CN105628861A - Method for quickly measuring content of vitamin C in Fructus lycii - Google Patents
Method for quickly measuring content of vitamin C in Fructus lycii Download PDFInfo
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- CN105628861A CN105628861A CN201610076573.1A CN201610076573A CN105628861A CN 105628861 A CN105628861 A CN 105628861A CN 201610076573 A CN201610076573 A CN 201610076573A CN 105628861 A CN105628861 A CN 105628861A
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- fructus lycii
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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
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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
- G01N21/75—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
- G01N21/78—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 change of colour
- G01N21/79—Photometric titration
Abstract
The invention relates to a method for measuring content of vitamin C in Fructus lycii, in particular to a method for quickly measuring content of vitamin C in Fructus lycii, and aims to solve the technical problem that decoloring or oxidizing needs to be performed on sample liquid and the technical problems of need for preparing many drugs, large instrument-equipment investment, complex operation and high time consumption. The method includes: 1, preparing a to-be-measured sample; 2, performing acid-base neutralization titration; 3, titrating for a blank test; 4, calculating content of vitamin C in Fructus lycii. The method has the advantages that decoloring or oxidizing does not need to be performed on colored sample liquid to be measured, the method has the advantages of small investment, low reagent consumption, simple operation, high stability and wide application range and is suitable for quickly measuring content of vitamin C in Fructus lycii, and the measuring range can be conveniently adjusted by increasing filtrate sampling amount or increasing sample liquid diluting ratio. The method is applied to measuring content of vitamin C in Fructus lycii.
Description
Technical field
The present invention relates to and a kind of measure the method for Vitamin C content in Fructus Lycii.
Background technology
Vitamin C (Vc), chemical name is ascorbic acid, hexuronic acid, and molecular formula is C6H8O6, molecular weight is 176.13, and sterling is white crystals or crystalline powder, odorless, sour in the mouth. Vitamin C is water soluble vitamins, and aqueous solution, in acidity, has reproducibility. Vitamin C is widely present in water fruits and vegetables, is one of the important indicator of fruit, vegetables quality inspection. Vitamin C is not only nutrient substance that human body needs, is also medical drugs, is also antioxidant conventional in food industry. Vitamin C can not synthesize in human body, and the vitamin C needed in human body mainly absorbs from fresh vegetables and fruit. The production of people, life tool are of great significance by Accurate Determining food with ascorbic content in medicine. At present, ascorbic assay method is broadly divided into physical method and chemical method. Physical method has polarimetry; Chemical method has titrimetry such as iodimetric titration, 2,6-dichloroindophenol titrimetrys, electrochemical methods, phenylhydrazine colorimetry, fluorescence method and high performance liquid chromatography etc. Adopt above-mentioned all methods to measure coloured fruit and vegerable sample to be required for its sample is decoloured or oxidation processes, and the generation of above-mentioned chemical method is all around what ascorbic reproducibility was launched. Vitamin C is often caused damage by coloured fruit and vegerable sample decolorising agent, especially as the decolouring of the such dark fruit and vegerable sample liquid of Fructus Lycii, mainly sample liquid is carried out desolventing technology by decolorizing with activated carbon and organic solvent extraction, decolorizing with activated carbon can cause ascorbic loss to make measurement not accurate, the decolouring of organic solvent extraction sample liquid is also not thorough, due to the coloured existence of sample liquid, greatly interfere with ascorbic mensuration in Fructus Lycii. It is bad that it is measured effect by 2,6-conventional dichloroindophenol redox titration methods, so being rarely employed. So ascorbic mensuration is mainly the instrumental methods such as fluorescence method, spectrophotography and high performance liquid chromatography in Fructus Lycii, sample liquid should carrying out desolventing technology or oxidation processes during mensuration, prepare many medicines again, instrument and equipment investment is big, complicated operation, the time used is long.
Summary of the invention
Sample liquid should be carried out desolventing technology or oxidation processes to solve ascorbic assay method in current Fructus Lycii by the present invention, prepare many medicines again, technical problem big, complicated operation, time length used invested by instrument and equipment, and provides a kind of method of Vitamin C content in quick mensuration Fructus Lycii.
In a kind of quick mensuration Fructus Lycii of the present invention, the method for Vitamin C content carries out according to the following steps:
One, testing sample is prepared: put in mortar by Fructus Lycii to be measured for 1g��2g, add acid solution and be totally immersed in acid solution to Fructus Lycii to be measured, Fructus Lycii to be measured is ground to form homogenate, homogenate is moved in the volumetric flask of 100mL, with acid solution wash mortar and washing liquid to be poured into the volumetric flask of 100mL, then it is settled to scale with acid solution, after shaking up, stands 10min, filter, obtain filtrate;
Two, acid base neutralization titration: the filtrate taking 10mL step one is placed in the conical flask of 250mL, add the deionized water of 50mL��100mL, add the phenolphthalein solution that 3 mass fractions are 0.5% to give instruction agent, carry out being titrated to pink colour with standard caustic soda solution, record the volume V of standard solution sodium hydroxide solution usedn;
Three, the titration of blank assay: take the acid solution of 10mL to the conical flask being placed in 250mL, add the deionized water of 50mL��100mL, add the phenolphthalein solution that 3 mass fractions are 0.5% to give instruction agent, carry out being titrated to pink colour with standard caustic soda solution, record the volume V of standard solution sodium hydroxide solution used0;
Four, ascorbic content in Fructus Lycii is calculated:
X=C �� (Vn-V0) �� M �� 10/W,
X is the amount of contained vitamin C in Fructus Lycii to be measured, and unit is mg/g,
C is the concentration of standard caustic soda solution, and unit is mol/L,
VnBeing the volume of standard solution sodium hydroxide solution used in step 2, unit is mL,
V0Being the volume of standard solution sodium hydroxide solution used in step 3, unit is mL,
W is the quality of Fructus Lycii to be measured, and unit is g,
M is ascorbic molal weight is 176.13g/mol;
Acid solution described in step one is concentration is aqueous hydrochloric acid solution or the oxalic acid aqueous solution of 0.001mol/L��0.1mol/L;
The concentration of the standard caustic soda solution described in step 2 is 0.001mol/L��0.1mol/L;
The solute of the acid solution described in step 3 is all identical with the acid solution described in step one with concentration;
The concentration of the standard caustic soda solution described in step 3 is identical with the standard caustic soda solution described in step 2.
Advantages of the present invention:
Coloured sample liquid to be measured in the method for the present invention is made without decolouring or oxidation processes, filtrate shade adds 50mL��100mL water and is diluted processing per sample, uses phenolphthalein to give instruction agent, uses standard caustic soda solution titration, sample liquid is by yellowish complexion changed pink colour, and variable color is obvious;
The present invention has small investment, and agents useful for same is few, simple to operate, good stability, feature applied widely, it is adaptable to the quick mensuration of Vitamin C content in Fructus Lycii, measurement range can pass through the method increasing filtrate sampling amount or increasing sample liquid extension rate, carries out convenient adjustment.
Accompanying drawing explanation
Fig. 1 is according to ascorbic content and Vn-V in the testing sample of the Plotting data of table 1 in test one0Relation curve.
Detailed description of the invention
Detailed description of the invention one: present embodiment is a kind of method of Vitamin C content in quick mensuration Fructus Lycii, specifically carries out according to the following steps:
One, testing sample is prepared: put in mortar by Fructus Lycii to be measured for 1g��2g, add acid solution and be totally immersed in acid solution to Fructus Lycii to be measured, Fructus Lycii to be measured is ground to form homogenate, homogenate is moved in the volumetric flask of 100mL, with acid solution wash mortar and washing liquid to be poured into the volumetric flask of 100mL, then it is settled to scale with acid solution, after shaking up, stands 10min, filter, obtain filtrate;
Two, acid base neutralization titration: the filtrate taking 10mL step one is placed in the conical flask of 250mL, add the deionized water of 50mL��100mL, add the phenolphthalein solution that 3 mass fractions are 0.5% to give instruction agent, carry out being titrated to pink colour with standard caustic soda solution, record the volume V of standard solution sodium hydroxide solution usedn;
Three, the titration of blank assay: take the acid solution of 10mL to the conical flask being placed in 250mL, add the deionized water of 50mL��100mL, add the phenolphthalein solution that 3 mass fractions are 0.5% to give instruction agent, carry out being titrated to pink colour with standard caustic soda solution, record the volume V of standard solution sodium hydroxide solution used0;
Four, ascorbic content in Fructus Lycii is calculated:
X=C �� (Vn-V0) �� M �� 10/W,
X is the amount of contained vitamin C in Fructus Lycii to be measured, and unit is mg/g,
C is the concentration of standard caustic soda solution, and unit is mol/L,
VnBeing the volume of standard solution sodium hydroxide solution used in step 2, unit is mL,
V0Being the volume of standard solution sodium hydroxide solution used in step 3, unit is mL,
W is the quality of Fructus Lycii to be measured, and unit is g,
M is ascorbic molal weight is 176.13g/mol;
Acid solution described in step one is concentration is aqueous hydrochloric acid solution or the oxalic acid aqueous solution of 0.001mol/L��0.1mol/L;
The concentration of the standard caustic soda solution described in step 2 is 0.001mol/L��0.1mol/L;
The solute of the acid solution described in step 3 is all identical with the acid solution described in step one with concentration;
The concentration of the standard caustic soda solution described in step 3 is identical with the standard caustic soda solution described in step 2.
Detailed description of the invention two: the difference of present embodiment and detailed description of the invention one is: the collocation method of the aqueous hydrochloric acid solution described in step one is: with pipet take 9.4mL mass fraction be 37.5% hydrochloric acid put in 1000mL volumetric flask, dilute, it is settled to scale, obtain the aqueous hydrochloric acid solution that concentration is 0.1mol/L, be then diluted according to actual needs. Other are identical with detailed description of the invention one.
Detailed description of the invention three: the present embodiment difference from detailed description of the invention one or two is: the compound method of the standard caustic soda solution described in step 2 is: the NaOH weighing 4g is dissolved in deionized water in small beaker, then move in the volumetric flask of 1000mL and be diluted with water to scale, demarcate with Potassium Hydrogen Phthalate, obtain standard caustic soda solution, be then diluted according to actual needs. Other are identical with detailed description of the invention one or two.
Beneficial effects of the present invention is verified by tests below:
Test one: this test is the relation of test vitamin C consumption and sodium hydroxide concentration, and concrete grammar is:
1, the preparation of reagent:
The aqueous hydrochloric acid solution of 0.1mol/L: with pipet take 9.4mL mass fraction be 37.5% hydrochloric acid put in 1000mL volumetric flask, dilute, be settled to scale, obtain the aqueous hydrochloric acid solution that concentration is 0.1mol/L;
The preparation of standard solution of sodium hydroxide: the NaOH weighing 4g is dissolved in deionized water in small beaker, then move in the volumetric flask of 1000mL and be diluted with water to scale, demarcate with Potassium Hydrogen Phthalate, obtain the standard caustic soda solution that concentration is 0.09909mol/L, then dilution 10 times, obtains the standard caustic soda solution that concentration is 0.009909mol/L;
The preparation of ascorbic standard solution: weigh 1.2500g vitamin C and be diluted with water to scale in the volumetric flask of 250mL, obtains the vitamin C standard solution of 5mg/mL;
2, prepare testing sample: in the conical flask of 10 250mL, add 0 respectively, the vitamin C standard solution of 5mg/mL of step one configuration of 1mL, 2mL, 3mL, 4mL, 5mL, 6mL, 7mL, 8mL and 9mL, be labeled as headpin, No. 2 bottles, No. 3 bottles, No. 4 bottles, kingpin, No. 6 bottles, No. 7 bottles, No. 8 bottles, No. 9 bottles and No. 10 bottles successively; Then in headpin, No. 2 bottles, No. 3 bottles, No. 4 bottles, kingpin, No. 6 bottles, No. 7 bottles, No. 8 bottles, No. 9 bottles and No. 10 bottles, add the deionized water of 9.5mL, 8.5mL, 7.5mL, 6.5mL, 5.5mL, 4.5mL, 3.5mL, 2.5mL, 1.5mL and 0.5ml successively, the aqueous hydrochloric acid solution of the 0.1mol/L of each step one configuration adding 0.5mL in 10 conical flasks, obtains 10 testing samples again;
3, titration testing sample: 3 mass fractions of each addition are the phenolphthalein solution of 0.5% in 10 testing samples, each deionized water adding 50mL in 10 testing samples again, be pink colour with solution to the solution in 10 testing samples of standard caustic soda solution titration that concentration is 0.009909mol/L of step one preparation, headpin, No. 2 bottles, No. 3 bottles, No. 4 bottles, kingpin, No. 6 bottles, No. 7 bottles, No. 8 bottles, No. 9 bottles and No. 10 bottle correspondence quota of expenditure sodium hydroxide solution volumes respectively are V0��V1��V2��V3��V4��V5��V6��V7��V8And V9, wherein the standard caustic soda solution volume of the vitamin C consumption of corresponding volume is Vn�CV0;
The relation of the volume of the standard caustic soda solution of the consumption of vitamin C standard solution and corresponding consumption is shown in table 1 below,
Table 1
Fig. 1 be the Plotting data according to table 1 testing sample in ascorbic content and Vn-V0Relation curve, equation of linear regression Y=5.697X-0.1182, R2=0.9998 (n=10). It is shown that measuring ascorbic content with sodium hydroxide titration be good linear relationship, vitamin C can be neutralized reaction with highly basic sodium hydroxide equimolar ratio as one organic monoacid, and may indicate that terminal with phenolphthalein agent of giving instruction. Therefore may utilize ascorbic weak acid character standard caustic soda solution and it is carried out titration, and calculate ascorbic content.
Test two: taking the Fructus Lycii dry granular of commercially available three kinds of different prices, carry out the mensuration of Vitamin C content X (mg/g) in sample by the method for the present invention, measurement result is as follows:
Ascorbic content in the different sample Fructus Lycii of table 2
Through calculating, the average recovery rate of the detection method of this test is 98.12%, and relative average debiation is 1.8%, and relative standard deviation is 5.15%.
Claims (3)
1. the method for Vitamin C content in a quick mensuration Fructus Lycii, it is characterised in that the method for Vitamin C content in Fructus Lycii that quickly measures carries out according to the following steps:
One, testing sample is prepared: put in mortar by Fructus Lycii to be measured for 1g��2g, add acid solution and be totally immersed in acid solution to Fructus Lycii to be measured, Fructus Lycii to be measured is ground to form homogenate, homogenate is moved in the volumetric flask of 100mL, with acid solution wash mortar and washing liquid to be poured into the volumetric flask of 100mL, then it is settled to scale with acid solution, after shaking up, stands 10min, filter, obtain filtrate;
Two, acid base neutralization titration: the filtrate taking 10mL step one is placed in the conical flask of 250mL, add the deionized water of 50mL��100mL, add the phenolphthalein solution that 3 mass fractions are 0.5% to give instruction agent, carry out being titrated to pink colour with standard caustic soda solution, record the volume V of standard solution sodium hydroxide solution usedn;
Three, the titration of blank assay: take the acid solution of 10mL to the conical flask being placed in 250mL, add the deionized water of 50mL��100mL, add the phenolphthalein solution that 3 mass fractions are 0.5% to give instruction agent, carry out being titrated to pink colour with standard caustic soda solution, record the volume V of standard solution sodium hydroxide solution used0;
Four, ascorbic content in Fructus Lycii is calculated:
X=C �� (Vn-V0) �� M �� 10/W,
X is the amount of contained vitamin C in Fructus Lycii to be measured, and unit is mg/g,
C is the concentration of standard caustic soda solution, and unit is mol/L,
VnBeing the volume of standard solution sodium hydroxide solution used in step 2, unit is mL,
V0Being the volume of standard solution sodium hydroxide solution used in step 3, unit is mL,
W is the quality of Fructus Lycii to be measured, and unit is g,
M is ascorbic molal weight is 176.13g/mol;
Acid solution described in step one is concentration is aqueous hydrochloric acid solution or the oxalic acid aqueous solution of 0.001mol/L��0.1mol/L;
The concentration of the standard caustic soda solution described in step 2 is 0.001mol/L��0.1mol/L;
The solute of the acid solution described in step 3 is all identical with the acid solution described in step one with concentration;
The concentration of the standard caustic soda solution described in step 3 is identical with the standard caustic soda solution described in step 2.
2. the method for Vitamin C content in a kind of quick mensuration Fructus Lycii according to claim 1, it is characterized in that the collocation method of the aqueous hydrochloric acid solution described in step one is: with pipet take 9.4mL mass fraction be 37.5% hydrochloric acid put in 1000mL volumetric flask, dilute, it is settled to scale, obtain the aqueous hydrochloric acid solution that concentration is 0.1mol/L, be then diluted according to actual needs.
3. the method for Vitamin C content in a kind of quick mensuration Fructus Lycii according to claim 1, it is characterized in that the compound method of the standard caustic soda solution described in step 2 is: the NaOH weighing 4g is dissolved in deionized water in small beaker, then move in the volumetric flask of 1000mL and be diluted with water to scale, demarcate with Potassium Hydrogen Phthalate, obtain standard caustic soda solution, be then diluted according to actual needs.
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| CN109507248A (en) * | 2018-12-12 | 2019-03-22 | 中国科学院兰州化学物理研究所 | With the method for glucose content in Instrument for Measuring Blood Sugar measurement fructus lycii |
| CN111380998A (en) * | 2018-12-27 | 2020-07-07 | 江苏艾兰得营养品有限公司 | Iodine titration method for rapidly determining VC content in vitamin C sustained-release tablets |
| CN113533632A (en) * | 2021-08-30 | 2021-10-22 | 西安乐析医疗科技有限公司 | Method for measuring total chlorine content in balanced salt solution for perfusion |
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