CN112326870A - Method for measuring chloride content in compound polyethylene glycol electrolyte powder - Google Patents
Method for measuring chloride content in compound polyethylene glycol electrolyte powder Download PDFInfo
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- CN112326870A CN112326870A CN202011055910.1A CN202011055910A CN112326870A CN 112326870 A CN112326870 A CN 112326870A CN 202011055910 A CN202011055910 A CN 202011055910A CN 112326870 A CN112326870 A CN 112326870A
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- polyethylene glycol
- electrolyte powder
- glycol electrolyte
- compound polyethylene
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- 238000000034 method Methods 0.000 title claims abstract description 26
- 150000001875 compounds Chemical class 0.000 title claims abstract description 15
- 239000002202 Polyethylene glycol Substances 0.000 title claims abstract description 14
- 239000003792 electrolyte Substances 0.000 title claims abstract description 14
- 229920001223 polyethylene glycol Polymers 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 title claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 16
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 16
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012488 sample solution Substances 0.000 claims abstract description 9
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 8
- 229920001353 Dextrin Polymers 0.000 claims abstract description 7
- 239000004375 Dextrin Substances 0.000 claims abstract description 7
- 235000019425 dextrin Nutrition 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 7
- 229910021538 borax Inorganic materials 0.000 claims abstract description 6
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 6
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052709 silver Inorganic materials 0.000 claims abstract description 5
- 239000004332 silver Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 39
- 239000012085 test solution Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000007865 diluting Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 239000003269 fluorescent indicator Substances 0.000 claims 1
- 238000004448 titration Methods 0.000 abstract description 11
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 abstract description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 abstract description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 abstract description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 16
- 238000012360 testing method Methods 0.000 description 9
- 235000011164 potassium chloride Nutrition 0.000 description 8
- 239000001103 potassium chloride Substances 0.000 description 8
- 239000011780 sodium chloride Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 238000011084 recovery Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 239000000460 chlorine Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- FTLYMKDSHNWQKD-UHFFFAOYSA-N (2,4,5-trichlorophenyl)boronic acid Chemical compound OB(O)C1=CC(Cl)=C(Cl)C=C1Cl FTLYMKDSHNWQKD-UHFFFAOYSA-N 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
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 229940057838 polyethylene glycol 4000 Drugs 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 229940085605 saccharin sodium Drugs 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 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
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/82—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a precipitate or turbidity
- G01N21/83—Turbidimetric titration
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Plasma & Fusion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The content of chloride in the compound polyethylene glycol electrolyte powder is determined by selecting a fluorescent yellow indicator and a silver precipitation method, and the interference of sodium bicarbonate in the compound polyethylene glycol electrolyte powder is eliminated by using dilute sulfuric acid. And (3) taking a proper amount of sample solution, placing the sample solution in a conical flask, adding 1 drop of phenolphthalein indicator, 5ml of 2% dextrin solution, 2ml of 2.5% borax solution and a proper amount of dilute sulfuric acid to ensure that the red color disappears and 5-8 drops of yellow fluorescence indicator solution, and titrating the solution by using silver nitrate titration solution (0.1mol/L) until the fluorescence color of the solution fades and becomes light pink.
Description
Technical Field
The invention relates to a method for measuring chloride content in compound polyethylene glycol electrolyte powder, which adopts a silver precipitation method to measure the chloride content in the compound polyethylene glycol electrolyte powder.
Background
The silver precipitation method is a titration analysis method based on precipitation reaction. The precipitation titration method must meet the conditions of 1. the solubility is small, and can be quantitatively completed; 2. the reaction speed is high; 3. with an appropriate indicator to indicate endpoint; 4. the adsorption phenomenon did not affect the endpoint observation.
The compound polyethylene glycol electrolyte powder is a compound preparation and consists of raw material medicines of polyethylene glycol 4000, sodium chloride, potassium chloride, sodium bicarbonate, sodium sulfate and an auxiliary material of saccharin sodium. The product has complex components and more influence factors. The compound polyethylene glycol electrolyte powder (III) has no obvious titration end point and is difficult to observe when detected according to the imported drug registration standard JX 20170714.
Dextrin solution is a colloid protective agent, so that the precipitate in the titration process is not aggregated, and the titration endpoint is easier to observe.
Disclosure of Invention
The invention aims to provide a novel chloride content determination method which has the advantages of accurate determination, good reproducibility, simple operation and high analysis speed.
In order to achieve the purpose, the invention is realized by the following technical scheme: the method for measuring the content of chloride in the compound polyethylene glycol electrolyte powder comprises the following steps:
preparation of a test solution: taking 1 bag of compound polyethylene glycol electrolyte powder, placing in a 1000ml measuring flask, adding appropriate amount of water, dissolving with ultrasound, diluting with water to scale, and shaking to obtain test solution.
The determination method comprises the following steps: the method comprises the steps of precisely measuring 50ml of a sample solution, placing the sample solution in a conical flask, adding 1 drop of phenolphthalein indicator, 5ml of 2% dextrin solution, 2ml of 2.5% borax solution and a proper amount of dilute sulfuric acid to make red disappear, adding 5-8 drops of a fluorescent yellow indicator solution, titrating the solution with a silver nitrate titration solution (0.1mol/L) until the fluorescent color of the solution fades to become light pink, wherein each 1ml of the silver nitrate titration solution (0.1mol/L) is equivalent to 0.003545g of Cl.
The invention has the beneficial technical effects that: the invention provides a method for preparing a composite material. The content of chloride in the compound polyethylene glycol electrolyte powder is determined by selecting a fluorescent yellow indicator and a silver precipitation method, and the interference of sodium bicarbonate in the compound polyethylene glycol electrolyte powder is eliminated by using dilute sulfuric acid.
Drawings
FIG. 1 is a graph showing a standard curve of chlorine content.
Detailed Description
In order to verify the effect of the measuring method of the invention, the inventor carries out a large number of experiments and scientifically verifies the finally determined measuring method, and the verification experiments are as follows:
specificity test
Blank solvent: water (W)
Test solution: taking 1 bag of the product, placing in a 1000ml measuring flask, adding appropriate amount of water, dissolving with ultrasound, diluting with water to scale, and shaking.
Blank adjuvant solution: precisely weighing about 71.5g of blank auxiliary materials in the prescription amount without containing sodium chloride and potassium chloride, putting the blank auxiliary materials in a 1000ml measuring flask, adding a proper amount of water to dissolve, adding water to dilute to a scale, and shaking up.
Respectively and precisely measuring 50ml of a blank solvent, 50ml of a blank auxiliary material solution and 50ml of a sample solution, placing the blank solvent, the blank auxiliary material solution and the sample solution in a conical flask, adding 1 drop of phenolphthalein indicator, 5ml of 2% dextrin solution, 2ml of 2.5% borax solution and a proper amount of dilute sulfuric acid to make red disappear, adding 5-8 drops of a fluorescent yellow indicator, and titrating the solution by using silver nitrate titrating solution (0.1mol/L) until the fluorescent color of the solution fades and becomes light pink.
After 1 drop of the titration solution is dripped into the blank solvent and the blank auxiliary material solution, no precipitate is generated, a precipitate is generated after the titration solution is dripped into the test solution, the fluorescence color of the solution fades to become light pink, and the end point phenomenon is obvious. Test results show that the content determination method has good specificity.
Linearity and range
Linear stock solution: precisely weighing about 1.46g of sodium chloride and 0.75g of potassium chloride as raw materials, putting into a 100ml volumetric flask, and adding water to dissolve to obtain the product.
The linear stock solution was diluted to 1 as follows#～5#Linear solutions. Taking the linear solution No. 1-5, adding 1 drop of phenolphthalein indicator, 5ml of 2% dextrin solution, 2ml of 2.5% borax solution and a proper amount of dilute sulfuric acid to ensure that the red color disappears, and 5-8 drops of yellow fluorescence indicator solution, and titrating by using silver nitrate titrating solution (0.1mol/L) until the solution becomes light pink when the fluorescence color fades. Linear regression analysis was performed using chlorine content as abscissa and volume of consumed silver nitrate titration solution (0.1mol/L) as ordinate. See in particular fig. 1.
TABLE 1 dilution procedure
TABLE 2 Linear test results
The test result shows that the chlorine content is in the range of 31.14 mg-93.42 mg (equivalent to the range of 50% -150% of the limit concentration) and shows good linearity.
Accuracy of
Test solution: weighing about 3.57g (equivalent to 0.073g of sodium chloride and 0.0375g of potassium chloride) of blank auxiliary materials except for sodium chloride and potassium chloride, precisely weighing 9 parts, respectively placing in conical flasks, and precisely weighing 3 parts of each of 0.0365g of sodium chloride and 0.0188g of potassium chloride; 0.073g of sodium chloride raw material and 0.0375g of potassium chloride raw material, 3 parts of each; 0.1095g of sodium chloride raw material and 0.0562g of potassium chloride raw material, 3 parts of each. Adding 50ml water respectively to dissolve, making into sample solution containing chloride of about 50%, 100%, and 150%, and shaking.
And adding 1 drop of phenolphthalein indicator, 5ml of 2% dextrin solution, 2ml of 2.5% borax solution and a proper amount of dilute sulfuric acid into the test solution to ensure that the red color disappears, and titrating 5-8 drops of yellow fluorescence indicator solution by using silver nitrate titrating solution (0.1mol/L) until the fluorescent color of the solution fades and becomes light pink. The content was measured, the measured values were compared with the theoretical values, the recovery was calculated, and the relative standard deviation of the 9 recovery data was calculated.
TABLE 3 accuracy test results
The method determines that the recovery rate of the high, medium and low concentration contents is between 99.0 and 101.0 percent, the average recovery rate is 99.33 percent, the RSD is 0.28 percent and is less than 1.0 percent; the method meets the requirements, and the test result shows that the method has high accuracy and good recovery rate.
Repeatability of
The content of 6 test solutions was calculated by the analyst a taking out the test solution under the same conditions.
TABLE 8 results of the repeatability tests
The content determination result RSD of 6 samples is 0.47 and less than 1.0 percent by parallel determination, and the test result shows that the method has good repeatability.
Intermediate precision
Taking the test solution by different analysts B at different time conditions for measurement, and calculating the content of 6 test solutions; finally, the RSD of 12 content data was calculated in combination with 6 content data (operator a assay) for reproducibility.
TABLE 9 intermediate precision
Different operators measure 6 samples in parallel at different time, the content measurement result RSD is 0.61%, the content repeatability and the 12 data RSD of the intermediate precision are 0.55%, and both are less than 1.0%, and the test result shows that the intermediate precision of the method is good.
Claims (1)
1. A method for measuring the content of chloride in compound polyethylene glycol electrolyte powder is characterized in that: the method adopts a silver precipitation method for determination, and comprises the following steps:
1) preparation of a test solution: taking 1 bag of compound polyethylene glycol electrolyte powder, placing in a 1000ml measuring flask, adding appropriate amount of water, dissolving with ultrasound, diluting with water to scale, and shaking to obtain test solution.
2) The determination method comprises the following steps: precisely measuring 50ml of sample solution, placing the sample solution in a conical flask, adding 1 drop of phenolphthalein indicator, 5ml of 2% dextrin solution, 2ml of 2.5% borax solution and a proper amount of dilute sulfuric acid to ensure that red disappears, adding 5-8 drops of yellow fluorescent indicator solution, and titrating the solution by using 0.1mol/L of silver nitrate titrating solution until the fluorescent color of the solution fades and becomes light pink.
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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 |
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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 |
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Application publication date: 20210205 |
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