CN110988256A - EDTA titration method for rapidly determining Zn content in vitamin C + zinc sustained release tablets - Google Patents
EDTA titration method for rapidly determining Zn content in vitamin C + zinc sustained release tablets Download PDFInfo
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- CN110988256A CN110988256A CN201911398799.3A CN201911398799A CN110988256A CN 110988256 A CN110988256 A CN 110988256A CN 201911398799 A CN201911398799 A CN 201911398799A CN 110988256 A CN110988256 A CN 110988256A
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- G—PHYSICS
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention relates to an EDTA titration method for rapidly determining Zn content in vitamin C + zinc sustained-release tablets, comprising the following steps of preparing dilute acetic acid solution; step two, sample treatment, step three, titration test. Calculating the Zn content in the sample according to the titration volume; the EDTA titration method for rapidly determining the Zn content in the vitamin C + zinc sustained-release tablets improves the existing sample treatment method, is more applicable, increases 95% ethanol as a cosolvent in the sample dissolving process, has obvious judgment on sample treatment time and titration end point and high recovery rate, and is suitable for the actual detection of the Zn content in the vitamin C + zinc sustained-release tablets (such as CTEM, MTHW and the like).
Description
Technical Field
The invention relates to the technical field of analysis and determination of components of nutritional and healthy products, in particular to an EDTA titration method for rapidly determining the Zn content in vitamin C + zinc sustained-release tablets.
Background
Zn is one of the essential trace elements for human body, plays an extremely important role in the development process of human body, can not be synthesized and stored by human body, and must be taken from the outside, so the Zn is known as 'flowers of life' and 'sources of intelligence'. It can maintain normal appetite and improve immunity. The existing determination methods of the Zn content in the nutritional and healthy products comprise a Chinese pharmacopoeia (Ch.P) method, a GB1903.4 method, an ICP-OES method and the like, wherein the ICP-OES method has long sample detection time and high detection cost, and the methods specified in the Ch.P method and the GB1903.4 have insufficient sample dissolution and difficult determination of titration end points, so that the detection time is too long and the detection error is too large.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides an EDTA titration method for rapidly determining the Zn content in the vitamin C + zinc sustained-release tablets.
The technical scheme adopted by the invention for solving the technical problems is as follows: an EDTA titration method for rapidly determining the Zn content in a vitamin C + zinc sustained release tablet comprises the following specific steps:
step one, preparing a dilute acetic acid solution: measuring 50-70mL of acetic acid, adding 500-700mL of water, mixing and shaking uniformly, diluting with water to 900-1100mL, and mixing uniformly to obtain a dilute acetic acid solution;
step two, sample treatment: taking 20 vitamin C + zinc sustained-release tablets, grinding, mixing uniformly, weighing 3-5g of sample in a 500mL conical flask, adding 18-22mL of 95% ethanol, dissolving by ultrasonic for 8-12min, adding 100mL of dilute acetic acid solution, dissolving by ultrasonic for 15-25min, adding 100mL of water, and mixing uniformly to obtain a sample solution;
step three, titration test: adding 40-60mg of xylenol orange into a sample solution, dissolving and mixing, adding 1.0-3.0g of urotropine, dissolving, titrating by using 0.03-0.06mol/L disodium Ethylene Diamine Tetraacetate (EDTA) until a purple-pink solution turns to orange, and calculating the Zn content in the vitamin C + zinc sustained-release tablet to be detected according to the titration result of the sample solution, wherein the calculation formula of the Zn content in the vitamin C + zinc sustained-release tablet is as follows:
in the formula: c: the concentration of EDTA titration solution, mol/L;
v: volume consumed by EDTA titration, mL;
w: average tablet weight, g/tablet;
m: sample weight, g.
The dilute acetic acid solution in the first step is prepared by the following steps: 60mL of acetic acid is weighed, 600mL of water is added, the mixture is stirred evenly, diluted to 1000mL by water and mixed evenly.
And step two, the sample treatment is to take 20 vitamin C + zinc sustained-release tablets, grind the tablets, mix the tablets evenly, weigh 4g of the sample into a 500mL conical flask, add 20mL of 95% ethanol, dissolve the sample by ultrasonic for 10min, add 100mL of dilute acetic acid solution, dissolve the sample by ultrasonic for 20min, add 100mL of water and mix the solution evenly, and take 95% ethanol as a cosolvent.
And the titration test in the third step is that 50mg of xylenol orange is added into the sample solution, dissolved and mixed, and after 2.0g of urotropine is added for dissolution, 0.05mol/L of Ethylene Diamine Tetraacetic Acid (EDTA) is used for titration until the purple-pink solution becomes orange, and the xylenol orange is used as an indicator.
The EDTA titration method for rapidly determining the Zn content in the vitamin C + zinc sustained release tablets has the beneficial effects that compared with the traditional mode: the method is more reasonable, and the 95% ethanol is added as the cosolvent to realize accurate determination of the Zn content, has high accuracy, obviously shortens the detection time, is suitable for actual detection of the Zn content in nutritional and healthy products, uses xylenol orange as an indicator, has more obvious judgment of the end point color after urotropine is added and dissolved in a sample solution, is more suitable for improving the existing sample processing method, is suitable for increasing the 95% ethanol as the cosolvent in the sample dissolving process, has obvious judgment of the sample processing time and the titration end point, has high recovery rate, and is suitable for actual detection of the Zn content in vitamin C + zinc sustained-release tablets (such as CTEM, MTHW and the like).
Detailed Description
The present invention will now be described in further detail.
Example 1:
batch number: CTEM19N3001 (CTEM: Slow Release Vitamin C & Zinc Tablet manufacturer: Jiangsu Elande Nutrition Co., Ltd.: Standard RDSOP6287601 of Jiangsu Elande Nutrition Co., Ltd.)
Step one, preparing a dilute acetic acid solution: measuring 60mL of acetic acid, adding 600mL of water, shaking up, diluting with water to 1000mL, and mixing uniformly to obtain a dilute acetic acid solution, wherein the dilute acetic acid is added to ensure that Zn in a sample completely reacts in the solution, so that the final detection result is influenced;
step two, sample treatment: taking 20 tablets of the product, grinding, uniformly mixing, weighing about 4g of sample into a 500mL conical flask, adding 20mL of 95% ethanol, ultrasonically dissolving for 10min, adding 100mL of diluted acetic acid, ultrasonically dissolving for 20min, adding 100mL of water, and uniformly mixing to obtain a sample solution, wherein 95% ethanol is used as a cosolvent to prevent the binder HPMC-4000CP in the sustained-release tablet from forming a cluster in the sample dissolving process, and wrapping Zn in the sample to influence the final detection result;
step three, titration test: adding 50mg of xylenol orange into the sample solution, dissolving and mixing, adding 2.0g of urotropine, dissolving, and titrating by using 0.05mol/L disodium ethylene diamine tetraacetate until the purple-pink solution becomes orange;
calculating the formula:
in the formula: c: the concentration of EDTA titration solution, mol/L;
v: volume consumed by EDTA titration, mL;
w: average tablet weight, g/tablet;
m: sample weight, g.
The invention is implemented specifically as follows: the first example was determined in comparison to the prior art method:
the experimental result shows that the recovery rate of the novel method is 100.2%, and the fact proves that the method can accurately measure the Zn content in the CTEM sample, is closer to the theoretical content than the original method, has reliable data, meets the detection requirement, and has high accuracy, good reproducibility and short detection period.
Example 2:
batch number: MTHW19N3001 (MTHW: Slow Released Vitamin C & Zinc Tablet manufacturer: Jiangsu Elande Nutrition Co., Ltd. meet the standard: Jiangsu Elande Nutrition Co., Ltd. standard RDSOP6290701)
Step one, preparing a dilute acetic acid solution: measuring 60mL of acetic acid, adding 600mL of water, shaking up, diluting with water to 1000mL, and mixing uniformly to obtain a dilute acetic acid solution, wherein the dilute acetic acid is added to ensure that Zn in a sample completely reacts in the solution, so that the final detection result is influenced;
step two, sample treatment: taking 20 tablets of the product, grinding, uniformly mixing, weighing about 4g of sample into a 500mL conical flask, adding 20mL of 95% ethanol, performing ultrasonic dissolution for 10min, adding 100mL of diluted acetic acid, performing ultrasonic dissolution for 20min, adding 100mL of water, uniformly mixing to obtain a sample solution, adding 95% ethanol as a cosolvent to prevent the binder HPMC-4000CP in the sustained-release tablet from forming a cluster in the sample dissolution process, and wrapping Zn in the sample to influence the final detection result.
Adding 50mg of xylenol orange into the sample solution, dissolving and mixing, adding 2.0g of urotropine, dissolving, and titrating by using 0.05mol/L disodium ethylene diamine tetraacetate until the purple-pink solution becomes orange;
calculating the formula:
in the formula: c: the concentration of EDTA titration solution, mol/L;
v: volume consumed by EDTA titration, mL;
w: average tablet weight, g/tablet
M: sample weight, g.
The invention is implemented specifically as follows: the second example compares the measurements with the prior art method:
the experimental result shows that the recovery rate of the novel method is 100.6%, and the fact proves that the method can accurately measure the Zn content in the MTHW sample, the Zn content is closer to the theoretical content than the original method, the data is reliable, the method meets the detection requirement, the accuracy is high, the reproducibility is good, and the detection period is short.
The method is suitable for the actual test of the Zn content in the vitamin C + zinc sustained-release tablets.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (4)
1. An EDTA titration method for rapidly determining Zn content in vitamin C + zinc sustained release tablets is characterized by comprising the following steps:
step one, preparing a dilute acetic acid solution: measuring 50-70mL of acetic acid, adding 500-700mL of water, mixing and shaking uniformly, diluting with water to 900-1100mL, and mixing uniformly to obtain a dilute acetic acid solution;
step two, sample treatment: taking 20 vitamin C + zinc sustained-release tablets, grinding, mixing uniformly, weighing 3-5g of sample in a 500mL conical flask, adding 18-22mL of 95% ethanol, dissolving by ultrasonic for 8-12min, adding 100mL of dilute acetic acid solution, dissolving by ultrasonic for 15-25min, adding 100mL of water, and mixing uniformly to obtain a sample solution;
step three, titration test: adding 40-60mg of xylenol orange into a sample solution, dissolving and mixing, adding 1.0-3.0g of urotropine, dissolving, titrating by using 0.03-0.06mol/L disodium Ethylene Diamine Tetraacetate (EDTA) until a purple-pink solution turns to orange, and calculating the Zn content in the vitamin C + zinc sustained-release tablet to be detected according to the titration result of the sample solution, wherein the calculation formula of the Zn content in the vitamin C + zinc sustained-release tablet is as follows:
in the formula: c: the concentration of EDTA titration solution, mol/L;
v: volume consumed by EDTA titration, mL;
w: average tablet weight, g/tablet;
m: sample weight, g.
2. The EDTA titration method for rapidly determining the Zn content in vitamin C + zinc sustained release tablets according to claim 1, which is characterized in that: the dilute acetic acid solution in the first step is prepared by the following steps: 60mL of acetic acid is weighed, 600mL of water is added, the mixture is stirred evenly, diluted to 1000mL by water and mixed evenly.
3. The EDTA titration method for rapidly determining the Zn content in vitamin C + zinc sustained release tablets according to claim 1, which is characterized in that: and step two, the sample treatment is to take 20 vitamin C + zinc sustained-release tablets, grind the tablets, mix the tablets evenly, weigh 4g of the sample into a 500mL conical flask, add 20mL of 95% ethanol, dissolve the sample by ultrasonic for 10min, add 100mL of dilute acetic acid solution, dissolve the sample by ultrasonic for 20min, add 100mL of water and mix the solution evenly, and take 95% ethanol as a cosolvent.
4. The EDTA titration method for rapidly determining the Zn content in vitamin C + zinc sustained release tablets according to claim 1, which is characterized in that: and the titration test in the third step is that 50mg of xylenol orange is added into the sample solution, dissolved and mixed, and after 2.0g of urotropine is added for dissolution, 0.05mol/L of Ethylene Diamine Tetraacetic Acid (EDTA) is used for titration until the purple-pink solution becomes orange, and the xylenol orange is used as an indicator.
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| CN103954730A (en) * | 2014-05-22 | 2014-07-30 | 山东安能输送带橡胶有限公司 | Method for detecting barium and zinc in zinc-barium liquid compound stabilizer |
| CN104007226A (en) * | 2014-05-04 | 2014-08-27 | 华南理工大学 | Method for measuring zinc content in hexavalent-chromium passivating solution for hot galvanizing |
| CN106841512A (en) * | 2016-12-23 | 2017-06-13 | 东北制药集团沈阳第制药有限公司 | A kind of method for detecting VC contents in vitamin C solid beverage |
| CN108572234A (en) * | 2017-03-07 | 2018-09-25 | 常州市五洲环保科技有限公司 | A kind of method of calcium Zn content in quick measurement calcium of organic acid zinc salt |
| CN109444328A (en) * | 2018-12-26 | 2019-03-08 | 重庆健能医药开发有限公司 | A kind of Direct spectrophotometry method in Zinc calcium gluconate oral solution |
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2019
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Patent Citations (10)
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| CN101696940A (en) * | 2009-10-10 | 2010-04-21 | 四川省畜科饲料有限公司 | Method for measuring zinc lactate content by measuring zinc content |
| CN101816753A (en) * | 2010-03-15 | 2010-09-01 | 江西新赣江药业有限公司 | Method for detecting quality of compound preparation for treating cold |
| CN103091449A (en) * | 2012-11-13 | 2013-05-08 | 江苏艾兰得营养品有限公司 | Method for identifying vitamin C content in vitamin/mineral health product |
| CN103091320A (en) * | 2012-11-13 | 2013-05-08 | 江苏艾兰得营养品有限公司 | Method for testing content of titanium dioxide by complexometric titration-back titration method |
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| CN103954730A (en) * | 2014-05-22 | 2014-07-30 | 山东安能输送带橡胶有限公司 | Method for detecting barium and zinc in zinc-barium liquid compound stabilizer |
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Application publication date: 20200410 |