CN102507550B - Manufacturing method of food odor visible sensor based on natural pigment - Google Patents
Manufacturing method of food odor visible sensor based on natural pigment Download PDFInfo
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Abstract
The invention discloses a manufacturing method of a food odor visible sensor based on natural pigment. The manufacturing method comprises the steps of: respectively adding 50-95% alcohol solution or 3-7% of citric acid solvent to black rice, azalea, peach flower and purple sweet potato raw materials, soaking in a 60-80 DEG C water bath pan, after obvious fading, filtering and concentrating to obtain four pigment concentrated solutions with water contents of 60-80%, adjusting the pH values of the four pigment solutions to 4, 5, 6, 7, 8 and 10 with water, 0.5-5% citric acid solution and 3-10% sodium bicarbonate solution respectively, detecting with a color difference meter and analyzing the color difference of each pigment under the conditions of different pH values by an LAB color space method, selecting the pigment with obvious AB value changes under the weak acid, neutral and weak basic conditions as a gas sensitive material, finally fixing the gas sensitive material to a substrate flat material, and drying to obtain a visible sensor array. According to the invention, the natural pigment is used as the gas sensitive material, thereby being nontoxic and harmless as well as eliminating the harm to human health.
Description
Technical field
The present invention relates to a kind of method for making of smell visible sensor; Refer in particular to the method for making of natural colouring matter as the food odor visible sensor of gas sensitive material.
Background technology
Food smell is an important indicator of judgement food quality and freshness,, because the most colourless naked eyes of food smell are invisible and easily collecting not, is difficult to carry out qualitative and quantitative analysis.Food smell has Acidity of Aikalinity and volatile usually, therefore can utilize this different characteristic to make the smell visible sensor.Present existing smell visible sensor is, according to the change color before and after specific gas sensitive material and gas reaction to be detected, gas to be measured is carried out qualitative and quantitative analysis.The patent No. is that the gas sensitive material that ZL200710024695.7, name are called in " method for making of color-sensitive gas sensor array " is generally porphyrins and hydrophobic pH indicator, although these gas sensitive materials have higher sensitivity, but because it has chemical toxicity, be not suitable for being directly used in food analysis, more can not with Food Contact.
Natural colouring matter compare with traditional gas sensitive material have advantages of outstanding, cost is extremely low, extracting method is simple, pigment content is large, renewable pollution-free etc., and the natural colouring matter of considerable part has chemical activity, and value of chromatism has obvious variation under different pH value environment, therefore can utilize natural colouring matter to make food odor visible sensor as gas sensitive material.
Summary of the invention
The objective of the invention is not to be suitable for for overcoming traditional gas sensitive material the deficiency of food analysis, propose a kind of
Method for making based on the food odor visible sensor of natural colouring matter, the natural colouring matter of different pH sensitivities is made nontoxic food odor visible sensor as gas sensitive material.
The method for making that the present invention is based on the food odor visible sensor of natural colouring matter is carried out in accordance with the following steps:
(1) extraction of natural colouring matter
The black rice that first will choose, azalea, peach blossom and four kinds of raw materials of purple potato grind after cleaning and drying, the citric acid solvent that adds respectively 50 ~ 95% alcoholic solutions or 3 ~ 7% in every kind of raw material, the mass ratio of every kind of raw material and solvent is 1:10 ~ 1:5, respectively every kind of raw material and solvent were soaked 24 ~ 30 hours in the water-bath of 60 ℃ ~ 80 ℃ again, after obviously fading, raw material filters out extract, then the extract evaporation and concentration being become water percentage is 60% ~ 80% concentrate, obtains respectively black rice pigments, azalea pigment, peach blossom pigment and purple potato pigment;
(2) choose based on the gas sensitive material of colour difference meter analysis
Water, 0.5 ~ 5% citric acid solution and 3 ~ 10% sodium bicarbonate solution transfer to the pH value of black rice pigments, azalea pigment, peach blossom pigment and purple potato pigment respectively the Acidity of Aikalinity of 4,5,6,7,8,10 6 different pH values with the simulated foods smell, use colour difference meter to detect and adopt LAB color space method to analyze the value of chromatism of every kind of pigment under six different pH condition, being chosen at AB value under faintly acid, neutrality, weak basic condition and changing obvious pigment as gas sensitive material;
(3) making of visible sensor
Extract described gas sensitive material with microscale sampler, and described gas sensitive material is fixed on the substrate plate material, obtain the visible sensor array after drying.
Beneficial effect of the present invention: the present invention uses the gas sensitive material of natural colouring matter as the smell visible sensor, nontoxicly can not produce harm to health.For Food Quality and Safety provides a kind of new detection and monitoring method.
Description of drawings
Fig. 1 (a) and Fig. 1 (b) are that when the pork deterioration smell is detected, sensor array of the present invention is listed in the front mirror figure of reaction:
Fig. 2 (a) and Fig. 2 (b) are that when the pork deterioration smell is detected, sensor array of the present invention is listed in reacted mirror figure.
Embodiment
The present invention is take black rice, azalea, peach blossom, purple potato as starting material, use nontoxic extracting method to extract natural colouring matter, analyze these four kinds of pigments situation that value of chromatism changes under faintly acid and weak basic condition based on colour difference meter and select gas sensitive material, finally gas sensitive material solution is fixed on base material and makes the visible sensor array, specifically:
select black rice, azalea, these four kinds of raw materials of peach blossom and purple potato extract natural colouring matter, the black rice that first will choose, azalea, four kinds of raw materials of peach blossom and purple potato grind after cleaning and drying, add respectively the citric acid solution of 50 ~ 95% alcoholic solutions or 3 ~ 7% as solvent in every kind of raw material, the mass ratio of every kind of raw material and solvent is 1:10 ~ 1:5, respectively every kind of raw material and solvent were soaked 24 ~ 30 hours in the water-bath of 60 ℃ ~ 80 ℃ again, after obviously fading, raw material filters out extract with qualitative filter paper, then extract is used the Rotary Evaporators evaporation and concentration, it is 60% ~ 80% concentrate that evaporation and concentration becomes water percentage, obtain respectively black rice pigments, the azalea pigment, peach blossom pigment and purple potato pigment.Wherein the selection of pigment extraction solvent is very important,, due to the gas sensitive material of natural colouring matter as food inspection, so the solvent of extraction pigment should possess natural colouring matter, dissolubility and nontoxic character is preferably arranged therein.These four kinds of pigments all are dissolved in polar solvent, therefore select water, alcohol, citric acid etc. as the solvent that extracts pigment.
To resulting black rice pigments, azalea pigment, peach blossom pigment and purple potato pigment, water, 0.5 ~ 5% citric acid solution and 3 ~ 10% sodium bicarbonate solution transfer to it respectively the pH value of 4,5,6,7,8,10 these six different gradients, with the Acidity of Aikalinity of simulated foods smell.Re-use the aberration that colour difference meter detects each pH value pigment, and analyze respectively the value of chromatism of four kinds of pigments under different pH condition, the color difference analysis method adopts LAB color space method.LAB color space method is the lightness with L value representation color; The red green degree of A value representation, the A value is on the occasion of the red degree of expression, and A value negative value represents green degree; B value representation champac degree: the B value is on the occasion of the yellow degree of expression, and B value negative value represents blue degree.Be chosen at AB value under faintly acid, neutrality, weak basic condition and change obvious pigment as gas sensitive material, complete based on the gas sensitive material of colour difference meter analysis and choose.
Extract gas sensitive material with microscale sampler and be fixed on the substrate plate material, obtain the visible sensor array after drying.The substrate plate material here can be anti-phase C
2Type silica gel plate, titania powder deposition plate, polytetrafluoroethylene or ethene flat board etc. are used for the flat board of the quick material of fixed air body colour.
Below provide 1 embodiment of the present invention further to set forth the present invention.
Embodiment
Adopt following methods to extract black rice pigments, azalea pigment, peach blossom pigment and these four kinds of natural colouring matters of purple potato pigment: 1, black rice pigments leaching process: to use Domestic fruit extractor that black rice is pulverized, cross 40 mesh sieves, accurately take sieve rear black rice sample and 200 milliliter of 80% ethanol water of 20 grams and put into triangular flask, take out after standing 2 hours in the water-bath of 80 ℃.2 azalea pigment leaching process: the azalea petal that will win takes 3 gram petals after cleaning and draining, and with mortar, mashes with 240 milliliter of 80% ethanolic solution and puts into together triangular flask, and lixiviate is 2 hours in 60 ℃ of water-baths.3 peach blossom pigment leaching process: the peach blossom lobe that will pluck, cleaning drains, and take 20 grams and smash to pieces with mortar, and the ethanolic solution of 200 milliliter 80% puts into triangular flask, and lixiviate is 2 hours in 30 ℃ of water-baths.4 purple potato pigment leaching process: get the purple potato of 20g and clean, diced shape is put into tissue refiner and is smashed to pieces, obtains slurries shape solution, measure 20 milliliters of purple potatos with graduated cylinder and smash liquid to pieces, pour in triangular flask, then add the citric acid of 200 milliliter 5%, shake up, be placed in 60 ℃ of thermostat water bath lixiviates 2 hours.After four kinds of raw materials obviously fade, filter out this four kinds of extracts with the qualitative filter paper of diameter 15cm, with the extract evaporation and concentration, being concentrated into water percentage is 60% ~ 80% with Rotary Evaporators, and the pH value without four kinds of pigments regulating the pH value that has just extracted this moment is all in 3 ~ 4 scopes.The black rice pigments that obtains concentrating, peach blossom pigment, azalea pigment and purple potato pigment.
Analyze the character of different pH value pigments with the full-automatic colour examining colour-difference-metre of DC-P3 type: at first use acidometer (model: PHS-3TC, Shanghai) detect the pH value of concentrated rear pigment, citric acid solution with 1% and 5% sodium bicarbonate solution are adjusted to respectively pH=4, pH=5, pH=6, pH=7, pH=8, pH=10 with every kind of pigment, six different target pH values.The current pH value of pigment that records when acidometer adds during greater than target pH value appropriate 1% citric acid solution to be adjusted to target pH value; The current pH value of pigment that records when acidometer adds during less than target pH value appropriate 5% sodium bicarbonate solution to be adjusted to target pH value.After colour difference meter start heat 30min, with the standard white plaque zeroing, adjust to white, pour the solution example of every kind of pigment under six kinds of different pH condition into cuvette in order, successively the value of chromatism of test sample solution.Observation black rice pigments, azalea pigment, peach blossom pigment, purple potato pigment are as follows in the situation of change of pH=4,5,6,7,8,10 o'clock AB values of chromatism: black rice pigments pH value be faintly acid extremely during neutrality value of chromatism in reddish yellow value scope red scale value higher than yellow value degree, show redness, but the yellow value degree of value of chromatism sharply rises over red scale value when the pH value becomes alkalescent by neutrality, shows yellow; The azalea pigment in the pH value value of chromatism that is faintly acid when neutral always in red scale value and yellow value degree scope, show aubergine, yellow value degree sharply rises during to alkalescent by neutrality, and by red scale value, becomes greenness index, be in yellow value degree and greenness index scope, show yellow green; Value of chromatism is all in red scale value and yellow value degree scope under six kinds of pH value conditions for the peach blossom pigment, and the pH value is changed little by faintly acid value of chromatism when neutral, neutral during to alkalescent red scale value and yellow value degree all sharply rise; Purple potato pigment the pH value be faintly acid during to neutrallty condition value of chromatism in red scale value and Lan Du value scope, show royal purple, neutral to value of chromatism under weak basic condition in yellow value degree and greenness index scope, yellow value degree is higher, shows yellow.According to the analysis of colour difference meter, these four kinds of pigments AB value under faintly acid and weak basic condition changes all clearly, so these four kinds of pigments all can be used as gas sensitive material.
, based on these four kinds of results that pigment is drawn by the colour difference meter analysis, with four kinds of gas sensitive material solution that microscale sampler 100mm * 0.8mm kapillary is got under the pH=3 that 1 μ L concentrated ~ 4 solutions of weak acidity, be fixed on two anti-phase C of base material
2On the type silica gel plate, make the visible sensor array after drying.
the visible sensor array of making is detected the rotten smell that produces of pork, as follows to detect the rotten situation of pork: as will to make two duplicate visible sensor arrays at the same terms and do contrast, then fresh pork is placed in beaker, cover to prick on beaker foraminate preservative film again will be wherein visible sensor array be placed on preservative film (be fixed with gas sensitive material one facing to beaker), another piece visible sensor array is placed on the sky beaker does blank (be fixed with gas sensitive material facing to beaker), place and observe the pigment change situation after six days.The sensor array of just having made as 1 figure (a) (b) as shown in, the first row gas sensitive material is followed successively by peach blossom pigment, azalea pigment from left to right; The second row gas sensitive material is followed successively by purple potato pigment, black rice pigments from left to right.Two beakers are placed after six days and observed variation phenomenon in 25 ℃ of closed environments, visible sensor array as shown in Figure 2 (a) shows is to be placed on the phenomenon of sky beaker after upper six day, and the visible sensor array shown in Fig. 2 (b) is to be placed on the phenomenon of beaker after upper six day that pork is housed.Pork muscle after six days is matt, fatty celadon, and appearance is glued hand, and new tangent plane is clamminess, and the depression after finger pressure can not be recovered, and leaves sharp trace, frowziness, meat soup is muddy, and yellow floccus is arranged, and fat seldom floats on surface, and frowziness has belonged to rotten meat.
Fig. 2 (a) compares look quick material color that sensor array lists and changes not quite with Fig. 1 (a), first row is peach blossom pigment yellow green from left to right, azalea pigment lilac; Second row purple potato pigment from left to right is red, the black rice pigments royal purple.Can find out obviously that by Fig. 2 (b) gas sensitive material that is placed on the sensor array on the beaker that pork is housed all has variation in various degree, first row peach blossom pigment from left to right is similar to the brown of white by faint yellow Fig. 2 of becoming (b) of Fig. 1 (b), and the azalea pigment is become and is similar to oyster by lilac; Second row from left to right purple potato by Fig. 1 (b) redness become Fig. 2 (b) approximate with white, it is light yellow that black rice becomes Fig. 2 (b) by Fig. 1 (b) royal purple.These change identical with the variation of pigment AB value under different pH values that colour difference meter records, and illustrate that selecting the method for gas sensitive material based on colour difference meter is that this sensor is feasibility reliably.
Claims (2)
1. method for making based on the food odor visible sensor of natural colouring matter is characterized in that carrying out as follows:
(1) extraction of natural colouring matter
the black rice that first will choose, azalea, four kinds of raw materials of peach blossom and purple potato grind after cleaning and drying, the citric acid solvent that adds respectively 50 ~ 95% alcoholic solutions or 3 ~ 7% in every kind of raw material, the mass ratio of every kind of raw material and solvent is 1:10 ~ 1:5, again respectively with black rice raw material and solvent in the water-bath of 80 ℃ standing 2 hours, with azalea and solvent in 60 ℃ of water-baths standing 2 hours, with peach blossom and solvent in 30 ℃ of water-baths standing 2 hours, with purple potato and solvent in 60 ℃ of water-baths standing 2 hours, after obviously fading, raw material filters out extract, then the extract evaporation and concentration being become water percentage is 60% ~ 80% concentrate, obtain respectively black rice pigments, the azalea pigment, peach blossom pigment and purple potato pigment,
(2) choose based on the gas sensitive material of colour difference meter analysis
Water, 0.5 ~ 5% citric acid solution and 3 ~ 10% sodium bicarbonate solution transfer to the pH value of black rice pigments, azalea pigment, peach blossom pigment and purple potato pigment respectively the Acidity of Aikalinity of 4,5,6,7,8,10 6 different pH values with the simulated foods smell, use colour difference meter to detect and adopt LAB color space method to analyze the value of chromatism of every kind of pigment under six different pH condition, being chosen at AB value under faintly acid, neutrality, weak basic condition and changing obvious pigment as gas sensitive material;
(3) making of visible sensor
Extract described gas sensitive material with microscale sampler, and described gas sensitive material is fixed on the substrate plate material, obtain the visible sensor array after drying.
2. the method for making of a kind of food odor visible sensor based on natural colouring matter according to claim 1, it is characterized in that: described substrate plate material is anti-phase C
2Type silica gel plate, titania powder deposition plate, polytetrafluoroethylene or ethene are dull and stereotyped.
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