, placing the stock solution in a 20ml polypropylene plastic volumetric flask, adding deionized water to dilute the stock solution to a scale, shaking the stock solution uniformly, precisely measuring 1ml of the stock solution, placing the stock solution in a 100ml polypropylene plastic volumetric flask, adding 5ml of 2% cesium chloride solution, adding water to dilute the stock solution to a scale, and shaking the mixture uniformly to obtain the test solution.
5. The method for determining the total sodium content in the compound polyethylene glycol electrolyte powder according to claim 1, wherein in the step (4), the preparation method of the blank solution comprises the following steps:
precisely weighing 40000.32g of polyethylene glycol, placing the weighed materials into a 250ml polypropylene plastic volumetric flask, adding a proper amount of deionized water to dissolve the materials to a scale, shaking up, precisely weighing 1ml of the materials, placing the materials into a 100ml polypropylene plastic volumetric flask, adding 5ml of 2% cesium chloride solution, adding a proper amount of deionized water to dissolve the materials to a scale, and shaking up to obtain the product.
6. The method for determining the total sodium content in the compound polyethylene glycol electrolyte powder according to claim 1, wherein in the steps (2), (3) and (4), the preparation method of the 2% cesium chloride solution comprises the following steps:
precisely weighing 5.00060g of cesium chloride, placing the cesium chloride in a 250ml polypropylene volumetric flask, adding a proper amount of water to dissolve the cesium chloride, diluting the cesium chloride to a scale mark, and shaking up the cesium chloride to obtain the cesium chloride.
7. The method for determining the total sodium content in the compound polyethylene glycol electrolyte powder as claimed in claim 1, wherein in the step (5), the atomic absorption spectrophotometry has the following spectral conditions:
the detection mode is as follows: flame is continuous; flame type: air-acetylene gas; detection wavelength: 589.0 nm; the width of the slit is as follows: 0.5 nm; lamp current: 5.0 mA; air flow rate: 13.50L/min; acetylene gas flow: 2.00L/min; height of the burner: 13.5 mm; lamp preheating time: and 15 min.
8. The method for determining the total sodium content in the compound polyethylene glycol electrolyte powder according to claim 1, wherein the atomic absorption spectrophotometry adopts an Agilent 240FS atomic absorption spectrophotometer, and the detection wavelength is 589.0 nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110342816.2A CN113029987A (en) | 2021-03-30 | 2021-03-30 | Method for measuring total sodium content in compound polyethylene glycol electrolyte powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110342816.2A CN113029987A (en) | 2021-03-30 | 2021-03-30 | Method for measuring total sodium content in compound polyethylene glycol electrolyte powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113029987A true CN113029987A (en) | 2021-06-25 |
Family
ID=76453030
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110342816.2A Pending CN113029987A (en) | 2021-03-30 | 2021-03-30 | Method for measuring total sodium content in compound polyethylene glycol electrolyte powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113029987A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113466149A (en) * | 2021-06-30 | 2021-10-01 | 上海耀大生物科技有限公司 | Method for measuring potassium chloride content in compound polyethylene glycol electrolyte powder |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101571478A (en) * | 2009-06-15 | 2009-11-04 | 株洲硬质合金集团有限公司 | Method for analyzing and detecting potassium and sodium impurity elements in vanadium carbide |
| CN103175794A (en) * | 2011-12-20 | 2013-06-26 | 四川科伦药物研究有限公司 | Method for determining content of sodium element in hydroxyethyl starch injection preparation |
| CN104964939A (en) * | 2015-06-30 | 2015-10-07 | 山东丹红制药有限公司 | Method for detecting content of sodium and potassium ions in Danhong injection |
| CN106645546A (en) * | 2016-10-20 | 2017-05-10 | 舒泰神（北京）生物制药股份有限公司 | Method for detecting content of sodium, potassium and chloride ions in polyethylene glycol electrolyte preparation |
-
2021
- 2021-03-30 CN CN202110342816.2A patent/CN113029987A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101571478A (en) * | 2009-06-15 | 2009-11-04 | 株洲硬质合金集团有限公司 | Method for analyzing and detecting potassium and sodium impurity elements in vanadium carbide |
| CN103175794A (en) * | 2011-12-20 | 2013-06-26 | 四川科伦药物研究有限公司 | Method for determining content of sodium element in hydroxyethyl starch injection preparation |
| CN104964939A (en) * | 2015-06-30 | 2015-10-07 | 山东丹红制药有限公司 | Method for detecting content of sodium and potassium ions in Danhong injection |
| CN106645546A (en) * | 2016-10-20 | 2017-05-10 | 舒泰神（北京）生物制药股份有限公司 | Method for detecting content of sodium, potassium and chloride ions in polyethylene glycol electrolyte preparation |
Non-Patent Citations (4)
| Title |
|---|
| 何燕莉: "原子吸收光谱法测定氨基酸葡萄糖注射液中钾、钠、钙、镁的含量", 《今日药学》 * |
| 李亚军 等: "离子色谱法测定复方聚乙二醇电解质散中钠钾的含量" * |
| 毛金银 等: "《仪器分析技术 供药品质量与管理、药品生产技术、食品检测技术专业用 第2版》", 31 January 2017, 中国医药科技出版社 * |
| 王曼熙: "聚乙二醇电解质散中氯化钾、碳酸氢钠的含量测定" * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113466149A (en) * | 2021-06-30 | 2021-10-01 | 上海耀大生物科技有限公司 | Method for measuring potassium chloride content in compound polyethylene glycol electrolyte powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101571478B (en) | Method for analyzing and detecting potassium and sodium impurity elements in vanadium carbide | |
| CN103134849A (en) | Quick method for simultaneously measuring potassium content and sodium content and calcium content and magnesium content in cigarette paper | |
| CN113029987A (en) | Method for measuring total sodium content in compound polyethylene glycol electrolyte powder | |
| CN101929959B (en) | Method for analyzing and detecting lead impurity element in beryllium-aluminum alloy | |
| Ganjali et al. | Novel erbium (III)-selective fluorimetric bulk optode | |
| CN113466149A (en) | Method for measuring potassium chloride content in compound polyethylene glycol electrolyte powder | |
| CN105067741A (en) | Method for measuring betaine content | |
| CN109239120A (en) | A kind of method of nuclear magnetic resonance hydrogen spectruming determining 1,2- Propylene Glycol Dinitrate moisture content | |
| CN106814144B (en) | Method for determining and analyzing content of dimethyl sulfate in dimethyl fumarate | |
| CN112798549B (en) | Method for determining sodium ion content in peritoneal dialysis solution by ultra-low acid hydrolysis-atomic absorption method | |
| CN113687016B (en) | Method for detecting chloride ion content in cyclobenzaprine hydrochloride | |
| CN104634778A (en) | Determination method for 2-chloromethyl-3,5 dimethyl-4-methoxyl pyridine hydrochloride | |
| RU2552311C2 (en) | Method of determining sodium thiosulphate in solutions | |
| CN111665228A (en) | Electric heating plate digestion-centrifugation-atomic fluorescence determination method for total arsenic in soil | |
| CN107991257B (en) | Quantitative detection method for content of sulfur monochloride and sulfur dichloride impurities in thionyl chloride | |
| CN104165965B (en) | Analysis method for determining content of mildronate bulk drug intermediate of 3-(2,2-dimethyl hydrazino)methyl propionate by non-aqueous titration | |
| CN111272897B (en) | Detection method of 2-amino-4,6-dihydroxypyrimidine and 4-amino-2,6-dihydroxypyrimidine in pemetrexed acid | |
| CN114184737B (en) | Method for measuring content of hexafluoro-cyclo-triphosphonitrile | |
| JPS6133467B2 (en) | ||
| McCormick et al. | Determination of nicotine in air | |
| CN104914091A (en) | Method for ICP analysis of sodium and potassium in low sodium salt | |
| Dougherty et al. | Spectrophotometric determination of nitrite ion with 4, 4'-bis (dimethylamino) thiobenzophenone | |
| CN113686799A (en) | Method for simultaneously determining potassium and sodium contents in balanced salt solution | |
| McDowell et al. | Determination of S (IV) at low parts per billion levels with anthranillic acid | |
| CN114002170A (en) | Method for measuring nicotine mobility of heated cigarette |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210625 |
|
| RJ01 | Rejection of invention patent application after publication |