CN103983733A - Method for detecting biogenic amine in yellow wine by using chromatographic sheet - Google Patents
Method for detecting biogenic amine in yellow wine by using chromatographic sheet Download PDFInfo
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Abstract
The invention discloses a method for detecting biogenic amine in yellow wine by using a chromatographic sheet, belonging to the technical field of analysis and detection of components in the yellow wine. The method comprises the steps of carrying out derivation on a biogenic amine standard substance and a to-be-tested yellow wine sample by using a derivatization reagent, enriching the biogenic amine by using liquid-liquid extraction, carrying out sample application on a sheet plate, arranging the sheet plate in a saturate tank loaded with a certain proportion of developing solvent and unfolding; developing and observing under an ultraviolet lamp, and qualitatively detecting the target biogenic amine; and finally, quantitatively measuring the biogenic amine in the yellow wine by using a thin layer chromatograph. According to the method, the detection limit range of the biogenic amine is 0.5-5 mug/mL, the average adding standard recovery rate is 88.5-110.3 percent, the standard deviation is 3.8-12.5 percent, and at most 13 samples can be simultaneously detected on a 20*20 thin layer glass plate. Compared with other analysis methods, the method has the advantages that qualitative and quantitative analysis of the biogenic amine in the yellow wine can be realized, the operation is simple and convenient, the cost is low, and a plurality of samples can be simultaneously detected.
Description
Technical field
The present invention relates to a kind of method that uses chromatographic sheet to detect biogenic amine in yellow rice wine, especially a kind of method that uses the contamination of biogenic amine in thin-layered chromatography qualitative and quantitative analysis yellow rice wine, belongs to yellow rice wine constituent analysis detection technique field.
Background technology
Yellow rice wine is the distinctive fermented wine of China, can be rated as east and brewages the Typical Representative on boundary.But its sweat is complicated and be difficult to control, therefore in yellow rice wine wine liquid, contain abundant and complicated composition, comprise moisture, ethanol, carbohydrate, organic acid, nitrogen-containing compound, total solid, non-volatile ester, volatile ingredient (comprising alcohol, acid, ester, hydroxyl compound), organic principle etc.The amino acid kind wherein containing is up to 18 kinds, and total content is that a times of other wine kinds (beer, grape wine, white wine) amino acid content is to several times.Amino acid can be formed by microbial metabolism the potential objectionable constituent such as biogenic amine, and the security of yellow rice wine is under suspicion.Biogenic amine (especially histamine) in yellow rice wine more and more receives consumer, manufacturer and researcher's concern, and the monitoring of therefore strengthening biogenic amine in yellow rice wine is significant to improving yellow rice wine quality and security.
Some researchs have been confirmed to have biogenic amine in the yellow rice wine from different regions, and the contamination of biogenic amine in yellow rice wine have been carried out detecting and analyzed.At present, the biogenic amine in yellow rice wine is mainly to detect by high performance liquid chromatography.Although high performance liquid chromatography technology is accurate, sensitive, not only costliness but also time-consuming, and once can only complete the detection of a kind of sample, can not meet high flux in actual production, cheap, easy, testing requirement fast far away.On the basis of original analyzing detecting method, need the method that a kind of expense of invention is low, simple to operate, can realize multiple sample detection simultaneously badly.
Thin-layered chromatography (thin-layer chromatography, TLC) is a kind of simple, semiquantitative method based on vision hot spot power, does not need heavy type or expensive equipment, and allows multiple samples to analyze simultaneously.The present invention has successfully analyzed the biogenic amine in yellow rice wine first application of thin layer chromatography quantitative and qualitative analysis, and accuracy and accuracy to method verify, shows that the method is a determination method that effectively substitutes HPLC.
Summary of the invention
The object of the invention is to be to provide a kind of method that uses chromatographic sheet to detect biogenic amine in yellow rice wine, especially a kind of method of using biogenic amine contamination in thin-layered chromatography qualitative and quantitative analysis yellow rice wine.Owing to lacking chromophoric group in biogenic amine molecule, itself not only without uv absorption, but also without fluorescence and electrochemical activity, make the separation of different kind organism amine and measure very difficult, so the inventive method utilizes derivatization reagent to derive the biogenic amine in yellow rice wine sample, make it bring luminophore, then point sample on thin-layer chromatography silica gel plate, with a certain proportion of developping agent expansion, thereby can be under ultraviolet or fluorescent light qualitative detection, adopt thin-layer chromatography analyzer to carry out quantitatively corresponding biogenic amine.
Technical scheme of the present invention mainly comprises the following steps:
(1) take the hydrochloric acid constant volume of appropriate biogenic amine mark product 0.1mol/L, make mother liquor for subsequent use; Taking appropriate dansyl Cl is dissolved in acetone to be prepared into the derivatization reagent of 1-10mg/mL for subsequent use;
Described biogenic amine comprises cadaverine, histamine, tyrasamine, spermidine, spermine, putrescine, tryptamines etc.;
(2) preparation of the biogenic amine standard solution of variable concentrations: 10-400 μ g/mL tyrasamine, spermidine standard solution; 5.0-200 μ g/mL spermine standard solution; 20-800 μ g/mL histamine, putrescine standard solution; 40-1000 μ g/mL cadaverine standard solution;
(3) derivative: to get respectively and isopyknicly treat that derivatives solution and yellow rice wine sample, in different plastic centrifuge tubes, add the saturated NaHCO of certain volume in each centrifuge tube
3solution makes it to be alkalescence, then adds the derivatization reagent of 1-5 times of sample solution volume, and on vortex mixer, vortex mixes, and is placed in dark thermostat water bath derivative, takes out; At room temperature place after a few minutes, add the saturated NaCl solution of 1/2 sample solution volume, then add and the isopyknic organic solvent extraction of sample solution, after layering, get upper organic phase point sample on thin-layer silicon offset plate; Described derivative temperature is 25 DEG C～60 DEG C, and the derivative time is 10～60min;
(4) point sample, separation: derive the separation of sample on silica gel thin-layer glass plate, sample starts point sample, at least 15mm of the distance between sample from the bottom 10mm apart from plate;
(5) launch: before analyzing, chromatography cylinder need to be saturated with developping agent potpourri, then the silica gel thin-layer glass plate after point sample is placed in to the thin layer chamber that developping agent is housed and launches, potpourri is raised to about 19cm from the bottom of dish to be stopped, and is dried;
(6) colour developing: develop the color under uviol lamp, compare with hybrid standard sample, the biogenic amine kind in qualitative analysis yellow rice wine sample.
(7) quantitative test: adopt thin layer chromatograph under 254nm condition, chromatosheet to be scanned, per sample in spot corresponding peak area quantification calculate in yellow rice wine the total amount of biogenic amine in each Content of Biogenic Amines and yellow rice wine.
The preferred isohexane of organic extractant, ether, ethyl acetate etc. in described step (3).
In described step (3), adding saturated alkaline solution is to allow derive under alkali condition carry out, and is more conducive to derivatization reaction and makes luminophore effective detectability that reduces this detection method on biogenic amine band.The object that adds saturated salt solution in step (3) is in order to improve sensitivity, promotes that biogenic amine enters organic phase, makes extraction efficiency the best.
The preferred development rate of developping agent ratio in described step (5) is the fastest, duration of run is the shortest, the ratio of expansion best results.
The developping agent chloroform that preferably 2:1～6:1 mixes by volume in described step (5): the chloroform that triethylamine or by volume 2:1:1～6:4:1 mixes: ether: triethylamine, optimal proportion is determined according to the separating effect of the length of duration of run, biogenic amine; Duration of run is 1～2h preferably.
The present invention improves classic method, has optimized pre-treating method, the ratio of derivative reagent, the derivatization conditions of sample, the ratio of biogenic amine extractant and developping agent.These modifications can be shortened detection time to greatest extent, thereby realize fast detecting.The inventive method is a kind of easy, high-throughout analytical approach, the linearity of typical curve is good, detecting lower range is 0.5 μ g/mL-5 μ g/mL, average recovery of standard addition 88.5%-110.3%, standard deviation is 3.8%-12.5%, and the method can be measured 13 yellow rice wine samples in 1-2h simultaneously.With the normally used analytical approach of modern measure biogenic amine in food: high performance liquid chromatography is compared with capillary electrophoresis, the present invention is without expensive analytical instrument, and expense is low, easy and simple to handle, quick, the qualitative and quantitative of biogenic amine in yellow rice wine is measured, can effectively be reduced testing cost.
Brief description of the drawings
Fig. 1: the biogenic amine mixed standard solution thin-layer chromatogram of variable concentrations; In figure, each well biogenic amine concentration is respectively from left to right: 80,40,20,10,5.0,2.0,1.0,0.5 μ g/mL
Fig. 2: the tyrasamine standard solution thin-layer chromatogram of variable concentrations; In figure, each well tyrasamine concentration is respectively from left to right: 10,20,40,80,160,320 μ g/mL
Fig. 3: the tyrasamine standard solution thin-layer chromatography typical curve of variable concentrations
Fig. 4: the histamine standard solution thin-layer chromatogram of variable concentrations; In figure, each well histamine concentration is respectively from left to right: 20,40,80,160,320,640 μ g/mL
Fig. 5: the histamine standard solution thin-layer chromatography typical curve of variable concentrations
Fig. 6: the spermidine standard solution thin-layer chromatogram of variable concentrations; In figure, each well spermidine concentration is respectively from left to right: 10,20,40,80,160,320 μ g/mL
Fig. 7: the spermidine standard solution thin-layer chromatography typical curve of variable concentrations
Fig. 8: the cadaverine standard solution thin-layer chromatogram of variable concentrations; In figure, each well cadaverine concentration is respectively from left to right: 40,80,160,320,640,1000 μ g/mL
Fig. 9: the cadaverine standard solution thin-layer chromatography typical curve of variable concentrations
Figure 10: the putrescine standard solution thin-layer chromatogram of variable concentrations; In figure, each well putrescine concentration is respectively from left to right: 20,40,80,160,320,640 μ g/mL
Figure 11: the putrescine standard solution thin-layer chromatography canonical plotting of variable concentrations
Figure 12: the thin-layer chromatogram of biogenic amine in different production phase yellow rice wine; In figure, each well sample production phase of living in is respectively from left to right: rice dipping the 2nd day, rice dipping the 3rd day, front ferment the 1st day, front ferment the 2nd day, front ferment the 3rd day, hybrid standard product, rear ferment the 5th day, rear ferment the 10th day, former wine, precipitation wine, hybrid standard product
Figure 13: the thin-layer chromatogram of biogenic amine in different year yellow rice wine sample; In figure, the time of each well sample is respectively from left to right: 2014,2013,2012,2011,2010,2009,2004,1988
Embodiment
Below in conjunction with concrete example, the present invention is described in further detail.
The method for making of embodiment 1 variable concentrations standard solution typical curve
Thin-layered chromatography is made the typical curve of different biogenic amines, comprises the following steps:
(1) preparation of the biogenic amine standard solution of variable concentrations: 10-400 μ g/mL tyrasamine, spermidine standard solution; 5.0-200 μ g/mL spermine standard solution; 20-800 μ g/mL histamine, putrescine standard solution; 40-1000 μ g/mL cadaverine standard solution.Get respectively the standard solution of variable concentrations in different plastic centrifuge tubes, first add and the isopyknic saturated NaHCO of standard solution
3solution makes it to be alkalescence, add again the dansyl Cl derivative solution (1-10mg/mL acetone) of 1-5 times of standard solution volume, on vortex mixer, vortex mixes after 1min, be placed in respectively after the derivative 10-60min time of dark 30 DEG C of-60 DEG C of thermostat water baths, take out, at room temperature place after a few minutes, add the saturated NaCl solution of 1/2 standard solution volume, add again and the volume organic solvent extraction of standard solution etc., after layering, get upper organic phase point sample on silica gel glass plate by sample introduction needle;
(2) on silica gel thin glass plate, derive the separation of sample, sample starts point sample from the bottom 10mm apart from plate, and distance between aliquot need to be at least 15mm;
(3) before analyzing, chromatography cylinder need to be saturated with developping agent potpourri, and developping agent potpourri is: the chloroform of 2:1-6:1 (V/V): triethylamine.Then silica gel thin glass plate is placed in to chromatography cylinder and launches, potpourri is raised to certain altitude (the about 17.5cm of bulk migration) from the bottom of dish, and silica gel thin glass plate is dry in fuming cupboard;
(4) colour developing: develop the color under the ultraviolet light of gel electrophoresis analysis imaging system, find the spot of biogenic amine colour developing in variable concentrations list standard solution.
(5) quantitative: to adopt thin layer chromatogram scanner under 254nm condition, chromatosheet to be scanned, obtain the peak value of biogenic amine colour developing spot in variable concentrations list standard solution, the content that the peak value of each spot is corresponding certain, thus the typical curve of each standard items can directly be obtained.
Embodiment 2 detects the biogenic amine in yellow rice wine sample derivative at different derivative temperature
The different biogenic amines that derive in yellow rice wine sample derivative at temperature of thin-layered chromatography qualitative and quantitative analysis, comprise the following steps:
(1) get respectively yellow rice wine sample in different plastic centrifuge tubes, first add and the isopyknic saturated NaHCO of yellow rice wine sample solution
3solution makes it to be alkalescence, add again the dansyl Cl derivative solution (1-10mg/mL acetone) of 1-5 times of sample solution volume, on vortex mixer, vortex mixes after 1min, be placed in respectively dark normal temperature, after the derivative 30min times of 35 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C thermostat water baths, take out, at room temperature place after a few minutes, add the saturated NaCl solution of 1/2 sample solution volume, add again and the volume organic solvent extraction of sample solution etc., after layering, get upper organic phase point sample on silica gel glass plate by sample introduction needle;
(2) on silica gel thin glass plate, derive the separation of sample, the distance that sample starts between point sample and aliquot from the bottom 10mm apart from plate need to be at least 15mm;
(3) before analyzing, chromatography cylinder need to be saturated with developping agent potpourri, and developping agent potpourri is the chloroform of 2:1-6:1 (V/V): triethylamine.Then silica gel thin glass plate is placed in to chromatography cylinder and launches, potpourri is raised to certain altitude (the about 17.5cm of bulk migration) from the bottom of dish, and silica gel thin glass plate is dry in fuming cupboard;
(4) colour developing: develop the color under the ultraviolet light of gel electrophoresis analysis imaging system, find the spot of target organism amine colour developing in yellow rice wine sample, the kind of biogenic amine in qualitative analysis yellow rice wine sample.
(5) quantitative: to adopt thin layer chromatogram scanner under 254nm condition, chromatosheet to be scanned, obtain at different derivative temperature the peak value of each biogenic amine spot in yellow rice wine sample, carry it into the typical curve of different biogenic amines, can calculate at different derivative temperature the content of each biogenic amine and the total amount of biogenic amine in yellow rice wine sample.
(6) sum up: according to interpretation, derivative temperature is 60 DEG C of the bests, at this temperature, the highest Content of Biogenic Amines can be detected.
Biogenic amine after the 3 different derivative times of detection of embodiment in yellow rice wine
By the method for biogenic amine in yellow rice wine after the derivative different time of thin-layered chromatography detection, comprise the following steps:
(1) the yellow rice wine sample of getting respectively variable concentrations, in different plastic centrifuge tubes, first adds and the isopyknic saturated NaHCO of yellow rice wine sample solution
3solution makes it to be alkalescence, add again the dansyl Cl derivative solution (1-10mg/mL acetone) of 1-5 times of sample solution volume, on vortex mixer, vortex mixes after 1min, being placed in respectively dark 60 DEG C of thermostat water baths derives respectively after 10min, 20min, 30min, 40min, 50min, 60min, take out, at room temperature place after a few minutes, add the saturated NaCl solution of 1/2 sample solution volume, add again and the volume organic solvent extraction of sample solution etc., after layering, get upper organic phase point sample on silica gel glass plate by sample introduction needle;
(2) on silica gel thin glass plate, derive the separation of sample, the distance that sample starts between point sample and aliquot from the bottom 10mm apart from plate need to be at least 15mm;
(3) before analyzing, chromatography cylinder need to be saturated with developping agent potpourri, and developping agent potpourri is the chloroform of 4:1 (V/V): triethylamine.Then silica gel thin glass plate is placed in to chromatography cylinder and launches, potpourri is raised to certain altitude (the about 17.5cm of bulk migration) from the bottom of dish, and silica gel thin glass plate is dry in fuming cupboard;
(4) colour developing: develop the color under the ultraviolet light of gel electrophoresis analysis imaging system, find the spot of target organism amine colour developing in yellow rice wine sample, the kind of biogenic amine in qualitative analysis yellow rice wine sample.
(5) quantitative: to adopt thin layer chromatogram scanner under 254nm condition, chromatosheet to be scanned, obtain under the different derivative time peak value of each biogenic amine spot in yellow rice wine sample, carry it into the typical curve of different biogenic amines, can calculate under the different derivative time content of each biogenic amine and the total amount of biogenic amine in yellow rice wine sample.
(6) sum up: according to interpretation, the derivative time is 30min the best, under this time, the highest Content of Biogenic Amines can be detected.
Embodiment 4 detects different proportion developping agent and launches the biogenic amine in rear yellow rice wine
Detect different proportion developping agent by thin-layered chromatography and launch the method for biogenic amine in rear yellow rice wine, comprise the following steps:
(1) the yellow rice wine sample of getting respectively variable concentrations, in different plastic centrifuge tubes, first adds and the isopyknic saturated NaHCO of sample solution
3solution makes it to be alkalescence, add again the dansyl Cl derivative solution (1-10mg/mL acetone) of 1-5 times of sample solution volume, on vortex mixer, vortex mixes after 1min, be placed in respectively after the derivative 10-60min time of dark 30 DEG C of-60 DEG C of thermostat water baths, take out, at room temperature place after a few minutes, add the saturated NaCl solution of 1/2 sample solution volume, add again and the volume organic solvent extraction of sample solution etc., after layering, get upper organic phase point sample on silica gel glass plate by sample introduction needle;
(2) on silica gel thin glass plate, derive the separation of sample, the distance that sample starts between point sample and aliquot from the bottom 10mm apart from plate need to be at least 15mm;
(3) before analyzing, chromatography cylinder need to be saturated with developping agent potpourri, and developping agent potpourri is respectively the chloroform of 2:1 (V/V): the chloroform of triethylamine, 6:1:1: ether: the chloroform of triethylamine and 6:1 (V/V): triethylamine.Then silica gel thin glass plate is placed in to chromatography cylinder and launches, potpourri is raised to certain altitude (the about 17.5cm of bulk migration) from the bottom of dish, and silica gel thin glass plate is dry in fuming cupboard;
(4) colour developing: develop the color under the ultraviolet light of gel electrophoresis analysis imaging system, find the spot of target organism amine colour developing in yellow rice wine sample, the kind of biogenic amine in qualitative analysis yellow rice wine sample.
(5) quantitative: to adopt thin layer chromatogram scanner under 254nm condition, chromatosheet to be scanned, obtain the peak value that different proportion developping agent launches each biogenic amine spot in rear yellow rice wine sample, carry it into the typical curve of different biogenic amines, can calculate different proportion developping agent and launch the content of each biogenic amine and the total amount of biogenic amine in rear yellow rice wine sample.
(6) sum up: according to interpretation, the chloroform of 6:1 (V/V): the best results that triethylamine launches can detect the highest Content of Biogenic Amines under the condition of this ratio developping agent.
Although the present invention with preferred embodiment openly as above; but it is not in order to limit the present invention, any person skilled in the art, without departing from the spirit and scope of the present invention; all can do various changes and modification, therefore protection scope of the present invention should be with being as the criterion that claims were defined.
Claims (8)
1. a method that uses chromatographic sheet to detect biogenic amine in yellow rice wine, it is characterized in that, be to utilize derivatization reagent to carry out derivatization treatment to the biogenic amine in yellow rice wine sample, make it bring luminophore, then adopt thin-layer chromatography analyzer to analyze biogenic amine.
2. method according to claim 1, is characterized in that, described derivatization is that yellow rice wine sample is placed in to centrifuge tube, then adds saturated NaHCO in centrifuge tube
3solution makes it to be alkalescence, add again derivatization reagent, on vortex mixer, vortex mixes, derivative under dark constant temperature, then take out and at room temperature place after a few minutes, add the saturated NaCl solution of 1/2 sample solution volume, then add and the isopyknic organic solvent extraction of sample solution, after layering, get upper organic phase for analyzing; Described derivatization reagent is dansyl Cl, is dissolved in acetone, and concentration is 1～10mg/mL, and consumption is 1-5 times of sample solution volume, and derivative temperature is 25 DEG C～60 DEG C, and the derivative time is 10min～60min.
3. method according to claim 1, is characterized in that, described biogenic amine comprises cadaverine, histamine, tyrasamine, spermidine, spermine, putrescine, tryptamines.
4. method according to claim 1 and 2, it is characterized in that, while adopting thin-layer chromatography analyzer to analyze biogenic amine, developping agent is the chloroform that 2:1～6:1 mixes by volume: the chloroform that triethylamine or by volume 2:1:1～6:4:1 mixes: ether: triethylamine.
5. method according to claim 1 and 2, is characterized in that, mainly comprises the following steps:
(1) derivative: to get respectively and a certain amount ofly treat that derivatives solution or yellow rice wine sample, in plastic centrifuge tube, add the saturated NaHCO of certain volume in each centrifuge tube
3solution makes it to be alkalescence, then adds the derivatization reagent of 1-5 times of sample solution volume, and on vortex mixer, vortex mixes, and is placed in dark 25 DEG C～60 DEG C derivative 10min～60min, takes out; At room temperature place after a few minutes, add the saturated NaCl solution of 1/2 sample solution volume, then add and the isopyknic organic solvent extraction of sample solution, after layering, get upper organic phase point sample on thin-layer silicon offset plate;
(2) point sample, separation: derive the separation of sample on silica gel thin-layer glass plate, sample starts point sample, at least 15mm of the distance between sample from the bottom 10mm apart from plate;
(3) launch: before analyzing, chromatography cylinder need to be saturated with developping agent potpourri, then the silica gel thin-layer glass plate after point sample is placed in to the thin layer chamber that developping agent is housed and launches, potpourri is raised to about 19cm from the bottom of dish to be stopped, and is dried;
(4) colour developing: develop the color under uviol lamp, compare with hybrid standard sample, the biogenic amine kind in qualitative analysis yellow rice wine sample.
(5) quantitative test: adopt thin layer chromatograph under 254nm condition, chromatosheet to be scanned, per sample in spot corresponding peak area quantification calculate in yellow rice wine the total amount of biogenic amine in each Content of Biogenic Amines and yellow rice wine.
6. method according to claim 5, is characterized in that, in described step (1), organic solvent is isohexane, ether or ethyl acetate.
7. method according to claim 5, is characterized in that, in described step (3), developping agent is the chloroform that 2:1～6:1 mixes by volume: the chloroform that triethylamine or by volume 2:1:1～6:4:1 mixes: ether: triethylamine.
8. method according to claim 5, is characterized in that, in described step (3), duration of run is 1～2h.
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Cited By (4)
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| CN104792915A (en) * | 2015-04-08 | 2015-07-22 | 广州浩意万医药科技有限公司 | Method for determining nystose content of morinda officinalis roots |
| CN106706834A (en) * | 2016-11-18 | 2017-05-24 | 江南大学 | Method for rapidly detecting multiple biogenic amines in dairy product by virtue of combination of high performance thin layer chromatography and adjustable surface enhanced raman spectroscopy |
| CN107290452A (en) * | 2017-06-23 | 2017-10-24 | 江南大学 | A kind of method for detecting reference state heterocycle amine content |
| CN109358151A (en) * | 2018-12-19 | 2019-02-19 | 广东盛泰华生物制药有限公司 | The thin-layered chromatography detection method of 1,4- butanediamine impurity in a kind of L-Arginine raw material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104792915A (en) * | 2015-04-08 | 2015-07-22 | 广州浩意万医药科技有限公司 | Method for determining nystose content of morinda officinalis roots |
| CN106706834A (en) * | 2016-11-18 | 2017-05-24 | 江南大学 | Method for rapidly detecting multiple biogenic amines in dairy product by virtue of combination of high performance thin layer chromatography and adjustable surface enhanced raman spectroscopy |
| CN107290452A (en) * | 2017-06-23 | 2017-10-24 | 江南大学 | A kind of method for detecting reference state heterocycle amine content |
| CN109358151A (en) * | 2018-12-19 | 2019-02-19 | 广东盛泰华生物制药有限公司 | The thin-layered chromatography detection method of 1,4- butanediamine impurity in a kind of L-Arginine raw material |
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