CN105973880A - Ready-to-use test paper for rapid assessment of content of aluminum elements in food, and use method and application thereof - Google Patents
Ready-to-use test paper for rapid assessment of content of aluminum elements in food, and use method and application thereof Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention relates to ready-to-use test paper for rapid assessment of the content of aluminum elements in food, wherein the test paper comprises the following preparation steps: preparing a 1% sulfuric acid solution; preparing an acetic acid-sodium acetate solution; preparing a 3% acetic acid solution; preparing a hexadecyl trimethylamine bromide solution; preparing a chrome azurol S solution; preparing developing test paper; preparing a standard colorimetric card; and obtaining the ready-to-use test paper. The test paper is used for detecting the content of aluminum based on a chrome azurol S method; a condition that aluminum is subjected to a reaction with chrome azurol S in the presence of hexadecyl trimethylamine bromide to become blue in the pH range of 6.7-7.0 is mainly utilized, and colorimetric quantitation is carried out; the test paper can rapidly accurately determine the content of aluminum in the food, better ensures consumer physical safety, improves the accuracy of safety indicators for detection of the food, strengthens the food market supervision, and has important significance; and at the same time, the test paper has the advantages of small size, portability, convenience in detection, low cost, and easy popularization.
Description
Technical field
The invention belongs to technical field of food safety detection, the instant reagent paper of a kind of rapid evaluation aluminum in food constituent content and using method thereof and application.
Background technology
Aluminum and compound thereof the most generally exist, and are the metallic elements that in the earth's crust, content is most, be widely used in daily life and production owing to it has excellent physicochemical property, aluminum and correlated product thereof, thus the aluminum exposure in crowd is inevitable.Epidemiological studies is it is demonstrated experimentally that the aluminum of long-time excess intake causes obvious function of nervous system to sexually revise, and affects intelligent development；When 5-10 times of aluminum content during aluminum content exceedes general meals in food, so that it may cause osteomalacia and fracture, thus make skeletogenous damage and deformation, there is the disease such as osteomalacia, osteoporosis.In addition, substantial amounts of scientific experiments research finds, the aluminum of long-time excess intake all produces chronic murder by poisoning to human reproductive systems, hemopoietic system, immune system, liver, lung, kidney, bone, heart etc., but people the most usually ignore existence and the chronic toxicity thereof of aluminum.According to calculating, an individual weight be the adult of 55kg weekly such as consumption 255g fritters of twisted dough, its meals aluminum intake just exceedes and tentative can tolerate weekly intake (PTWI).So measuring aluminum content to be accurately and rapidly to ensure that the important prerequisite of consumer safety.
Therefore, develop the reagent paper of a kind of rapid and accurate determination Aluminum Content in Food, for better ensuring that the physical safety of consumer, the safety index of detection food, reinforcement food products market are supervised significant.
The detection method of current existing aluminum has a lot, such as: spectrophotography, GFAAS, mass spectrography, inductive coupling plasma emission spectrum method etc., they mostly need expensive instrument and operate complexity, special technical staff, and detection cycle length, costly, it is impossible to realize Site Detection and universal.And reagent paper inspection technology has the features such as reagent paper volume little, Portable belt, easy to detect, low cost, it is a kind of detection food and detection method of Aluminium in Drinking Water content quickly and accurately can being applied in everyday home life.
By retrieval, find following two patent publication us relevant to present patent application:
1, aluminium ion Test paper and preparation method thereof and using method (CN103499574A), this Test paper uses filter paper to take out after infiltrating in impregnation liquid, dried prepared, described impregnation liquid includes that chrome azurol S 0.1-0.6 gram dissolves in 100 milliliters of distilled water, and uniform mixed preparing impregnation liquid I and 0.5 gram of ascorbic acid and Phen 2 grams dissolve in the impregnation liquid II of uniform mixed preparing in 100 milliliters of distilled water successively；This Test paper is with chrome azurol S as developer, coordinate and mixed homogeneously the activator use being configured to by 0.2mol/L disodium phosphate soln 12.64mL and 0.1mol/L citric acid solution 7.37mL, make simple, with low cost, easy to use, free from environmental pollution, environmental；Test scope is wide, operate without professional, is particularly well-suited to rapid field detection aluminum content.
2, a kind of reagent paper for aluminum content detection and its preparation method and application (CN103913455A), described reagent paper, including carrier and developer, described carrier has water absorption, described developer is adsorbed almost uniformly on the carrier, and described developer is chrome azurol S.Described reagent paper uses simple immersion process to prepare, can be used for the quick detection of aluminum content, there is advantage quick, sensitive, easy and simple to handle, with low cost, and operate without professional, it is particularly suited in edible jelly fungi illegally adding the quick detection of aluminum phosphate, it is easy to the common people use the most voluntarily, it is possible to for food safety, the detection the most in real time in market.
By contrast, there are the different of essence from above-mentioned patent publication us in present patent application.
Summary of the invention
In place of it is an object of the invention to overcome the deficiencies in the prior art, the instant reagent paper of a kind of rapid evaluation aluminum in food constituent content and using method thereof and application are provided, when using the detection that this reagent paper carries out Aluminum Content in Food, sample handling characteristics mensuration simple and efficient, efficient, with low cost, test result accurately, be easy to popularize, this reagent paper can be widely applied to the detection of Aluminum Content in Food.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of instant reagent paper of rapid evaluation aluminum in food constituent content, making step is as follows:
(1) prepare the sulfuric acid solution of 1%: draw 1mol/L sulphuric acid dilute with water, until the percentage by volume that addition sulphuric acid accounts for overall solution volume is 1-3%, obtain the sulfuric acid solution of 1%；
(2) prepare ethyl sodium solution: weighing the sodium acetate mass concentration to sodium acetate soluble in water is 0.075～0.076g/mL, it is subsequently adding glacial acetic acid, adjusting pH to 5-5.5, the mass concentration being then diluted with water to sodium acetate is 0.068g/mL, obtains ethyl sodium solution；
Described sodium acetate: ratio g:mL of glacial acetic acid is 17:1.3-1.5；
(3) prepare 3% acetic acid solution: drawing the percentage by volume that glacial acetic acid is slowly added in ultra-pure water to glacial acetic acid is 3%, then mixes, obtains 3% acetic acid solution；
(4) prepare cetrimonium bronmide solution: weighing cetrimonium bronmide and being diluted with water to the concentration of cetrimonium bronmide is 0.2-0.25g/L, obtains cetrimonium bronmide solution；
(5) prepare chrome azurol S solution: weighing chrome azurol S and being diluted with water to the concentration of chrome azurol S is 0.5-0.6g/L, obtains chrome azurol S solution；
(6) develop the color the making of reagent paper: the sulfuric acid solution by 1%, ethyl sodium solution, 3% acetic acid solution, cetrimonium bronmide solution, chrome azurol S solution are mixed and made into soak according to the ratio that volume ratio is 1:5:1:1:1, reagent paper carrier is cut into length takes advantage of the rectangle of a width of 4.5-5.5cm × 0.8-1.2cm to soak 3-5 hour in soak, 50 DEG C of vacuum constant temperatures are dried 4h, preserve, obtain colour developing reagent paper；
Described reagent paper carrier is chromatography filter paper；
(7) the making of standard color comparison card: dripped by the aluminum standard solution of variable concentrations on colour developing reagent paper, after chromogenic reaction occurs 1-3 minute, uses color difference meter to take color, makes standard color comparison card；
The most i.e. obtain instant reagent paper.
And, making step is as follows:
(1) prepare the sulfuric acid solution of 1%: draw 1mol/L sulphuric acid dilute with water, until the percentage by volume that addition sulphuric acid accounts for overall solution volume is 1%, obtain the sulfuric acid solution of 1%；
(2) prepare ethyl sodium solution: weighing the sodium acetate mass concentration to sodium acetate soluble in water is 0.075～0.076g/mL, it is subsequently adding glacial acetic acid, adjusting pH to 5.5, the mass concentration being then diluted with water to sodium acetate is 0.068g/mL, obtains ethyl sodium solution；
Described sodium acetate: ratio g:mL of glacial acetic acid is 17:1.3；
(3) prepare 3% acetic acid solution: drawing the percentage by volume that glacial acetic acid is slowly added in ultra-pure water to glacial acetic acid is 3%, then mixes, obtains 3% acetic acid solution；
(4) prepare cetrimonium bronmide solution: weighing cetrimonium bronmide and being diluted with water to the concentration of cetrimonium bronmide is 0.2g/L, obtains cetrimonium bronmide solution；
(5) prepare chrome azurol S solution: weighing chrome azurol S and being diluted with water to the concentration of chrome azurol S is 0.5g/L, obtains chrome azurol S solution；
(6) develop the color the making of reagent paper: the sulfuric acid solution by 1%, ethyl sodium solution, 3% acetic acid solution, cetrimonium bronmide solution, chrome azurol S solution are mixed and made into soak according to the ratio that volume ratio is 1:5:1:1:1, reagent paper carrier is cut into length takes advantage of the rectangle of a width of 5cm × 1cm to soak in soak 4 hours, 50 DEG C of vacuum constant temperatures are dried 4h, preserve, obtain colour developing reagent paper；
Described reagent paper carrier is chromatography filter paper；
(7) the making of standard color comparison card: the aluminum standard solution of variable concentrations 0.25g/L, 0.5g/L, 1g/L, 2g/L, 4g/L is dripped on colour developing reagent paper, after chromogenic reaction occurs 1 minute, use color difference meter to take color, make standard color comparison card；
The most i.e. obtain instant reagent paper.
And, the optimization method of the described step (5) concentration of middle chrome azurol S is as follows:
Based on chrome azurol S compound concentration in GB GB/T5009.182 2003, in addition to the 0.5g/L concentration of national regulations, also separately design the chrome azurol S concentration of 0.25g/L, 1g/L, 2g/L and 4g/L, selected the suitableeest chrome azurol S concentration according to perusal readability, obtain 0.5g/L；
Or, the optimization method of described step (6) pilot scale paper carrier is as follows:
A4 paper, common quantitative filter paper and chromatography filter paper is used to make by the manufacture method of instant reagent paper as reagent paper carrier, and aluminum standard solution is dripped on reagent paper carrier, observe the colour developing area on each reagent paper carrier and color developing effect, and select the suitableeest reagent paper carrier, i.e. chromatography filter paper；
Or, the optimization method of the described step (6) drying mode of middle colour developing reagent paper is as follows:
Select natural drying, freeze-day with constant temperature and vacuum constant temperature to be dried three kinds of drying modes, determine optimum drying condition, i.e. 50 DEG C, 4h of vacuum drying from the flatness of dried paper, color and miscellaneous speckle situation；
Or, the optimization method of described step (7) middle observation testing result time is as follows:
Drip on reagent paper with aluminum standard solution, observe different time colour developing situation of reagent paper after 0.5-60 minute, after determining that optimal viewing testing result time, i.e. chromogenic reaction occurs 1 minute.
The using method of the instant reagent paper of rapid evaluation aluminum in food constituent content as above, step is as follows:
Being added to the water after being shredded by food, ratio g:mL of food and water is 1:5-12, adds the acetic acid that percentage by volume is 3%, and described food is 1:1-3 with ratio g:mL of acetic acid；Take soak after heating 1-60 minute with water-bath 30-60 DEG C and drop on display reagent paper, observing response district color, and contrast with standard color comparison card, realize the detection to aluminum content according to the depth of color.
And, the detection method of described aluminum in food constituent content is as follows:
Being added to the water after being shredded by food, ratio g:mL of food and water is 1:9, adds the acetic acid that percentage by volume is 3%, and described food is 1:1 with ratio g:mL of acetic acid；Take soak after soaking heating 30-50 minute with water-bath 40 DEG C and drop on display reagent paper, observing response district color, and contrast with standard color comparison card, realizing the detection to aluminum content according to the depth of color, the most qualified regulation according to national standard of aluminium element content in the food of detection judges.
And, the condition optimizing of described food pre-treatment is as follows:
Food is divided into 8 groups, ratio g:mL being separately added into food and acetic acid is 0, the ethanol that percentage by volume is 3% of 10:1,5:1,2:1,1:1,1:4,1:8,1:10, selecting the suitableeest 3% acetic acid addition, instant food is 1:1 with ratio g:mL of acetic acid；
To add the food of the suitableeest 3% acetic acid addition, heat 1-60 minute with water-bath 25-100 DEG C, at different temperatures 25-100 DEG C, sampling detection, observes the leaching content of its aluminum, selects the water-bath soaking temperature of the suitableeest food, be 40 DEG C；
Food heated at constant temperature under the water-bath soaking temperature of the suitableeest food of the suitableeest 3% acetic acid addition will be added, in different time sampling detection in 1-60 minute, observe the aluminum leaching content of sample, select the heat time heating time of the suitableeest food, be 30 minutes.
The application in Rapid determination of aluminum in food content of the instant reagent paper of rapid evaluation aluminum in food constituent content as above.
And, described food is Rhopilema esculenta or fritters of twisted dough.
The present invention obtain advantage and good effect be:
1, reagent paper of the present invention detects aluminum content method based on chrome azurol S method, mainly utilize in the range of PH6.7～7.0, aluminum reacts with chrome azurol S in the presence of bromohexadecane base trimethylamine, au bleu, carry out colorimetric assay, this reagent paper focuses on the method for a kind of simple and efficient detection aluminum content of exploitation, this reagent paper can aluminum content in rapid and accurate determination food, better assure that the physical safety of consumer, improve the accuracy of the safety index of detection food, strengthen food products market supervision, significant, simultaneously, it is little that this reagent paper has volume, Portable belt, easy to detect, low cost, it is easy to the advantage popularized.
2, reagent paper of the present invention uses in preparation process and draws the percentage by volume that glacial acetic acid is slowly added in ultra-pure water to glacial acetic acid is 3%, mixing, in order to simulate white vinegar common in daily life, achieve the real-time monitoring to food materials aluminum content under home environment, extremely easy to use, improve the range of this reagent paper.
3, the reagent paper after reagent paper of the present invention will soak in preparation process uses vacuum drying drying mode to compare and natural drying and hot air drying, and reagent paper surfacing corrugationless, without obvious locus coeruleus, impurity effect is little, achieves unforeseeable technique effect.
4, the method for reagent paper of the present invention assessment aluminum in food constituent content is simple to operate, need not heavy-duty machines and professional, the operation of can testing the most completely of costliness, reduce testing cost, improve the convenience of detection, be very easy to detection.
5, reagent paper of the present invention makes the detection of Aluminum Content in Food compared with conventional method with the pre-treating method of detected food, more quick, and there is the recovery of standard addition (94.6%-105.8%) of preferable minimum quantitative limit (0.5mg/L), aluminum in soak is detected and with ICP-MS method result, there is the higher goodness of fit, equation after two kinds of method detected value linear fits is: Y=1.0159x-0.0724, R2=0.9624.
Accompanying drawing explanation
Fig. 1 be in the present invention different reagent paper carriers to aluminum solutions reaction solution situation map；
Fig. 2 is different chromogenic agents and Al in the present invention3+Solution reaction colour developing situation map；
Fig. 3 is the colour developing situation map of different developing times in the present invention；
When Fig. 4 is detection paper in the present invention, the different acid adding amounts of food affect figure to leaching content；
When Fig. 5 is detection paper in the present invention, the different heating soaking temperature of food affects figure to leaching content；
When Fig. 6 is detection paper in the present invention, the different heating soak time of food affects figure to leaching rate；
Fig. 7 is Plays colorimetric card pattern of the present invention；
Fig. 8 is soak detection paper result and the Linear Fit Chart of ICP-MS testing result in the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described；Following embodiment is illustrative, is not determinate, it is impossible to limit protection scope of the present invention with following embodiment.
Raw material used in the present invention, if no special instructions, is the commercially available prod of routine；Method used in the present invention, if no special instructions, is the conventional method of this area.
Embodiment 1
A kind of instant reagent paper of rapid evaluation aluminum in food constituent content, making step is as follows:
(1) prepare the sulfuric acid solution of 1%: draw 1mol/L sulphuric acid dilute with water, until the percentage by volume that addition sulphuric acid accounts for overall solution volume is 1-3%, obtain the sulfuric acid solution of 1%；
(2) prepare ethyl sodium solution: weighing the sodium acetate mass concentration to sodium acetate soluble in water is 0.075～0.076g/mL, it is subsequently adding glacial acetic acid, adjusting pH to 5-5.5, the mass concentration being then diluted with water to sodium acetate is 0.068g/mL, obtains ethyl sodium solution；
Described sodium acetate: ratio g:mL of glacial acetic acid is 17:1.3-1.5；
(3) prepare 3% acetic acid solution: drawing the percentage by volume that glacial acetic acid is slowly added in ultra-pure water to glacial acetic acid is 3%, then mixes, obtains 3% acetic acid solution；
(4) prepare cetrimonium bronmide solution: weighing cetrimonium bronmide and being diluted with water to the concentration of cetrimonium bronmide is 0.2-0.25g/L, obtains cetrimonium bronmide solution；
(5) prepare chrome azurol S solution: weighing chrome azurol S and being diluted with water to the concentration of chrome azurol S is 0.5-0.6g/L, obtains chrome azurol S solution；
(6) develop the color the making of reagent paper: the sulfuric acid solution by 1%, ethyl sodium solution, 3% acetic acid solution, cetrimonium bronmide solution, chrome azurol S solution are mixed and made into soak according to the ratio that volume ratio is 1:5:1:1:1, reagent paper carrier is cut into length takes advantage of the rectangle of a width of 4.5-5.5cm × 0.8-1.2cm to soak 3-4 hour in soak, 50 DEG C of vacuum constant temperatures are dried 4h, preserve, obtain colour developing reagent paper；
Described reagent paper carrier is chromatography filter paper；
(7) the making of standard color comparison card: dripped by the aluminum standard solution of variable concentrations on colour developing reagent paper, after chromogenic reaction occurs 1-3 minute, uses color difference meter to take color, makes standard color comparison card；
The most i.e. obtain instant reagent paper.
More preferably, the instant reagent paper of above-mentioned rapid evaluation aluminum in food constituent content, making step is as follows:
(1) prepare the sulfuric acid solution of 1%: draw 1mol/L sulphuric acid dilute with water, until the percentage by volume that addition sulphuric acid accounts for overall solution volume is 1%, obtain the sulfuric acid solution of 1%；
(2) prepare ethyl sodium solution: weighing the sodium acetate mass concentration to sodium acetate soluble in water is 0.075～0.076g/mL, it is subsequently adding glacial acetic acid, adjusting pH to 5.5, the mass concentration being then diluted with water to sodium acetate is 0.068g/mL, obtains ethyl sodium solution；
Described sodium acetate: ratio g:mL of glacial acetic acid is 17:1.3；
(3) prepare 3% acetic acid solution: drawing the percentage by volume that glacial acetic acid is slowly added in ultra-pure water to glacial acetic acid is 3%, then mixes, obtains 3% acetic acid solution；
(4) prepare cetrimonium bronmide solution: weighing cetrimonium bronmide and being diluted with water to the concentration of cetrimonium bronmide is 0.2g/L, obtains cetrimonium bronmide solution；
(5) prepare chrome azurol S solution: weighing chrome azurol S and being diluted with water to the concentration of chrome azurol S is 0.5g/L, obtains chrome azurol S solution；
(6) develop the color the making of reagent paper: the sulfuric acid solution by 1%, ethyl sodium solution, 3% acetic acid solution, cetrimonium bronmide solution, chrome azurol S solution are mixed and made into soak according to the ratio that volume ratio is 1:5:1:1:1, reagent paper carrier is cut into length takes advantage of the rectangle of a width of 5cm × 1cm to soak in soak 4 hours, 50 DEG C of vacuum constant temperatures are dried 4h, preserve, obtain colour developing reagent paper；
Described reagent paper carrier is chromatography filter paper；
(7) the making of standard color comparison card: dripped by the aluminum standard solution of variable concentrations 0.25g/L, 0.5g/L, 1g/L, 2g/L, 4g/L on colour developing reagent paper, after chromogenic reaction occurs 1 minute, uses color difference meter to take color, makes standard color comparison card；
The most i.e. obtain instant reagent paper.
The optimization method of the described step (5) concentration of middle chrome azurol S can be such that
Based on chrome azurol S compound concentration in GB GB/T5009.182 2003, sensitivity in view of the color being visually observed is low, test strips and air contact can make Some Drugs aoxidize and the factors such as inefficacy, in addition to the 0.5g/L concentration of national regulations, also separately design the chrome azurol S concentration of 0.25g/L, 1g/L, 2g/L and 4g/L, select the suitableeest chrome azurol S concentration according to perusal readability, obtain 0.5g/L；
Or, the optimization method of described step (6) pilot scale paper carrier is as follows:
A4 paper, common quantitative filter paper and chromatography filter paper is used to make by the manufacture method of instant reagent paper as reagent paper carrier, and aluminum standard solution is dripped on reagent paper carrier, observe the colour developing area on each reagent paper carrier and color developing effect, and select the suitableeest reagent paper carrier, i.e. chromatography filter paper；
Or, the optimization method of the described step (6) drying mode of middle colour developing reagent paper is as follows:
Selecting natural drying, freeze-day with constant temperature and vacuum constant temperature to be dried three kinds of drying modes, different drying modes is shown in Table 1, determines optimum drying condition, i.e. 50 DEG C, 4h of vacuum drying from the flatness of dried paper, color and miscellaneous speckle situation；
Or, the optimization method of described step (7) middle observation testing result time is as follows:
Drip on reagent paper with aluminum standard solution, observe the colour developing situation of 0.5-60 minute reagent paper of different time, determine the optimal viewing testing result time, after i.e. chromogenic reaction occurs 1 minute.
The using method of the instant reagent paper of rapid evaluation aluminum in food constituent content as above, step is as follows:
Being added to the water after being shredded by food, ratio g:mL of food and water is 1:5-12, adds the acetic acid that percentage by volume is 3%, and described food is 1:1-3 with ratio g:mL of acetic acid；Take soak after heating 1-60 minute with water-bath 30-60 DEG C and drop on display reagent paper, observing response district color, and contrast with standard color comparison card, realize the detection to aluminum content according to the depth of color.
Further, the detection method of described aluminum in food constituent content is as follows:
Being added to the water after being shredded by food, ratio g:mL of food and water is 1:9, adds the acetic acid that percentage by volume is 3%, and described food is 1:1 with ratio g:mL of acetic acid；Take soak after soaking heating 30-50 minute with water-bath 40 DEG C and drop on display reagent paper, observing response district color, and contrast with standard color comparison card, realizing the detection to aluminum content according to the depth of color, the most qualified regulation according to national standard of aluminium element content in the food of detection judges.
Further, the condition optimizing of described food pre-treatment is as follows: food is divided into 8 groups, ratio g:mL being separately added into food and acetic acid is 0, the ethanol that percentage by volume is 3% of 10:1,5:1,2:1,1:1,1:4,1:8,1:10, selecting the suitableeest 3% acetic acid addition, instant food is 1:1 with ratio g:mL of acetic acid；
To add the food of the suitableeest 3% acetic acid addition, heat 30 minutes with water-bath 25-100 DEG C, at different temperatures 25-100 DEG C, sampling detection, observes the leaching content of its aluminum, selects the water-bath soaking temperature of the suitableeest food, be 40 DEG C；
Food heated at constant temperature under the water-bath soaking temperature of the suitableeest food of the suitableeest 3% acetic acid addition will be added, in different time 1-60 minute sampling detection, observe the aluminum leaching content of sample, select the heat time heating time of the suitableeest food, i.e. 30 minutes.
The instant reagent paper of above-mentioned rapid evaluation aluminum in food constituent content can be applied in Rapid determination of aluminum in food content, such as, apply the detection of aluminum content in Rhopilema esculenta or fritters of twisted dough.
Embodiment 2
A kind of instant reagent paper of rapid evaluation aluminum in food constituent content, making step is as follows:
One, the preparation of early stage solution
1, the sulfuric acid solution of 1%: draw 1mL1mol/L sulphuric acid and be diluted with water to 100mL scale.
2, ethyl sodium solution: weigh 34g sodium acetate and be dissolved in 450mL water, adds 2.6mL glacial acetic acid, adjusts pH to 5.5, is diluted with water to 500mL.
3,3% acetic acid solution: draw 3mL glacial acetic acid and be slowly added in 97mL ultra-pure water, mix (in order to simulate white vinegar common in daily life).
4, cetrimonium bronmide solution: weigh 20mg cetrimonium bronmide and be diluted with water to 100mL scale, this solution 0.2g/L.
5, chrome azurol S solution: weigh 50mg chrome azurol S and be diluted with water to 100mL scale, this solution 0.5g/L.
Two, the manufacturing conditions optimization of reagent paper
Selected reagent paper carrier is cut into the long rectangle taking advantage of a width of 5cm × 1cm, through being dried after soaking in reaction solution, and preserves.
The optimization method of described reagent paper carrier is as follows:
A4 paper, common quantitative filter paper and chromatography filter paper is used to make by the manufacture method of instant reagent paper as reagent paper carrier, and aluminum standard solution is dripped on reagent paper carrier, observe the colour developing area on each reagent paper carrier and color developing effect, and select the suitableeest reagent paper carrier, i.e. chromatography filter paper, result is shown in Fig. 1, with A4 paper, common quantitative filter paper and chromatography filter paper and the Al3+ solution reaction of variable concentrations.From the point of view of colour developing situation, chromatography filter paper makes the aluminum color range of variable concentrations more apparent, and the diffusion of A4 paper reactant liquor is uneven and to inhale dose few, and dose inhaled by common quantitative filter paper and chromatography filter paper is very nearly the same, but gradient color developing effect relatively chromatography filter paper is poor；
The optimization method of the concentration of described chrome azurol S is as follows:
Based on chrome azurol S compound concentration in GB GB/T5009.182 2003, sensitivity in view of the color being visually observed is low, test strips and air contact can make Some Drugs aoxidize and the factors such as inefficacy, therefore in addition to the 0.5g/L concentration of national regulations, also separately design the chrome azurol S concentration of 0.25g/L, 1g/L, 2g/L and 4g/L, the suitableeest chrome azurol S concentration is selected according to perusal readability, obtain 0.5g/L, result is shown in that Fig. 2 0.5g/L concentration is good compared with other concentration color developing effects, it is simple to perusal；
The optimization method of the drying mode of described colour developing reagent paper is as follows:
Natural drying, freeze-day with constant temperature and vacuum constant temperature is selected to be dried three kinds of drying modes, optimum drying condition is determined from the flatness of dried paper, color and miscellaneous speckle situation, i.e. 50 DEG C, 4h of vacuum drying, processing mode and the results are shown in Table 1, through repetition test, vacuum drying can get rid of the major part introduced contaminants impact on reagent paper, and when temperature is 50 DEG C, reagent paper outward appearance is optimal, drying time 4h.Therefore it is that 50 DEG C of vacuum constant temperatures are dried 4h that reagent paper is dried optimum condition；
The optimization method of described step (7) middle observation testing result time is as follows:
Drip on reagent paper with aluminum standard solution, the colour developing situation of reagent paper after observation different time 0.5min, 1min, 2min, 3min, 5min, 10min, 20min, 30min, 60min, determine the optimal viewing testing result time, after i.e. chromogenic reaction occurs 1 minute, result is shown in Fig. 3, test paper color development district color similarity between developing time 30s～2min, and after 2min, colour developing district color increases in time and shoals, and is unfavorable for perusal.Considering to ensure that aluminum reacts completely with the developer on reagent paper, selecting developing time eventually is 1min.
The different drying mode of table 1 affects table to reagent paper
Table 1 result shows, through repetition test, naturally dries and needs 7h, and drying time is long, and affected by environment relatively big, reagent paper quality is unstable；Reagent paper is affected relatively big under the conditions of freeze-day with constant temperature by baking temperature, and reagent paper quality is low；Vacuum drying can get rid of the major part introduced contaminants impact on reagent paper, and when temperature is 50 DEG C, reagent paper outward appearance is optimal, drying time 4h.
Result shows, it is that 50 DEG C of vacuum constant temperatures are dried 4h that reagent paper is dried optimum condition.
Three, the making of instant reagent paper:
1, the making of colour developing reagent paper: the sulfuric acid solution by 1%, ethyl sodium solution, 3% acetic acid solution, cetrimonium bronmide solution, chrome azurol S solution are mixed and made into soak according to the ratio that volume ratio is 1:5:1:1:1, reagent paper carrier is cut into length takes advantage of the rectangle of a width of 4.5-5.5cm × 0.8-1.2cm to soak 4-5 hour in soak, 50 DEG C of vacuum constant temperatures are dried 4h, preserve, obtain colour developing reagent paper；
Described reagent paper carrier is chromatography filter paper；
2, the making of standard color comparison card: dripped by the aluminum standard solution of variable concentrations on colour developing reagent paper, after chromogenic reaction occurs 1-3 minute, uses color difference meter to take color, makes standard color comparison card, obtain instant reagent paper.
Four, food samples Pretreatment optimizes
Food is divided into 8 groups, ratio g:mL being separately added into food and acetic acid is 0, the ethanol that percentage by volume is 3% of 10:1,5:1,2:1,1:1,1:4,1:8,1:10, select the suitableeest 3% acetic acid addition, instant food is 1:1 with ratio g:mL of acetic acid, result is shown in Fig. 4, in the range of 3% acetic acid consumption is 0～5mL, the leaching rate of aluminum increases sharply with the increase of acid adding amount.In the range of 3% acetic acid consumption is 5～50mL, along with acetic acid consumption steps up, the leaching rate of aluminum tends to be steady.
The food of the suitableeest 3% acetic acid addition will be added, heat 1-60 minute with water-bath 25-100 DEG C, sampling detection at different temperatures 25-100 DEG C, observe the leaching content of its aluminum, select the water-bath soaking temperature 40 DEG C of the suitableeest food, result is shown in Fig. 5, soaking temperature be room temperature (24 DEG C) to 60 DEG C in the range of, aluminum leaching rate gradually rises with the rising of temperature, in the range of soaking temperature is 60～100 DEG C, along with the raising of soaking temperature, the leaching rate of aluminum declines, and in soaking temperature 80～100 DEG C, leaching rate declines substantially.
Food heated at constant temperature under the water-bath soaking temperature of the suitableeest food of the suitableeest 3% acetic acid addition will be added, in different time sampling detection in 1-60 minute, observe the aluminum leaching content of sample, select the heat time heating time of the suitableeest food, i.e. 30 minutes, result is shown in Fig. 6, in soak time is 1～30min, the prolongation in time of aluminum leaching rate and increase, in soak time is 30～60min, along with the prolongation of soak time, the leaching rate of aluminum tends to be steady.
Five, instant reagent paper of the present invention application of aluminium element content in detection food (such as Rhopilema esculenta sample)
Being added to the water after being shredded by 5g Rhopilema esculenta, ratio g:mL of Rhopilema esculenta and water is 1:9, adds the acetic acid 5mL that percentage by volume is 3%；Take soak after heating 30 minutes with water-bath 40 DEG C and drop on reagent paper, observing response district color, and contrast with standard color comparison card, the depth according to color realizes the detection to aluminum content, the most qualified regulation according to national standard of aluminium element content in the food of detection judges, such as aluminum content, more than 100mg/kg, is defective.
Comparing embodiment: utilize the aluminum content in the method detection Rhopilema esculenta sample of prior art
1) prepared by reagent paper: choosing filter paper is reagent paper material, and (1.5g/L chromazurine s) soaking temperature 50 DEG C dries after soaking 5h to place soak.
2) standard color comparison card makes: draw the Al standard solution (0.1g/L) of 0,0.1,0.25,0.5,1,3mL respectively, adds 0.2g/L brocide solution 1mL in each pipe, and 10.0g/L ascorbic acid 2mL is settled to 10mL.Taking the series concentration aluminum standard solution and 1 of preparation respectively) test-paper for preparing of step carries out chromogenic reaction.Observing color change under room temperature after 1min, by digital camera Taking Pictures recording experimental result, mark out corresponding Al concentration, colour print prepares standard color comparison card.
3) Rhopilema esculenta sample detection: Rhopilema esculenta deionized water is soaked more than 10 minutes, obtain Rhopilema esculenta sample liquid, take Rhopilema esculenta sample liquid and be fully uniformly mixed so as to obtain solution to be measured with brocide and ascorbic acid solution successively, solution to be measured is added drop-wise to 1) on the reagent paper prepared of step, it is made to carry out chromogenic reaction with detection paper of aluminum,test sheet, reacted reagent paper is contrasted with standard color comparison card, directly reads the concentration of Al in liquid to be measured.The recovery of standard addition drawing Rhopilema esculenta sample is 85.1%-127.8%, detects aluminum in liquid to be measured and compares the R after drawing two kinds of method detected value linear fits afterwards with ICP-MS method2=0.8243.
Use detection paper Rhopilema esculenta sample of the present invention, the recovery of standard addition drawing sample is 94.6%-105.8%, detecting aluminum in soak and have the higher goodness of fit with ICP-MS method result, the equation after two kinds of method detected value linear fits is: Y=1.0159x-0.0724, R2=0.9624.
To sum up, the method for this instant detection paper Aluminum Content in Food, compared with the method for comparing embodiment, substantially increases detection range and the accuracy rate of aluminium element in food samples.
Claims (8)
1. the instant reagent paper of a rapid evaluation aluminum in food constituent content, it is characterised in that: making step is as follows:
(1) prepare the sulfuric acid solution of 1%: draw 1mol/L sulphuric acid dilute with water, until adding sulphuric acid to account for the body of overall solution volume
Long-pending percent is 1-3%, obtains the sulfuric acid solution of 1%；
(2) prepare ethyl sodium solution: weighing the sodium acetate mass concentration to sodium acetate soluble in water is
0.075～0.076g/mL, it is subsequently adding glacial acetic acid, adjusts pH to 5-5.5, the mass concentration being then diluted with water to sodium acetate is
0.068g/mL, obtains ethyl sodium solution；
Described sodium acetate: ratio g:mL of glacial acetic acid is 17:1.3-1.5；
(3) prepare 3% acetic acid solution: drawing the percentage by volume that glacial acetic acid is slowly added in ultra-pure water to glacial acetic acid is 3%, so
Rear mixing, obtains 3% acetic acid solution；
(4) prepare cetrimonium bronmide solution: weigh cetrimonium bronmide and be diluted with water to hexadecyl three
The concentration of methylamine is 0.2-0.25g/L, obtains cetrimonium bronmide solution；
(5) prepare chrome azurol S solution: weighing chrome azurol S and being diluted with water to the concentration of chrome azurol S is 0.5-0.6g/L, obtains chromium sky
Blue or green S solution；
(6) develop the color the making of reagent paper: the sulfuric acid solution by 1%, ethyl sodium solution, 3% acetic acid solution, cetyl
Base trimethylamine solution, chrome azurol S solution are mixed and made into soak, by reagent paper according to the ratio that volume ratio is 1:5:1:1:1
Carrier is cut into length and takes advantage of the rectangle of a width of 4.5-5.5cm × 0.8-1.2cm to soak in soak 3-5 hour, and 50 DEG C of vacuum constant temperatures are done
Dry 4h, preserves, obtains colour developing reagent paper；
Described reagent paper carrier is chromatography filter paper；
(7) the making of standard color comparison card: being dripped by the aluminum standard solution of variable concentrations on colour developing reagent paper, chromogenic reaction occurs 1-3 to divide
Zhong Hou, uses color difference meter to take color, makes standard color comparison card；
The most i.e. obtain instant reagent paper.
The instant reagent paper of rapid evaluation aluminum in food constituent content the most according to claim 1, it is characterised in that: make
Step is as follows:
(1) prepare the sulfuric acid solution of 1%: draw 1mol/L sulphuric acid dilute with water, until adding sulphuric acid to account for the body of overall solution volume
Long-pending percent is 1%, obtains the sulfuric acid solution of 1%；
(2) prepare ethyl sodium solution: weighing the sodium acetate mass concentration to sodium acetate soluble in water is
0.075～0.076g/mL, it is subsequently adding glacial acetic acid, adjusts pH to 5.5, the mass concentration being then diluted with water to sodium acetate is
0.068g/mL, obtains ethyl sodium solution；
Described sodium acetate: ratio g:mL of glacial acetic acid is 17:1.3；
(3) prepare 3% acetic acid solution: drawing the percentage by volume that glacial acetic acid is slowly added in ultra-pure water to glacial acetic acid is 3%, so
Rear mixing, obtains 3% acetic acid solution；
(4) prepare cetrimonium bronmide solution: weigh cetrimonium bronmide and be diluted with water to hexadecyl three
The concentration of methylamine is 0.2g/L, obtains cetrimonium bronmide solution；
(5) prepare chrome azurol S solution: weighing chrome azurol S and being diluted with water to the concentration of chrome azurol S is 0.5g/L, obtains chrome azurol S
Solution；
(6) develop the color the making of reagent paper: the sulfuric acid solution by 1%, ethyl sodium solution, 3% acetic acid solution, cetyl
Base trimethylamine solution, chrome azurol S solution are mixed and made into soak, by reagent paper according to the ratio that volume ratio is 1:5:1:1:1
Carrier is cut into length and takes advantage of the rectangle of a width of 5cm × 1cm to soak in soak 4 hours, and 50 DEG C of vacuum constant temperatures are dried 4h, preserves,
Must be developed the color reagent paper；
Described reagent paper carrier is chromatography filter paper；
(7) the making of standard color comparison card: the aluminum standard solution of variable concentrations 0.25g/L, 0.5g/L, 1g/L, 2g/L, 4g/L is dripped
In on colour developing reagent paper, after chromogenic reaction occurs 1 minute, use color difference meter to take color, make standard color comparison card；
The most i.e. obtain instant reagent paper.
The instant reagent paper of rapid evaluation aluminum in food constituent content the most according to claim 1 and 2, it is characterised in that:
The optimization method of the described step (5) concentration of middle chrome azurol S is as follows:
Based on chrome azurol S compound concentration in GB GB/T5009.182 2003, except the 0.5g/L concentration of national regulations
Outward, also separately design the chrome azurol S concentration of 0.25g/L, 1g/L, 2g/L and 4g/L, selected according to perusal readability
Select the suitableeest chrome azurol S concentration, obtain 0.5g/L；
Or, the optimization method of described step (6) pilot scale paper carrier is as follows:
A4 paper, common quantitative filter paper and chromatography filter paper is used to make by the manufacture method of instant reagent paper as reagent paper carrier,
And aluminum standard solution is dripped on reagent paper carrier, observe the colour developing area on each reagent paper carrier and color developing effect, and select the suitableeest
Reagent paper carrier, i.e. chromatography filter paper；
Or, the optimization method of the described step (6) drying mode of middle colour developing reagent paper is as follows:
Natural drying, freeze-day with constant temperature and vacuum constant temperature is selected to be dried three kinds of drying modes, from the flatness of dried paper, color and miscellaneous
Speckle situation determines optimum drying condition, i.e. 50 DEG C, 4h of vacuum drying；
Or, the optimization method of described step (7) middle observation testing result time is as follows:
Drip on reagent paper with aluminum standard solution, observation different time colour developing situation of reagent paper after 0.5-60 minute, determine optimal viewing
After testing result time, i.e. chromogenic reaction occur 1 minute.
4. the using method of the instant reagent paper of the rapid evaluation aluminum in food constituent content as described in any one of claims 1 to 3,
It is characterized in that: step is as follows:
Being added to the water after being shredded by food, ratio g:mL of food and water is 1:5-12, and adding percentage by volume is 3%
Acetic acid, described food is 1:1-3 with ratio g:mL of acetic acid；Immersion drop is taken after heating 1-60 minute with water-bath 30-60 DEG C
On display reagent paper, observing response district color, and contrast with standard color comparison card, realize the inspection to aluminum content according to the depth of color
Survey.
The using method of the instant reagent paper of rapid evaluation aluminum in food constituent content the most according to claim 4, its feature
It is: the detection method of described aluminum in food constituent content is as follows:
Being added to the water after being shredded by food, ratio g:mL of food and water is 1:9, adds the second that percentage by volume is 3%
Acid, described food is 1:1 with ratio g:mL of acetic acid；Immersion drop is taken after soaking heating 30-50 minute with water-bath 40 DEG C
On display reagent paper, observing response district color, and contrast with standard color comparison card, realize the inspection to aluminum content according to the depth of color
Surveying, the most qualified regulation according to national standard of aluminium element content in the food of detection judges.
The using method of the instant reagent paper of rapid evaluation aluminum in food constituent content the most according to claim 5, its feature
It is: the condition optimizing of described food pre-treatment is as follows:
Food is divided into 8 groups, ratio g:mL being separately added into food and acetic acid is 0,10:1,5:1,2:1,1:1,
The percentage by volume of 1:4,1:8,1:10 is the ethanol of 3%, selects the suitableeest 3% acetic acid addition, instant food and acetic acid
Ratio g:mL is 1:1；
The food of the suitableeest 3% acetic acid addition will be added, heat 1-60 minute with water-bath 25-100 DEG C, in different temperatures 25-100 DEG C
Lower sampling detection, observes the leaching content of its aluminum, selects the water-bath soaking temperature of the suitableeest food, be 40 DEG C；
By adding food heated at constant temperature under the water-bath soaking temperature of the suitableeest food of the suitableeest 3% acetic acid addition, at different time
Sampling detection in 1-60 minute, observes the aluminum leaching content of sample, selects the heat time heating time of the suitableeest food, be 30 minutes.
7. the instant reagent paper of the rapid evaluation aluminum in food constituent content as described in any one of claims 1 to 3 is quickly measuring
Application in Aluminum Content in Food.
The instant reagent paper of rapid evaluation aluminum in food constituent content the most according to claim 7 is at Rapid determination of aluminum in food
Application in content, it is characterised in that: described food is Rhopilema esculenta or fritters of twisted dough.
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