CN100373152C - Method for measuring galacturonic acid in fruit juice and beverage - Google Patents
Method for measuring galacturonic acid in fruit juice and beverage Download PDFInfo
- Publication number
- CN100373152C CN100373152C CNB200410073309XA CN200410073309A CN100373152C CN 100373152 C CN100373152 C CN 100373152C CN B200410073309X A CNB200410073309X A CN B200410073309XA CN 200410073309 A CN200410073309 A CN 200410073309A CN 100373152 C CN100373152 C CN 100373152C
- Authority
- CN
- China
- Prior art keywords
- galacturonic acid
- resin
- deionized water
- sample
- standard solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The present invention relates to a method for measuring galacturonic acid in fruit juices and beverages, which can reduce cost and quickly measure the content of galacturonic acid in a smaple to be measured by means of a resin absorption and spectrophotometric method for measuring galacturonic acid in fruit juices and beverage. The present invention comprises the following operation steps that (1) standard solutions containing galacturonic acid standard solutions and galacturonic acid series standard solutions are prepared; (2) the sample is processed; (3) the sample is preprocessed; (4) the resins are packed; (5) the standard solutions are absorbed by the resin and desorbed; (6) a standard curve is made; (7) the sample is measured; (8) the content is calculated.
Description
One, technical field:
The present invention relates to a kind of method of measuring galacturonic acid in fruit juice, the beverage, its galacturonic acid that is applicable to fruits and vegetables inspissated juice, fruit-vegetable juice beverage, beverage etc. detects.
Two, background technology:
At present, the production of fruit juice industry develops to international direction, continual renovation along with production technology, equipment, quality requirements to product also improves constantly, the European market begins the galacturonic acid content in the fruit juice has been made preliminary regulation, require in the samples of juice of 11.5Brix galacturonic acid content less than 1000mg/L, this is not for to playing the consideration of security, but propose at production technology and management level.The at present domestic method of still not having galacturonic acid in the mensuration fruit juice, the method of existing mensuration galacturonic acid is only applicable to can be with the isolated material of polymer pectin of galacturonic acid, and the galacturonic acid in the fruit juice is a micromolecule, adopts conventional alcohol precipitation obviously unworkable.The external high performance liquid chromatography that adopts, sample preparation is simpler, but advances chromatographic column] to go out the peak measured value consuming time longer, and generally about 200,000 yuan, therefore this method cost input for domestic fruit juice manufacturing enterprise is too high for its price.
Three, summary of the invention:
The present invention is in order to solve the weak point in the above-mentioned background technology, a kind of method of measuring galacturonic acid in fruit juice, the beverage is provided, it adopts galacturonic acid in resin adsorption-spectrophotometry fruit juice, the beverage, can reduce the detection cost, quickly and easily the galacturonic acid content in the working sample.
For achieving the above object, the technical solution used in the present invention is:
A kind of method of measuring galacturonic acid in fruit juice, the beverage, its special character is to comprise following operation steps: (1) sampling; (2) filter; (3) resin adsorption, desorb; (4) measure; (5) calculate content.
Comprise following operation steps:
(1) preparing standard solution: comprise preparation galacturonic acid standard solution and preparation series standard solution;
(2) sample preparation;
(3) pre-service of resin;
(4) dress post;
(5) resin adsorption, desorb;
(6) do typical curve;
(7) test sample;
(8) calculate content.
Comprise following operation steps:
(1) preparing standard solution: comprise preparation galacturonic acid standard solution and preparation series standard solution, accurately take by weighing galacturonic acid, use the deionized water dissolving constant volume, get the galacturonic acid standard solution, preserve standby; Draw the sodium standard then and use liquid, place volumetric flask respectively, be diluted to scale with deionized water again, promptly be made into the series standard solution that contains sodium, use deionized water as zero standard solution;
(2) sample preparation: refilter if the sample pol, then is diluted to 11.5Brix earlier greater than 11.5Brix; If the sample pol is less than 11.5Brix, direct filtration then;
(3) pre-service of resin: resin is used H earlier
2SO
4Handle 1h, float to neutrality with deionized water, handle 1h with NaOH then, deionized water floats to neutrality;
(4) dress post: measure the good resin of pre-service, water dress post, rinsing;
(5) resin adsorption, wash-out: draw the fruit juice of handling well, deionized water flush away neutral sugar is used in absorption then, uses the NaOH desorb at last; With the deionized water is blank, and operation as above;
(6) do typical curve: adopting spectrophotometer, reagent blank is measured absorbance respectively, is ordinate with the absorbance, and the galacturonic acid concentration is a horizontal ordinate, does typical curve;
(7) test sample: method is the same;
(8) calculate content: calculate galacturonic acid concentration in the reading substitution typical curve with solution to be measured, just obtain the galacturonic acid content in the sample under the 11.5Brix after multiply by extension rate.
Compared with prior art, the advantage and the effect that have of the present invention is as follows:
1, sulfuric acid carbazole method is widely used in the pectous material as a kind of method of more common mensuration galacturonic acid, and does not still have a relevant bioassay standard for being determined at of the galacturonic acid content in the fruit juice is domestic.The present invention utilizes the adsorbability of LX200 resin to acid, by the acid in the adsorption-desorption separation fruit juice, eliminates the interference of neutral sugar wherein, measures galacturonic acid with sulfuric acid carbazole method then.Resin is a kind of recyclable materials, and its maximum characteristics are can reuse up to a hundred times even thousands of times, therefore utilize resin can reduce the detection cost.Spectrophotometric structure is very simple, and the galacturonic acid content in the working sample, and this instrument low price quickly and easily is the conventional sense instrument of fruit juice manufacturing enterprise.
2, spectrophotometric ultimate principle is that material in the solution excites down in the irradiation of light, produced absorption effect to light, material is to have optionally to the absorption of light, various material all has its absorption spectrum separately, therefore when certain monochromatic light passes through solution, play its energy and will be absorbed and weaken, the degree that luminous energy weakens and the concentration of material have certain proportionate relationship, promptly meet colorimetric principle-law of Beer.When the optical path length of incident light, absorption coefficient and solution is constant, transmitted light is that the concentration according to solution changes, the galacturonic acid and the concentrated sulphuric acid can generate intermediate product 5-formyl-2 furancarboxylic acid when heating, this product can with the carbazole displaing amaranth, the depth of colour developing is relevant with concentration, can be in the 530nm quantitative measurement.
Four, description of drawings:
Accompanying drawing is a process chart of the present invention.
Five, embodiment:
1, preparing standard solution:
Preparation galacturonic acid standard solution: accurately take by weighing galacturonic acid 500mg, be settled to 100mL with deionized water dissolving, get 5mg/mL galacturonic acid standard solution, 4 ℃ of preservations are standby;
Preparation series standard solution: absorption 1.0,2.0,4.0,6.0,8.0,10.0mL sodium standard are used liquid, place the 50mL volumetric flask respectively, be diluted to scale with deionized water again, promptly be made into the series standard solution that contains sodium 100,200,400,600,800,1000mg/L, use deionized water as zero standard solution;
2, sample preparation: refilter if the sample pol, then is diluted to 11.5Brix earlier greater than 11.5Brix; If the sample pol is less than 11.5Brix, direct filtration then;
3, the pre-service of resin: the H that the LX200 resin is used the 0.25mol/L of 2-3BV earlier
2SO
4Handle 1h, float to neutrality with deionized water, the 2%NaOH with 2-3BV handles 1h then, and deionized water floats to neutrality.The desorb of galacturonic acid is the LX200 regeneration of resin, the LX100 resin H of the 0.25mol/L of 2-3BV
2SO
4Handle 1h, the same pre-service of regenerating, regeneration can directly be carried out on post;
4, dress post: post is the chromatographic column of internal diameter 20mm, high 20-30mm, measures the good resin of 10mL pre-service, water dress post, rinsing;
5, resin adsorption, desorb: draw the fruit juice (or galacturonic acid solution) that 10.0mL handles well, flow velocity absorption with 1mL/min, use deionized water flush away neutral sugar (the galacturonic acid post is operated equally) then, use the NaOH desorb of 90mL2% at last, flow velocity 0.5mL/min is settled to 100mL; Is blank with the deionized water, the operation as above contrast of cider to be measured is the malic acid that is equivalent to fruit juice acidity, then adopts corresponding acid based on the sample of other acid, as citric acid, tartrate etc.;
6, do typical curve: 7 in test tube getting 20 * 20mm, inject each 6mL of the concentrated sulphuric acid with suction pipe, slowly add above-mentioned each 1mL of galacturonic acid standard solution that crosses the variable concentrations behind the resin then respectively, after fully mixing, in boiling water bath, heated 10 minutes immediately, after being cooled to room temperature, add 0.15% each 0.5mL of carbazole solution, fully mix, after room temperature is placed 30min, adopt 723 type spectrophotometers, under wavelength 530nm, reagent blank is measured absorbance respectively, with the absorbance ordinate, the galacturonic acid concentration is a horizontal ordinate, does typical curve;
7, test sample: method is the same;
8, calculate content: calculate galacturonic acid concentration in the reading substitution typical curve with solution to be measured, just obtain the galacturonic acid content in the sample under the 11.5Brix after multiply by extension rate.
Wherein reagent comprises:
1, deionized water is used in experiment: meet the requirement of the one-level water of regulation among the GB GB6682-92 " analyzing experimental water specification and experimental technique ".
2, ethanol: analyze pure absolute ethyl alcohol.
3, exquisite ethanol: get and analyze pure absolute ethyl alcohol 1000mL, add zinc powder 4g and sulfuric acid (1:1) 4mL, put in the water bath with thermostatic control behind the backflow 10h, with full glass apparatus distillation, the every 1000mL adding zinc powder of distillate and each 4g of potassium hydroxide carry out redistillation.
4,0.15% carbazole ethanolic solution: take by weighing chemical pure carbazole 0.15g, be dissolved in exquisite ethanol, and be settled to 100mL, the carbazole dissolving slowly need be stirred.
5, standard galacturonic acid: with the D-galacturonic acid (containing a part water) of sigma company as the standard galacturonic acid.
6, sulfuric acid: the high-quality pure concentrated sulphuric acid.
7, malic acid: DL-malic acid, sigma company.
8, NaOH: analyze pure.
Instrument and material comprise:
1, VIS-723 type spectrophotometer, the Beijing Rayleigh Analytical Instrument Co.,Ltd.
2, HH SY21-Ni6C electric-heated thermostatic water bath, the long bearing instruments and meters in Beijing company.
3, the accurate pH meter of Phs-3B, Shanghai thunder magnetic instrument plant.
4, hand-held saccharimeter, optical instrument factory, Quanzhou, Fujian.
5, LX200 resin, LX100 resin, sorbing material Ltd is changed in the blue deep friendship in Xi'an.
Statistical evaluation of the present invention: the accuracy of the inventive method:
With the content of galacturonic acid in the galacturonic acid standard solution mensuration galacturonic acid standard solution of same train concentration, measurement result such as table 1.
Table 1
| Measure number of times | Galacturonic acid mg/L | ||||||||
| 20 | 30 | 40 | 50 | 60 | 70 | 80 | 100 | 120 | |
| 1234 absolute error relative errors (%) | 20.458 16.889 20.525 19.347 1.187 5.93 | 30.686 29.883 32.418 31.193 1.104 3.68 | 39.373 35.742 40.356 38.969 1.568 3.92 | 52.682 48.556 46.464 51.833 2.374 4.75 | 58.197 61.324 64.338 57.389 2.519 4.20 | 69.369 72.138 62.139 68.356 3.069 4.38 | 77.137 81.887 81.293 82.338 2.095 2.62 | 100.500 97.600 98.213 102.356 1.761 1.76 | 119.927 122.378 118.331 119.369 1.188 0.99 |
With high performance liquid chromatography comparative result such as table 2:
Table 2
| 1 | 2 | 3 | 4 | 5 | |
| HPLC method measured value resin adsorption-spectrophotometric method measured value absolute error relative error (%) | 53.5 58.26 0.476 8.90 | 174.9 155.80 1.91 10.9 | 225.3 204.56 2.074 9.21 | 415.6 392.71 2.289 5.51 | 687.1 665.67 2.143 3.12 |
Relative error is in the error range that general analysis allowed, and when content was 0.01-0.1%, the relative error of permission was 50-20%, and when content was 0.001-0.01%, the relative error of permission was 100-50%.The adsorption process of resin is the process of absorbate enrichment, and the sample low to content can strengthen upper column quantity, to improve measuring accuracy.
The precision of the inventive method:
After getting two parts of concentrated apple juice sample preparation, survey the content of galacturonic acid, 8 times measured values are as shown in table 3 with average measurement result.The precision of this method survey galacturonic acid content is good as shown in Table 3.
Table 3
Interference experiment:
Experiment finds when following ion excess exists mensuration is had interference:
C (Fe
3+) 0.00005%, c (NO
3 -) 0.00005%, c (Cu
3+) 0.00005% o'clock, add to measure in the liquid behind the developer and blueness or blue-green occur, so the above-mentioned ion in testing sample or the agents useful for same (mainly being the concentrated sulphuric acid) can influence mensuration when exceeding standard, so should the strict purity of controlling institute's water and sulfuric acid and other reagent.Since by resin adsorption galacturonic acid not only arranged, also have a large amount of acid that exist in the fruit juice such as malic acid, experimental results show that in the concentration range of fruit juice the influence of malic acid is a systematic error, can be by the contrast deduction.
Variable concentrations sample tie-in 4 times, observing under the situation that concentration difference exists seldom influences measurement result, the results are shown in Table 4.As can be seen from Table 4, therefore the Variation Lines number average of the galacturonic acid measurement result of four parts of variable concentrations does not carry and pollutes generation within the conventional range of variation in laboratory.
The different galacturonic acid concentrations of table 4 carry variation (mg/L)
Claims (1)
1. method of measuring galacturonic acid in fruit juice, the beverage is characterized in that comprising following operation steps:
(1) preparing standard solution: comprise preparation galacturonic acid standard solution and preparation series standard solution, accurately take by weighing galacturonic acid, use the deionized water dissolving constant volume, get the galacturonic acid standard solution, preserve standby; Draw the sodium standard then and use liquid, place volumetric flask respectively, be diluted to scale with deionized water again, promptly be made into the series standard solution that contains sodium, use deionized water as zero standard solution;
(2) sample preparation: refilter if the sample pol, then is diluted to 11.5Brix earlier greater than 11.5Brix; If the sample pol is less than 11.5Brix, direct filtration then;
(3) pre-service of resin: resin is used H earlier
2SO
4Handle 1h, float to neutrality with deionized water, handle 1h with NaOH then, deionized water floats to neutrality; Wherein, used resin is the LX200 resin;
(4) dress post: measure the good resin of pre-service, water dress post, rinsing;
(5) resin adsorption, wash-out: draw the fruit juice of handling well, deionized water flush away neutral sugar is used in absorption then, uses the NaOH desorb at last; With the deionized water is blank, and operation as above;
(6) do typical curve: adopting spectrophotometer, reagent blank is measured absorbance respectively, is ordinate with the absorbance, and the galacturonic acid concentration is a horizontal ordinate, does typical curve;
(7) test sample: method is the same;
(8) calculate content: calculate galacturonic acid concentration in the reading substitution typical curve with solution to be measured, just obtain the galacturonic acid content in the sample under the 11.5Brix after multiply by extension rate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410073309XA CN100373152C (en) | 2004-11-23 | 2004-11-23 | Method for measuring galacturonic acid in fruit juice and beverage |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410073309XA CN100373152C (en) | 2004-11-23 | 2004-11-23 | Method for measuring galacturonic acid in fruit juice and beverage |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1664577A CN1664577A (en) | 2005-09-07 |
| CN100373152C true CN100373152C (en) | 2008-03-05 |
Family
ID=35035767
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200410073309XA Expired - Fee Related CN100373152C (en) | 2004-11-23 | 2004-11-23 | Method for measuring galacturonic acid in fruit juice and beverage |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100373152C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102023136A (en) * | 2010-05-21 | 2011-04-20 | 湖北紫鑫生物科技有限公司 | Method for detecting purple sweet potato anthocyanidin pigment by ultraviolet spectrophotometry |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105319169B (en) * | 2014-07-30 | 2018-05-25 | 厦门茶叶进出口有限公司 | A kind of recognition detection method of sugaring black tea |
| CN104655771B (en) * | 2014-08-22 | 2018-11-13 | 谱尼测试集团股份有限公司 | The detection method of Determination of galactooligosacchariin in a kind of measurement formula milk |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0748265A (en) * | 1993-06-03 | 1995-02-21 | Nippon Chem Res Kk | Remitting agent for nephritic syndrome and hepatopathic symptom |
| CN1398630A (en) * | 2002-08-30 | 2003-02-26 | 中国科学院上海有机化学研究所 | Active largehead atractylodes saccharide complex for reducing blood sugar and its prepn and use |
-
2004
- 2004-11-23 CN CNB200410073309XA patent/CN100373152C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0748265A (en) * | 1993-06-03 | 1995-02-21 | Nippon Chem Res Kk | Remitting agent for nephritic syndrome and hepatopathic symptom |
| CN1398630A (en) * | 2002-08-30 | 2003-02-26 | 中国科学院上海有机化学研究所 | Active largehead atractylodes saccharide complex for reducing blood sugar and its prepn and use |
Non-Patent Citations (4)
| Title |
|---|
| 一种改良的糖醛酸含量测定方法. 林颖等.《中草药》药剂与工艺，第30卷第11期. 1999 * |
| 咔唑比色法测定玉米种皮中的果胶含量. 李春明等.中国公共卫生，第20卷第4期. 2004 * |
| 果胶的咔唑硫酸分光光度测定法研究. 张小玲.甘肃农业大学学报，第34卷第1期. 1999 * |
| 离子交换在制糖工业中应用的最新进展（下）. 刘树楷等.中国甜菜糖业，第6期. 1993 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102023136A (en) * | 2010-05-21 | 2011-04-20 | 湖北紫鑫生物科技有限公司 | Method for detecting purple sweet potato anthocyanidin pigment by ultraviolet spectrophotometry |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1664577A (en) | 2005-09-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Mato et al. | A review of the analytical methods to determine organic acids in grape juices and wines | |
| Guo et al. | Simultaneous spectrophotometric determination of trace copper, nickel, and cobalt ions in water samples using solid phase extraction coupled with partial least squares approaches | |
| Ma et al. | Determination of nanomolar levels of nutrients in seawater | |
| US9857348B2 (en) | Method and apparatus for simultaneous online assay of nitrites and nitrates in water samples | |
| CN106053627A (en) | Method for simultaneously detecting 26 organic acids and inorganic negative ions in juice | |
| CN103091273B (en) | Method for rapidly determining starch content of sorghum grains | |
| CN108896504B (en) | Method for simultaneously determining nitrate content of p-nitrophenol and degradation product thereof | |
| Norfun et al. | Reverse flow injection spectrophotometric for determination of aluminium (III) | |
| CN104215731A (en) | Method for distinguishing true apple juice from false apple juice by virtue of liquid chromatogram-isotope ratio mass spectrometry (LC-IRMS) determination | |
| CN104297367B (en) | Device and method for amperometric detection of total cyanide and sulfide of wastewater by online photolysis dialysis/chromatographic separation | |
| Daşbaşı et al. | Synthesis, characterization and application of a new chelating resin for on-line separation, preconcentration and determination of Ag (I) by flame atomic absorption spectrometry | |
| Shahida et al. | Flow injection on-line determination of uranium after preconcentration on XAD-4 resin impregnated with dibenzoylmethane | |
| CN100373152C (en) | Method for measuring galacturonic acid in fruit juice and beverage | |
| de Peña et al. | Continuous flow system for lead determination by FAAS in spirituous beverages with solid phase extraction and on-line copper removal | |
| Liang et al. | Flow injection analysis of nanomolar level orthophosphate in seawater with solid phase enrichment and colorimetric detection | |
| CN103760266A (en) | Method for detecting content of urea in brewed wine by using high performance liquid chromatography | |
| CN102507757A (en) | Method for measuring ascorbic acid content in porphyra yezoensis by high performance liquid chromatography | |
| CN102735639B (en) | Unlabeled-type homogeneous colorimetric method for detecting lead ions | |
| Páscoa et al. | A multi-syringe flow injection system for the spectrophotometric determination of trace levels of iron in waters using a liquid waveguide capillary cell and different chelating resins and reaction chemistries | |
| CN106018386A (en) | Analytical method of antioxidant capacity in tea or tea products | |
| CN113406221B (en) | Method for simultaneously detecting 11 common substances in water body by utilizing ion chromatography | |
| Chen et al. | Determination of total and free sulfite in foods and beverages | |
| Ping et al. | Determination of organic acids exuded from plant roots by high performance liquid chromatography | |
| Asaoka et al. | An online solid phase extraction method for the determination of ultratrace level phosphate in water with a high performance liquid chromatograph | |
| CN114441675A (en) | Pretreatment method and automatic pretreatment device for haloacetic acid detection |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080305 |