CN113466149A - Method for measuring potassium chloride content in compound polyethylene glycol electrolyte powder - Google Patents
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- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000001103 potassium chloride Substances 0.000 title claims abstract description 42
- 235000011164 potassium chloride Nutrition 0.000 title claims abstract description 42
- 239000002202 Polyethylene glycol Substances 0.000 title claims abstract description 36
- 229920001223 polyethylene glycol Polymers 0.000 title claims abstract description 36
- 150000001875 compounds Chemical class 0.000 title claims abstract description 25
- 239000003792 electrolyte Substances 0.000 title claims abstract description 24
- 239000000843 powder Substances 0.000 title claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 72
- 239000013558 reference substance Substances 0.000 claims abstract description 39
- 239000012086 standard solution Substances 0.000 claims abstract description 39
- 239000012085 test solution Substances 0.000 claims abstract description 29
- 238000005303 weighing Methods 0.000 claims abstract description 28
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 21
- 239000011591 potassium Substances 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 238000002835 absorbance Methods 0.000 claims abstract description 19
- 239000012490 blank solution Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 61
- 239000004743 Polypropylene Substances 0.000 claims description 43
- -1 polypropylene Polymers 0.000 claims description 43
- 229920001155 polypropylene Polymers 0.000 claims description 43
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims description 38
- 229920003023 plastic Polymers 0.000 claims description 34
- 239000004033 plastic Substances 0.000 claims description 34
- 239000011550 stock solution Substances 0.000 claims description 21
- 238000007865 diluting Methods 0.000 claims description 20
- 238000001514 detection method Methods 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 238000012360 testing method Methods 0.000 claims description 13
- 238000003321 atomic absorption spectrophotometry Methods 0.000 claims description 11
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 7
- 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 5
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 5
- 239000012088 reference solution Substances 0.000 claims description 5
- 230000003595 spectral effect Effects 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 150000003109 potassium Chemical class 0.000 claims description 3
- 235000002639 sodium chloride Nutrition 0.000 claims description 3
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 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 abstract 1
- 229910052708 sodium Inorganic materials 0.000 abstract 1
- 239000011734 sodium Substances 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 25
- 239000003814 drug Substances 0.000 description 10
- 229940079593 drug Drugs 0.000 description 10
- 229910001414 potassium ion Inorganic materials 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 239000012488 sample solution Substances 0.000 description 6
- 238000010561 standard procedure Methods 0.000 description 4
- 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
- 239000003574 free electron Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 210000002429 large intestine Anatomy 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 206010010774 Constipation Diseases 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- 239000004111 Potassium silicate Substances 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
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 210000003736 gastrointestinal content Anatomy 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 1
- 229910052913 potassium silicate Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 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
- 239000000126 substance Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a method for measuring the content of potassium chloride in compound polyethylene glycol electrolyte powder, which comprises the following steps: (1) preparing a reference substance solution: preparing a potassium element reference substance solution; (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 potassium 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 766.5nm, describing a regression equation according to the concentration and the absorbance of the standard solution, and calculating the concentration of potassium chloride 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 potassium chloride 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 potassium chloride content in the imported drug registration standard JX20170220 is measured by adopting an atomic absorption spectrophotometry (standard curve method) to measure the absorbance at the wavelength of 404.4 nm. At least 5 parts of potassium 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 potassium 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 potassium 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 potassium chloride content. And 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, potassium ions are very easy to ionize, a common glass measuring flask contains potassium silicate, and the potassium ions are easily dissolved out of the wall of the glass container, 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 content of potassium chloride in compound polyethylene glycol electrolyte powder, which can effectively inhibit the ionization of potassium ions, has good linearity and repeatability and accurately detects the content of total potassium chloride, aiming at overcoming the defect of insufficient ionization of potassium ions in the existing measuring method.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for measuring the content of potassium chloride in compound polyethylene glycol electrolyte powder, which comprises the following steps:
(1) preparing a reference substance solution: accurately weighing a potassium chloride reference substance, placing the reference substance in a polypropylene plastic volumetric flask, adding anhydrous sodium sulfate, sodium bicarbonate, sodium chloride and polyethylene glycol 4000, diluting to a scale by using deionized water, preparing a reference substance solution with the concentration of potassium element of 19.7196mg/L, and shaking uniformly to obtain the potassium 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 potassium 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 potassium element series standard solution, and shaking up to obtain the potassium element series standard solution;
(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 test solution, measuring the absorbance at the wavelength of 766.5nm 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 potassium in the test solution according to the regression equation.
Further, in the step (1), the preparation method of the reference solution comprises:
taking 0.094g of potassium chloride reference substance, precisely weighing, placing in a250ml polypropylene plastic volumetric flask, adding 0.715g of anhydrous sodium sulfate, 0.21g of sodium bicarbonate, 0.185g of sodium chloride and 40008.0g of polyethylene glycol, adding water to dissolve and dilute to scale, and shaking up; and precisely measuring 10ml, placing in a 100ml polypropylene plastic volumetric flask, adding water to dilute to the scale, and shaking up to obtain the product.
Further, the preparation method of the standard solution in the step (2) comprises the following steps:
precisely measuring control solutions 2ml, 3ml, 4ml, 5ml and 6ml, respectively placing into 100ml polypropylene plastic volumetric flasks, adding 2% cesium chloride solution 3ml, adding water to dilute to scale, and shaking to obtain potassium series standard solutions 0.3944mg/L, 0.5916mg/L, 0.7888mg/L, 0.9860mg/L and 1.1832 mg/L.
Further, 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 2000ml polypropylene plastic volumetric flask, adding a proper amount of deionized water for dissolving and diluting to a scale, and taking the solution as a stock solution of a test sample;
precisely measuring 1ml of a sample stock solution, placing the sample stock solution into a 20ml polypropylene plastic volumetric flask, adding deionized water for diluting to a scale, shaking up, precisely measuring 1ml, placing the sample stock solution into a 50ml polypropylene plastic volumetric flask, adding 3ml of 2% cesium chloride solution, adding water for diluting to a scale, and shaking up to obtain the test solution.
Further, 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 a250ml polypropylene plastic volumetric flask, adding a proper amount of water to dissolve the materials to a scale, shaking up, precisely weighing 10ml, 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 product.
Further, 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 a250ml 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 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: 766.5 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 burner height: 13.5 mm; lamp preheating time: and 15 min.
Furthermore, the atomic absorption spectrophotometry adopts an Agilent 240FS atomic absorption spectrophotometer, and the detection wavelength is 766.5 nm.
By adopting the technical scheme, compared with the existing method and technology for measuring the content of the potassium chloride in the imported drug registration standard JX20170220, 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 the interference caused by dissolution of potassium 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 free electrons by itself to inhibit potassium ionization, so that the solution is more stable;
(3) through the detection of the same batch of samples, the linear correlation coefficient of a standard curve adopting the method can reach more than 0.999, and the absorbance of a standard solution and a test solution of an imported drug registration standard method is more than 0.97;
(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 potassium chloride content in the compound polyethylene glycol electrolyte powder by using the method of the present invention.
Detailed Description
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
The method for measuring the content of potassium chloride in the compound polyethylene glycol electrolyte powder comprises the following steps:
(1) preparing a reference substance solution: taking 0.094g of potassium chloride reference substance, precisely weighing, placing in a250ml polypropylene plastic volumetric flask, adding 0.715g of anhydrous sodium sulfate, 0.21g of sodium bicarbonate, 0.185g of sodium chloride and 40008.0g of polyethylene glycol, adding water to dissolve and dilute to scale, shaking up, precisely weighing 10ml, placing in a 100ml polypropylene plastic volumetric flask, adding water to dilute to scale, and shaking up to obtain the potassium chloride reference substance;
(2) preparation of a standard solution: precisely measuring reference substance solutions 2ml, 3ml, 4ml, 5ml and 6ml, respectively placing in 100ml polypropylene plastic volumetric flasks, respectively adding 2% cesium chloride solution 3ml, adding water to dilute to scale, and shaking to obtain potassium series standard solutions 0.3944mg/L, 0.5916mg/L, 0.7888mg/L, 0.9860mg/L and 1.1832 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 50ml polypropylene plastic volumetric flask, adding 3ml 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 a250ml polypropylene plastic volumetric flask, adding a proper amount of water to dissolve the materials to a scale, shaking up, precisely weighing 10ml 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 product;
(5) spectral conditions: the detection mode is as follows: flame is continuous; flame type: air-acetylene; gas detection wavelength: 766.5 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 the wavelength of 766.5nm 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 potassium 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:
the method comprises the following steps of (I) standard registration method of imported drugs:
(1) stock solution of test sample: taking the contents in the sample bag 4, precisely weighing, placing in a 2000ml measuring flask, adding appropriate amount of water, ultrasonically dissolving, adding water to dilute to scale, and shaking uniformly to obtain solution A; precisely measuring the solution A250ml, placing the solution in a 500ml measuring flask, diluting the solution to a scale with water, and shaking up to obtain a solution B;
(2) preparing a reference substance solution: 1.88g of potassium chloride reference substance dried for 2 hours at 130 ℃ is precisely weighed, placed in a 500ml measuring flask, added with 1.43g of anhydrous sodium sulfate, 0.42g of sodium bicarbonate, 0.37g of sodium chloride and 400016.0g of polyethylene glycol, dissolved in water and diluted to scale, and shaken uniformly;
(3) preparation of a standard solution: precisely measuring 5ml, 8ml, 10ml, 12ml and 15ml of reference substance solution, respectively placing in a 50ml volumetric flask, adding water to dilute to scale, and shaking uniformly to obtain a series of standard solutions, wherein the potassium concentration is 98.6023mg/L, 157.7636mg/L, 197.2046mg/L, 236.6455mg/L and 295.8068mg/L in sequence;
(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 40003.2g of polyethylene glycol reference substance, placing in a 100ml measuring flask, adding water to dilute to scale, and shaking up;
(6) setting the spectral conditions: the detection mode is as follows: flame is continuous; flame type: air-acetylene gas; detection wavelength: 404.4 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;
(7) 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 potassium chloride in the sample solution according to the regression equation.
(II) the method for measuring the content of potassium chloride in the compound polyethylene glycol electrolyte powder
(1) Preparing a stock solution of a test sample: taking the contents in the 4 bags of the test sample, precisely weighing, placing in a 2000ml measuring flask, adding a proper amount of water, ultrasonically dissolving, adding water to dilute to a scale, and shaking uniformly to serve as a test sample stock solution;
(2) preparing a reference substance solution: taking 0.094g of potassium chloride reference substance dried for 2 hours at 130 ℃, precisely weighing, placing in a250ml measuring flask, adding 0.715g of anhydrous sodium sulfate, 0.21g of sodium bicarbonate, 0.185g of sodium chloride and 40008.0g of polyethylene glycol, adding water to dissolve and dilute to scale, shaking up, precisely weighing 10ml, placing in a 100ml polypropylene volumetric flask, adding water to dilute to scale, and shaking up to obtain the product;
(3) preparation of 2% cesium chloride solution: accurately weighing 5.0g, placing in a250ml 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 3.0ml, adding water to dilute to scale, and shaking up to obtain a series of standard solutions, wherein the potassium concentrations are 0.3944mg/L, 0.5916mg/L, 0.7888mg/L, 0.9860mg/L and 1.1832mg/L in sequence;
(5) preparing a test solution: precisely measuring 1ml, placing in a 20ml polypropylene volumetric flask, adding water to dilute to scale, shaking up, precisely measuring 1ml, placing in a 50ml polypropylene volumetric flask, adding 3.0ml 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 40000.32g of polyethylene glycol, placing the weighed materials into a250ml 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 3.0ml of 2% cesium chloride solution, and shaking up to obtain the product;
(7) setting the spectral conditions: the detection mode is as follows: flame is continuous; flame type: air-acetylene gas; detection wavelength: 766.5 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 operation method comprises the following steps: and (3) taking the blank solution, the standard solution and the sample solution, measuring the absorbance at the wavelength of 766.5nm 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 potassium in the sample solution 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
Calculating the potassium chloride content in each bag of compound polyethylene glycol electrolyte powder according to the following formula according to the potassium concentration (Ck) (mg/L) in the test solution measured by the method of the invention respectively according to the method (I) adopting the standard registration method of the imported drugs and the method (II) adopting the standard registration method of the imported drugs:
M-Ck/1000/1000-2000 dilution factor/4-74.55/39.1
In the formula: m-amount of potassium chloride per bag (g); ck-concentration of potassium in the test solution (mg/L).
(IV) accuracy specificity experiments
Preparation of the accuracy solution: taking a proper amount of potassium 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 of potassium chloride with 3 concentrations at high, medium and low levels. 3 parts of each concentration is prepared in parallel, 9 parts of solutions with the 3 concentrations are respectively injected and measured, and the experimental results are shown in table 2.
The results show that: the average recovery rate is 100.7%, and the RSD is 0.7%, which shows that the method has high accuracy, high specificity and good instrument precision.
Table 2 recovery data:
(V) stability test
The reference solution and the test solution are respectively subjected to sample injection detection by the detection method at 0 hour, 2 hours, 4 hours, 8 hours, 12 hours and 24 hours, the detected content is compared with the content at 0 hour, and the stability data are shown in the following table 3.
TABLE 3 stability test data
| Time | Content g of sample | The content ratio of the water to the water is 0 percent | STD3 content g | The content ratio of the water to the water is 0 percent |
| 0h | 0.757 | / | 0.09467 | / |
| 2h | 0.754 | 99.5 | 0.09428 | 99.6 |
| 4h | 0.763 | 100.7 | 0.09575 | 101.1 |
| 8h | 0.756 | 99.9 | 0.09390 | 99.2 |
| 12h | 0.748 | 98.8 | 0.09431 | 99.6 |
| 24h | 0.748 | 98.7 | 0.09419 | 99.5 |
As can be seen from the above comparative test and each detection data, compared with the method for determining the content of potassium chloride in the imported drug registration standard JX20170220, the method has the following advantages: the interference generated by potassium ion dissolution can be eliminated by using the polypropylene measuring flask; by adding a 2% cesium chloride solution, cesium chloride ionizes by itself to give free electrons, thereby inhibiting potassium ionization and making the solution more stable.
In addition, the linear correlation coefficient of the standard curve of the method can reach more than 0.999 through the detection of the same batch of samples, and the linear correlation coefficient of the standard curve of the standard method for registering imported drugs can only reach more than 0.97. And when the standard solution returns, 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. The method has the advantages of simple and quick operation, high sensitivity, good repeatability, good solution stability and more accurate measured data.
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 content of potassium chloride in compound polyethylene glycol electrolyte powder is characterized by comprising the following steps:
(1) preparing a reference substance solution: accurately weighing a potassium chloride reference substance, placing the reference substance in a polypropylene plastic volumetric flask, adding anhydrous sodium sulfate, sodium bicarbonate, sodium chloride and polyethylene glycol 4000, diluting to a scale by using deionized water, preparing a reference substance solution with the concentration of potassium element of 19.7196mg/L, and shaking uniformly to obtain the potassium 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 potassium 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 potassium element series standard solution, and shaking up to obtain the potassium element series standard solution;
(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 test solution, measuring the absorbance at the wavelength of 766.5nm 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 potassium in the test solution according to the regression equation.
2. The method for determining the content of potassium chloride 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:
taking 0.094g of potassium chloride reference substance, precisely weighing, placing in a250ml polypropylene plastic volumetric flask, adding 0.715g of anhydrous sodium sulfate, 0.21g of sodium bicarbonate, 0.185g of sodium chloride and 40008.0g of polyethylene glycol, adding water to dissolve and dilute to scale, and shaking up; and precisely measuring 10ml, placing in a 100ml polypropylene plastic volumetric flask, adding water to dilute to the scale, and shaking up to obtain the product.
3. The method for determining the content of potassium chloride 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 control solutions 2ml, 3ml, 4ml, 5ml and 6ml, respectively placing into 100ml polypropylene plastic volumetric flasks, adding 2% cesium chloride solution 3ml, adding water to dilute to scale, and shaking to obtain potassium series standard solutions 0.3944mg/L, 0.5916mg/L, 0.7888mg/L, 0.9860mg/L and 1.1832 mg/L.
4. The method for determining the content of potassium chloride 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 2000ml polypropylene plastic volumetric flask, adding a proper amount of deionized water for dissolving and diluting to a scale, and taking the solution as a stock solution of a test sample;
precisely measuring 1ml of a sample stock solution, placing the sample stock solution into a 20ml polypropylene plastic volumetric flask, adding deionized water for diluting to a scale, shaking up, precisely measuring 1ml, placing the sample stock solution into a 50ml polypropylene plastic volumetric flask, adding 3ml of 2% cesium chloride solution, adding water for diluting to a scale, and shaking up to obtain the test solution.
5. The method for determining the content of potassium chloride 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 a250ml polypropylene plastic volumetric flask, adding a proper amount of water to dissolve the materials to a scale, shaking up, precisely weighing 10ml, 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 product.
6. The method for determining the content of potassium chloride 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 a250ml 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 content of potassium chloride in the compound polyethylene glycol electrolyte powder according to 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: 766.5 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 burner height: 13.5 mm; lamp preheating time: and 15 min.
8. The method for determining the content of potassium chloride in the compound polyethylene glycol electrolyte powder according to claim 1, wherein an Agilent 240FS atomic absorption spectrophotometer is adopted in the atomic absorption spectrophotometry, and the detection wavelength is 766.5 nm.
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