CN103604803A - Method for rapidly detecting content of iron ion in red wine - Google Patents
Method for rapidly detecting content of iron ion in red wine Download PDFInfo
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- CN103604803A CN103604803A CN201310557025.7A CN201310557025A CN103604803A CN 103604803 A CN103604803 A CN 103604803A CN 201310557025 A CN201310557025 A CN 201310557025A CN 103604803 A CN103604803 A CN 103604803A
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- Prior art keywords
- iron ion
- compound
- red wine
- ion content
- nitrogen
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 33
- 235000020095 red wine Nutrition 0.000 title claims abstract description 28
- 239000003381 stabilizer Substances 0.000 claims abstract description 18
- 239000011347 resin Substances 0.000 claims abstract description 11
- 229920005989 resin Polymers 0.000 claims abstract description 11
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 9
- -1 iron ion Chemical class 0.000 claims description 47
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 14
- 229910001447 ferric ion Inorganic materials 0.000 claims description 14
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 claims description 10
- 239000003002 pH adjusting agent Substances 0.000 claims description 9
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000003463 adsorbent Substances 0.000 claims description 7
- 159000000013 aluminium salts Chemical class 0.000 claims description 7
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 7
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 6
- 238000004440 column chromatography Methods 0.000 claims description 6
- RLFWWDJHLFCNIJ-UHFFFAOYSA-N 4-aminoantipyrine Chemical compound CN1C(C)=C(N)C(=O)N1C1=CC=CC=C1 RLFWWDJHLFCNIJ-UHFFFAOYSA-N 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 4
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 4
- 235000010489 acacia gum Nutrition 0.000 claims description 4
- 239000001785 acacia senegal l. willd gum Substances 0.000 claims description 4
- PQLAYKMGZDUDLQ-UHFFFAOYSA-K aluminium bromide Chemical compound Br[Al](Br)Br PQLAYKMGZDUDLQ-UHFFFAOYSA-K 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 229960005070 ascorbic acid Drugs 0.000 claims description 4
- HKOOXMFOFWEVGF-UHFFFAOYSA-N phenylhydrazine Chemical compound NNC1=CC=CC=C1 HKOOXMFOFWEVGF-UHFFFAOYSA-N 0.000 claims description 4
- 229940067157 phenylhydrazine Drugs 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 108010010803 Gelatin Proteins 0.000 claims description 3
- 239000012539 chromatography resin Substances 0.000 claims description 3
- 239000008273 gelatin Substances 0.000 claims description 3
- 229920000159 gelatin Polymers 0.000 claims description 3
- 235000019322 gelatine Nutrition 0.000 claims description 3
- 235000011852 gelatine desserts Nutrition 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 2
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 claims description 2
- ALYNCZNDIQEVRV-UHFFFAOYSA-N 4-aminobenzoic acid Chemical compound NC1=CC=C(C(O)=O)C=C1 ALYNCZNDIQEVRV-UHFFFAOYSA-N 0.000 claims description 2
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 2
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 claims description 2
- WVVOBOZHTQJXPB-UHFFFAOYSA-N N-anilino-N-nitronitramide Chemical compound [N+](=O)([O-])N(NC1=CC=CC=C1)[N+](=O)[O-] WVVOBOZHTQJXPB-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 239000001164 aluminium sulphate Substances 0.000 claims description 2
- 235000011128 aluminium sulphate Nutrition 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 229960004050 aminobenzoic acid Drugs 0.000 claims description 2
- RWZYAGGXGHYGMB-UHFFFAOYSA-N anthranilic acid Chemical compound NC1=CC=CC=C1C(O)=O RWZYAGGXGHYGMB-UHFFFAOYSA-N 0.000 claims description 2
- KXDHJXZQYSOELW-UHFFFAOYSA-N carbonic acid monoamide Natural products NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 2
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 150000002240 furans Chemical class 0.000 claims description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 claims description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 2
- 150000003233 pyrroles Chemical class 0.000 claims description 2
- 239000000741 silica gel Substances 0.000 claims description 2
- 229910002027 silica gel Inorganic materials 0.000 claims description 2
- 235000010413 sodium alginate Nutrition 0.000 claims description 2
- 239000000661 sodium alginate Substances 0.000 claims description 2
- 229940005550 sodium alginate Drugs 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 229930192474 thiophene Natural products 0.000 claims description 2
- KJAMZCVTJDTESW-UHFFFAOYSA-N tiracizine Chemical compound C1CC2=CC=CC=C2N(C(=O)CN(C)C)C2=CC(NC(=O)OCC)=CC=C21 KJAMZCVTJDTESW-UHFFFAOYSA-N 0.000 claims description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 12
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 abstract description 2
- 238000005457 optimization Methods 0.000 abstract 1
- 238000004381 surface treatment Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- 238000013016 damping Methods 0.000 description 8
- 239000012530 fluid Substances 0.000 description 8
- 235000014101 wine Nutrition 0.000 description 8
- 241000219095 Vitis Species 0.000 description 7
- 235000009754 Vitis X bourquina Nutrition 0.000 description 7
- 235000012333 Vitis X labruscana Nutrition 0.000 description 7
- 235000014787 Vitis vinifera Nutrition 0.000 description 7
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 4
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000004737 colorimetric analysis Methods 0.000 description 3
- TYQCGQRIZGCHNB-JLAZNSOCSA-N l-ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(O)=C(O)C1=O TYQCGQRIZGCHNB-JLAZNSOCSA-N 0.000 description 3
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 235000018553 tannin Nutrition 0.000 description 2
- 239000001648 tannin Substances 0.000 description 2
- 229920001864 tannin Polymers 0.000 description 2
- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 description 1
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 1
- VEQOALNAAJBPNY-UHFFFAOYSA-N antipyrine Chemical compound CN1C(C)=CC(=O)N1C1=CC=CC=C1 VEQOALNAAJBPNY-UHFFFAOYSA-N 0.000 description 1
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012916 chromogenic reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000003712 decolorant Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 235000019990 fruit wine Nutrition 0.000 description 1
- 210000002216 heart Anatomy 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 150000004698 iron complex Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 210000000496 pancreas Anatomy 0.000 description 1
- 238000004816 paper chromatography Methods 0.000 description 1
- 229960005222 phenazone Drugs 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000012372 quality testing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 238000004809 thin layer chromatography Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
本发明提供一种快速检测红酒中铁离子含量的方法，取待检样品加入稳定剂混合后再加入显色剂，层析观察铁离子显色带，根据铁离子显色带长度计算铁离子含量。本发明通过在待检样品中加入稳定剂，解决了现有技术中显色剂与红酒作用会生成沉淀，导致铁离子含量检测结果不准确甚至无法检测的问题；通过优选和表面处理，使树脂选择性吸附铁与显色剂所显示的红色，而不吸附红酒自身的颜色，因此检测前无需对红酒进行脱色处理；且本方法所采用试剂及设备简单，检测成本低廉；检测周期短，可快速得到检测结果，可广泛应用于现场快速检测。The invention provides a method for quickly detecting the iron ion content in red wine. The sample to be tested is mixed with a stabilizer and then added with a color developer, the iron ion color band is observed by chromatography, and the iron ion content is calculated according to the length of the iron ion color band. The present invention solves the problem in the prior art that the reaction between the color developer and the red wine will generate precipitation by adding a stabilizer to the sample to be tested, resulting in inaccurate or even undetectable iron ion content detection results; through optimization and surface treatment, the resin It selectively adsorbs the red color displayed by iron and chromogen, but does not adsorb the color of red wine itself, so there is no need to decolorize red wine before detection; and the reagents and equipment used in this method are simple, and the detection cost is low; the detection cycle is short and can be The detection results can be obtained quickly, and can be widely used in on-site rapid detection.
Description
Technical field
The present invention relates to a kind of method of fast detecting iron ion content, specifically a kind of method of iron ion content in fast detecting red wine.
Background technology
In recent years, from the report of each quality testing department, can see, have in a large number underproof grape wine on market, wherein to exceed standard be one of subject matter to iron ion content.The content overproof of iron not only can affect mouthfeel, makes product occur precipitation, also accelerates oxidation vinous and the process that decays, and causes the qualities such as color vinous that large change occurs, and directly has influence on quality vinous.In addition human body excess intake or wrongly take excessive iron element and also may cause iron poisoning, produces infringement to the heart, liver and pancreas, affects healthy.In order to guarantee that quality vinous must be carried out deironing and iron content detects, the mandatory national standards GB15037 < < of People's Republic of China (PRC) grape wine > > stipulates iron content :≤8.0mg/L.
OIV's (International office of vine and wine is called for short OIV) has issued iron content examination criteria method in grape wine, adopts atomic absorption spectrography (AAS).This standard or World Trade Organization (WTO) be accepted standard aspect grape wine.China standard GB/T/T15038-2006 < < grape wine fruit wine universaling analysis method > > adopts respectively atomic absorption spectrophotometry, o-phenanthroline colourimetry and sulfosalicylic acid colourimetry.On the one hand, adopt instrument to detect, need to buy expensive instrument and equipment, conventional instrument and equipment has Atomic Absorption Spectrometer (AAS), icp ms (ICP-MS) etc. now, needs technical professional to operate simultaneously; On the other hand, while adopting colorimetric determination, conventional colorimetric determination utilizes exactly divalence or ferric ion and developer complexing to generate red complex and detects, and claret itself is exactly red, cannot demonstrate the color of iron complex at all, cannot directly carry out colorimetric detection, therefore two kinds of colourimetrys all need grape wine sample to carry out pre-treatment, Wet or dry method digestion, two kinds of equal complex steps of method, reagent dosage is large, consuming time longer; Moreover, no matter adopting which kind of method, normal sense cycle all needs more than 3 days, cannot meet the needs of fast detecting.
Document " conventional iron ion content exploration of analysis method " (Cheng Fangting etc., Treatment of Industrial Water, 2007,27,61-63) sum up the method for several fast detecting ferric ions, mainly contained sulfosalicylia acid spectrophotometry, Phen photometry and EDTA complexometry etc.Wherein, EDTA complexometry selectivity is not strong, may cause testing result seriously higher.Other method be all by chromogenic reagent and the reacted change color of ferric ion and standard color comparison card to recently judging the iron content in solution, for on-the site analysis, operate cumbersomely, and colorimetric resultant error is larger.In addition, because shown color mostly is red or orange after above-mentioned developer reacts with ferric ion, be difficult to distinguish with the color of orange, red liquid itself, so need to first decolour, then develop the color again, decolorization unavoidably can cause the loss of part ferric ion, and testing result error is large.The more important thing is, for red wine, owing to wherein containing a large amount of tannin class, phenols, alcohols and letones, complicated chemical reaction can occur after developer adds in red wine and produce deposit, cause colorimetric failure, can not accurately detect.
Summary of the invention
Technical matters to be solved by this invention is to provide the method for iron ion content in a kind of fast detecting red wine, to solve above-mentioned deficiency of the prior art, improves accuracy of detection, shortens sense cycle, reduces testing cost.
The scheme that the present invention solves the problems of the technologies described above is to provide the method for iron ion content in a kind of fast detecting red wine, comprise the following steps: (1) is got sample to be checked and added stabilizing agent to obtain mixed liquor I, described stabilizing agent comprises EDTA, pH adjusting agent, aluminium salt, nitrogen-containing compound, jelling agent; Described nitrogen-containing compound is selected from hydrazine class compound, contains amino-compound, amino-contained compound or nitrogen-containing heterocycle compound; (2) in described mixed liquor I, add developer to obtain mixed liquor I I; (3) will after the I of mixed liquor I described in step 2 colour developing, carry out chromatography, observe ferric ion colour developing band, according to ferric ion colour developing strip length, calculate iron ion content.
As a further improvement on the present invention, described chromatography is polymeric adsorbent column chromatography, and described polymeric adsorbent column chromatography resin used is the selective adsorption resin of grain diameter 1-100 micron.
The method of iron ion content in fast detecting red wine provided by the present invention, by add stabilizing agent in sample to be checked, solving in prior art developer and red wine does the used time and can generate and precipitate with the substance reaction such as tannin class, phenols, alcohols and ketone in red wine, cause the inaccurate problem that even cannot detect of iron ion content testing result, effectively improved testing result accuracy; After ferric ion colour developing, be adsorbed onto the fixing color in mutually of chromatography and red wine and carry color and can obviously distinguish by naked eyes, not needing decolorant is observable; Reagent that this method adopts and equipment are simple, do not need the high experimental facilitiess such as Atomic Absorption Spectrometer, and testing cost is cheap; This method sense cycle is short, can obtain fast testing result, can be widely used in field quick detection.
Accompanying drawing explanation
Fig. 1 is iron ion content working curve diagram.
Embodiment
In order to make technical matters to be solved by this invention, technical scheme and beneficial effect clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The method of iron ion content in fast detecting red wine of the present invention, comprises the following steps: (1) is got sample to be checked and added stabilizing agent to obtain mixed liquor I, and described stabilizing agent comprises EDTA, pH adjusting agent, aluminium salt, nitrogen-containing compound, jelling agent; Described nitrogen-containing compound is selected from hydrazine class compound, contains amino-compound, amino-contained compound or nitrogen-containing heterocycle compound; (2) in described mixed liquor I, add developer to obtain mixed liquor I I; (3) will after the I of mixed liquor I described in step 2 colour developing, carry out chromatography, observe ferric ion colour developing band, according to ferric ion colour developing strip length, calculate iron ion content.
Preferably, described chromatography is polymeric adsorbent column chromatography, and described polymeric adsorbent column chromatography resin used is the selective adsorption resin of grain diameter 1-100 micron.
Preferably, stabilizing agent comprises 0.005g/L-50g/L EDTA, 0.005g/L-100g/L aluminium salt, 0.005g/L-50g/L nitrogen-containing compound, 0.005g/L-50g/L jelling agent and pH adjusting agent.Wherein aluminium salt is selected from least one in aluminium bromide, aluminium sulphate, aluminum chloride, aluminium nitrate, aluminum fluoride; Hydrazine class compound is selected from least one in the alkyl derivative, phenylhydrazine, paranitrophenylhydrazine, dinitrophenylhydrazine of hydrazine, hydrazine; Containing amino/amine compound, be selected from fatty amine and the homologs thereof such as carbamic acid, carbamate and homolog thereof, aminobenzoic acid, anthranilate and homolog thereof, ethylenediamine and homolog thereof, amino-antipyrine and homolog thereof, methylamine, ethamine, propylamine, comprise monoamine, diamine, tertiary amine simultaneously; Described nitrogen-containing heterocycle compound is selected from the double heteroatoms heterogeneous ring compounds such as single heteroatoms heterogeneous ring compound such as pyrroles, furans, thiophene or azole.Jelling agent is selected from least one of Arabic gum, sodium alginate, sucrose fatty acid ester, gelatin, silica gel, polyvinylpyrrolidone.
Preferably, developer is 0.005g/L-50g/L Phen, 0.005g/L-50g/L vitamin c and damping fluid or 0.005g/L-50g/L thiocyanate, 0.005g/L-50g/L persulfate and pH adjusting agent.The pH value adjustable damping fluid of pH adjusting agent for coexisting with other materials arbitrarily, as the mixed solution of weak acid and salt thereof (HAc and NaAc), the mixed solution (NH of weak base and salt thereof
3h
2o and NH
4cl), the pH value of developer is 1-13, and preferably pH value is 6-8.
Preferably, also can will add in the sample impouring polymeric adsorbent chromatographic column to be checked of described stabilizing agent and developer, observe ferric ion colour developing band, according to colour developing strip length, calculate iron ion content in red wine.Described iron ion content height is linear positive correlation with variable color strip length, and national standard is limited the quantity of as 8ppm to the highest of ferric ion in grape wine, and the present invention has measured the working curve of the corresponding variable color strip length of 1-12ppm iron ion content c l relation, as shown in Figure 1.
More preferably, choose known iron concentration and be 8ppm red wine sample according to the present invention operation steps, according to test result, on resin column, delimit acceptance line.Whether the iron ion content that the method can detect red wine sample quickly and efficiently meets national standard restriction, has widespread use and is worth.
Similarly, the method of the invention can be different according to selected chromatography method, further optimize and have paper chromatography fast detection method, thin-layer chromatography detection method etc., described method all can be delimited acceptance line according to national standard, prepare corresponding device for fast detecting, be applied to field quick detection, there is widespread use value and great economy and be worth.
By a plurality of embodiment, the present invention is described further below, wherein red wine sample is stochastic buying gained on the market, is labeled as sample A, sample B, sample C.
S11: the preparation of stabilizing agent
Get EDTA0.25mg, aluminium nitrate 5mg, phenylhydrazine 5mg, Arabic gum 25mg join in the damping fluid of 5mL, regulate pH=7.0;
S12: the preparation of developer
Get Phen 1mg, vitamin c 0.5mg and join in the damping fluid of 5mL, regulate pH=7.0;
S13: iron ion content detects
Get 5mL red wine sample to be measured A, add wherein the stabilizing agent of S11 preparation gained, add the developer of S12 preparation gained after shaking up again, after shaking up, add resin column, measure the length of resin column variable color part, this length is directly proportional to iron content.Through contrasting with working curve, the iron ion content obtaining in red wine sample A is 2.5ppm.
S21: the preparation of stabilizing agent
Get EDTA15mg, aluminium nitrate 30mg, antipyrine 5mg, Arabic gum 30mg join in the damping fluid of 3mL, regulate pH=6.0;
S22: the preparation of developer
Get Phen 1mg, vitamin c 0.5mg and join in the damping fluid of 3mL, regulate pH=6.0;
S23: iron ion content detects
Get 5mL red wine sample to be measured B, add wherein the stabilizing agent of S21 preparation gained, add the developer of S22 preparation gained after shaking up again, after shaking up, add resin column, measure the length of resin column variable color part, this length is directly proportional to iron content.Through contrasting with working curve, the iron ion content obtaining in red wine sample B is 6.2ppm.
S31: the preparation of stabilizing agent
Get EDTA15mg, aluminium nitrate 30mg, phenylhydrazine 30mg, ethylenediamine 30mg, gelatin 30mg joins in the damping fluid of 3mL, regulates pH=8;
S32: the preparation of developer
Get potassium rhodanide 30mg, potassium persulfate 30mg and join in the damping fluid of 3mL, regulate pH=8;
S33: iron ion content detects
Get 5mL red wine sample to be measured B, add wherein the stabilizing agent of S31 preparation gained, add the developer of S32 preparation gained after shaking up again, after shaking up, add resin column, measure the length of resin column variable color part, this length is directly proportional to iron content.Through contrasting with working curve, the iron ion content obtaining in red wine sample B is 10.9ppm.
Comparative example 1 testing result accuracy comparison
Get red wine sample A, B, the C censorship identical with embodiment, censorship test result is respectively: 2.4ppm, 6.3ppm, 10.8ppm.To sum up, testing result deviation of the present invention is less than 3%, meets the actual needs that detect completely.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a method for iron ion content in fast detecting red wine, comprises the following steps: (1) is got sample to be checked and added stabilizing agent to obtain mixed liquor I, and described stabilizing agent comprises EDTA, pH adjusting agent, aluminium salt, nitrogen-containing compound, jelling agent; Described nitrogen-containing compound is selected from hydrazine class compound, contains amino-compound, amino-contained compound or nitrogen-containing heterocycle compound; (2) in described mixed liquor I, add developer to obtain mixed liquor I I; (3) will after the I of mixed liquor I described in step 2 colour developing, carry out chromatography, observe ferric ion colour developing band, according to ferric ion colour developing strip length, calculate iron ion content.
2. method according to claim 1, is characterized in that, described chromatography is polymeric adsorbent column chromatography, and described polymeric adsorbent column chromatography resin used is the selective adsorption resin of grain diameter 1-100 micron.
3. method according to claim 1, is characterized in that, described stabilizing agent comprises 0.005g/L-50g/LEDTA, 0.005g/L-100g/L aluminium salt, 0.005g/L-50g/L nitrogen-containing compound, 0.005g/L-50g/L jelling agent and pH adjusting agent.
4. method according to claim 1, is characterized in that, described developer is 0.005g/L-50g/L Phen, 0.005g/L-50g/L vitamin c and pH adjusting agent, and pH value is 6-8.
5. method according to claim 1, is characterized in that, described developer is 0.005g/L-50g/L thiocyanate, 0.005g/L-50g/L persulfate and pH adjusting agent, and pH value is 6-8.
6. method according to claim 1, is characterized in that, described aluminium salt is selected from least one in aluminium bromide, aluminium sulphate, aluminum chloride, aluminium nitrate, aluminum fluoride.
7. according to the method described in any one in claims 1 to 3, it is characterized in that, described hydrazine class compound is selected from least one in the alkyl derivative, phenylhydrazine, paranitrophenylhydrazine, dinitrophenylhydrazine of hydrazine, hydrazine.
8. according to the method described in any one in claims 1 to 3, it is characterized in that, the described amino/amine compound that contains is selected from carbamic acid, carbamate and homolog thereof, aminobenzoic acid, anthranilate and homolog thereof, ethylenediamine and homolog thereof, amino-antipyrine and homolog thereof, fatty amine and homolog thereof.
9. according to the method described in any one in claims 1 to 3, it is characterized in that, described nitrogen-containing heterocycle compound is selected from pyrroles, furans, thiophene, azole.
10. according to the method described in any one in claims 1 to 3, it is characterized in that, described jelling agent is selected from least one of Arabic gum, sodium alginate, sucrose fatty acid ester, gelatin, silica gel, polyvinylpyrrolidone, and the total concentration of described jelling agent is controlled at 0.005g/L-50g/L.
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| CN110865075A (en) * | 2019-12-31 | 2020-03-06 | 南通大学 | Conventional urinary iron detection kit and detection method thereof |
| CN112014386A (en) * | 2020-08-14 | 2020-12-01 | 湘潭华辰仪器有限公司 | Method for detecting content of trace iron in quartz sand |
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