CN109580516A - A kind of detection method of polyacrylamide - Google Patents
A kind of detection method of polyacrylamide Download PDFInfo
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- CN109580516A CN109580516A CN201910032040.7A CN201910032040A CN109580516A CN 109580516 A CN109580516 A CN 109580516A CN 201910032040 A CN201910032040 A CN 201910032040A CN 109580516 A CN109580516 A CN 109580516A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N2021/786—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour with auxiliary heating for reaction
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Abstract
The present invention provides a kind of detection methods of polyacrylamide, belong to field of organic compound detection.The present invention is stood after mixing sample to be tested with water, takes supernatant；Amylase is added into supernatant, and is heated, pretreatment liquid is obtained；In sodium acetate-aluminum sulfate buffer, is stood after pretreatment liquid is successively mixed with bromine water, sodium formate and starch-iodide cadmium solution, obtain prepare liquid；Using the absorbance value of spectrophotometer test prepare liquid, the content of polyacrylamide in sample to be tested is then calculated according to the concentration of polyacrylamide-absorbance value standard curve.Method accuracy provided by the invention and precision are higher, embodiment the result shows that, the recovery of standard addition of method provided by the invention is 102.9%~109.3%, and precision is 3.8%~5.1%.
Description
Technical field
The present invention relates to field of organic compound detection more particularly to a kind of detection methods of polyacrylamide.
Background technique
It is water-soluble that polyacrylamide (polyacrylamide, PAM) is that acrylamide (acrylamide, AM) is polymerized
Property linear polymeric polymer, do not dissolve in most of organic solvents, have good flocculability, be widely used in oil exploitation,
The industries such as wastewater treatment, papermaking.Because of its special flocculating property, GB2760-2014 regulation polyacrylamide can be used as flocculation
Agent, filter aid are used for processing technology, sugar refining technology and the zymotechnique of beverage (water process).It is decomposed due to polyacrylamide
Monomeric acrylamide is classified as " may be to people's carcinogen ", national food safety standard by international cancer research institution (IARC)
Acrylamide monomer content must not exceed 0.025% in " GB31629-2016 " regulation food grade polyacrylamide, and except above-mentioned
Outside purposes, it cannot make an addition in food and be used as thickener or other types additive.
Commercially available Molecular Weight for Polyacrylamide between 2,000,000 to 20,000,000, by ion characteristic can be divided into nonionic, yin from
Son, cation and four seed type of amphoteric.Polyacrylamide in presently found food is cationic, and molecular weight is
8000000~12,000,000.Existing polyacrylamide detection method has starch-iodide chromium method, mass concentration method etc., is suitable for petroleum
The industries such as exploitation, wastewater treatment.Since Protein in Food, starch, fat are macromolecular substances, polypropylene in the prior art
The detection method of amide haves the shortcomings that specificity is low, interference is big, and sensitivity and dosing accuracy are difficult to meet actual demand.
Therefore it is badly in need of researching and developing a kind of accurate, polyacrylamide additive amount in simplicity measurement food detection method.
Summary of the invention
The present invention provides a kind of detection method of polyacrylamide, method accuracy provided by the invention and precision are equal
Higher, wherein recovery of standard addition is 102.9%~109.3%, and precision is 3.8%~5.1%.
The present invention provides a kind of detection methods of polyacrylamide, comprising the following steps:
(1) it is stood after mixing sample to be tested with water, takes supernatant；The sample to be tested is Flour product and/or rice made products；
(2) amylase is added in the supernatant that Xiang Suoshu step (1) obtains, and is heated, obtain pretreatment liquid；
(3) in sodium acetate-aluminum sulfate buffer, the pretreatment liquid that the step (2) is obtained successively with bromine water, formic acid
It is stood after sodium and the mixing of starch-iodide cadmium solution, obtains prepare liquid；
(4) using the absorbance value of spectrophotometer test prepare liquid, then according to concentration-absorbance of polyacrylamide
The content of polyacrylamide in sample to be tested is calculated in value standard curve.
Preferably, in the step (1) sample to be tested include in flour, rice flour, noodles, vermicelli, steamed bun and rice cake one
Kind is a variety of.
Preferably, the temperature heated in the step (2) is 50 DEG C, time 80min.
Preferably, sodium acetate-aluminum sulfate buffer pH value is 5.0 in the step (3).
Preferably, sodium formate is aqueous sodium formate solution in the step (3), and the mass concentration of the aqueous sodium formate solution is
1.0%.
Preferably, the test wavelength of spectrophotometer is 550nm in the step (4).
Preferably, concentration-absorbance value standard curve of polyacrylamide is y=0.00027821x in the step (4)
+ 0.033629, x are concentration of polyacrylamide, and y is polyacrylamide absorbance value, the R of standard curve2=0.0996.
The present invention provides a kind of detection method of polyacrylamide, is stood after sample to be tested is mixed with water, take supernatant
Liquid；The sample to be tested is Flour product and/or rice made products；Amylase is added into supernatant, and is heated, before obtaining
Treatment fluid；In sodium acetate-aluminum sulfate buffer, pretreatment liquid is successively mixed with bromine water, sodium formate and starch-iodide cadmium solution
It is stood after conjunction, obtains prepare liquid；Using the absorbance value of spectrophotometer test prepare liquid, then according to the dense of polyacrylamide
The content of polyacrylamide in sample to be tested is calculated in degree-absorbance value standard curve.Method provided by the invention can be surveyed
Examination obtains the polyacrylamide amine content in Flour product and/or rice made products, and Flour product can not accurately be tested in the prior art by solving
And/or the problem of rice made products polyacrylamide amine content.In the present invention, the amide groups in the sample to be tested reacts life with bromine water
At N- bromo-acid amide, the N- bromo-acid amide is unstable in water, and N- bromo-acid amide occurs hydrolysis and generates hypobromous acid, and cadmium iodide is fixed
Amount ground is reacted with hypobromous acid generates iodine, and three iodo-complexes of iodine and Starch formation blue carry out chromogenic reaction, then pass through test
The absorbance value of prepare liquid after colour developing, it can be deduced that the content of polyacrylamide in sample to be tested.Method provided by the invention
Accuracy and precision are higher, embodiment the result shows that, the recovery of standard addition of method provided by the invention is 102.9%~
109.3%, precision is 3.8%~5.1%.
Specific embodiment
The present invention provides a kind of detection methods of polyacrylamide, comprising the following steps:
(1) it is stood after mixing sample to be tested with water, takes supernatant；The sample to be tested is Flour product and/or rice made products；
(2) amylase is added in the supernatant that Xiang Suoshu step (1) obtains, and is heated, obtain pretreatment liquid；
(3) in sodium acetate-aluminum sulfate buffer, the pretreatment liquid that the step (2) is obtained successively with bromine water, formic acid
It is stood after sodium and the mixing of starch-iodide cadmium solution, obtains prepare liquid；
(4) using the absorbance value of spectrophotometer test prepare liquid, then according to concentration-absorbance of polyacrylamide
The content of polyacrylamide in sample to be tested is calculated in value standard curve.
The present invention is stood after mixing sample to be tested with water, takes supernatant.In the present invention, the sample to be tested is wheat flour
Product and/or rice made products preferably include one of flour, rice flour, noodles, vermicelli, steamed bun and rice cake or a variety of；The present invention is to sample
The content of polyacrylamide does not require in product.The present invention preferably crushes sample to be tested, the grain of sample to be tested after crushing
Diameter is preferably 80~100 mesh.In the present invention, the amount ratio of the sample to be tested and water is preferably 0.8~1.5g:10mL.This
Invention mixes sample to be tested with water preferably by the way of being stirred, and the revolving speed being stirred is preferably 400~
600rpm.In the present invention, the time of the standing is preferably 6~12h.After the completion of standing, supernatant is collected.The present invention passes through
Within the above range by the size controlling of sample to be tested, and by the control of the amount ratio of sample to be tested and water within the above range, knot
The collective effect for closing speed of agitator and time of repose, can sufficiently be transferred to supernatant for the polyacrylamide in sample to be tested
In.The polyacrylamide type that the present invention tests is preferably cationic, the polyacrylamide that molecular weight is 8,000,000~12,000,000
Amine.
After obtaining supernatant, amylase is added into supernatant by the present invention, and is heated, and obtains pretreatment liquid.
In the present invention, the activity of the amylase is preferably 15~25U/mL, further preferably 20U/cm.In the present invention, institute
The temperature for stating heat treatment is preferably 45~55 DEG C, and further preferably 50 DEG C, the time is preferably 80~90min.The present invention is logical
Addition amylase is crossed, can be reduced sugar by the Starch Hydrolysis in sample to be tested, avoid the starch in sample to be tested to subsequent inspection
The interference of survey process chromogenic reaction.The present invention preferably controls the activity of amylase within the above range, is conducive to supernatant
In remaining starch be fully hydrolyzed, to eliminate influence of the starch to subsequent chromogenic reaction.
After obtaining pretreatment liquid, the present invention in sodium acetate-aluminum sulfate buffer, by pretreatment liquid successively with bromine water, first
It is stood after sour sodium and the mixing of starch-iodide cadmium solution, obtains prepare liquid.
In the present invention, the sodium acetate-aluminum sulfate buffer pH value is preferably 4.8~5.2, further preferably
5.0, the sodium acetate-aluminum sulfate buffer preparation method preferably includes: after sodium acetate trihydrate crystal is mixed with water, adding
Enter hydrazine aluminum sulfate, the pH value for adjusting mixed solution with acetic acid obtains sodium acetate-aluminum sulfate buffer to above-mentioned pH value；It is described
The amount ratio of sodium acetate trihydrate crystal and water is preferably 20~30g:800mL, further preferably 25g:800mL；Described three
The mass ratio for being hydrated acetic acid sodium crystal and hydrazine aluminum sulfate is preferably 20~30:0.7~0.8, further preferably 25:0.75.
The present invention mixes in sodium acetate-aluminum sulfate buffer, by pretreatment liquid with bromine water.In the present invention, the bromine
Water is preferably saturated bromine water, and the bromine water volume and sodium acetate-aluminum sulfate buffer volume ratio are 1~3:25, further preferably
For 2:25.The present invention is stood after preferably mixing pretreatment liquid and bromine water, so that the amide groups in bromine water and pretreatment liquid
Reaction completely generates N- bromo-acid amide；The time of the standing is preferably 4~10min, further preferably 5min.The present invention
It is preferred that keeping bromine water excessive, the amide groups in pretreatment liquid is fully converted into N- bromo-acid amide.
After having reacted with bromine water, sodium formate is added into above-mentioned system to be measured in the present invention.In the present invention, the sodium formate
Preferably aqueous sodium formate solution, the mass concentration of the aqueous sodium formate solution are preferably 0.8%~1.1%, further preferably
1.0%；The volume ratio of the aqueous sodium formate solution and bromine water is preferably 4~6:2, further preferably 5:2.The present invention preferably exists
After sodium formate is added, system to be measured is stood, so that sodium formate can restore excessive bromine water, avoids bromine water
Strong oxidizing property has an impact detection process, and the obtained Br ion pair testing result that restores does not influence；The standing
Time is preferably 3~10min, further preferably 4min.
After the reaction was completed with sodium formate, the present invention, which continues up, states addition starch-iodide cadmium solution in system to be measured, then
It stands, obtains prepare liquid.In the present invention, volume ratio preferably 2~3:1 of the starch cadmium iodide and bromine water, further preferably
For 5:2.In the present invention, the time of the standing is preferably 5~10min, further preferably 5min.In the present invention, preceding
The N- bromo-acid amide that amide groups in treatment fluid reacts generation with bromine water is unstable in water, and N- bromo-acid amide occurs hydrolysis and generates
Hypobromous acid, cadmium iodide, which is quantitatively reacted with hypobromous acid, generates iodine, and three iodo-complexes of iodine and Starch formation blue develop the color anti-
It answers, obtains prepare liquid.
After obtaining prepare liquid, the present invention tests the absorbance value of prepare liquid using spectrophotometer, then according to polypropylene
The content of polyacrylamide in sample to be tested is calculated in the concentration of amide-absorbance value standard curve.In the present invention, described
The concentration of polyacrylamide-absorbance value standard curve is preferably y=0.00027821x+0.033629, and x is polyacrylamide
Concentration, y are polyacrylamide absorbance value, the R of standard curve2=0.0996.In the present invention, the polyacrylamide is dense
Degree-absorbance value standard curve is preferably obtained by following steps:
(i) standard items of polyacrylamide are configured to the standard solution that concentration is gradient；
(ii) in sodium acetate-aluminum sulfate buffer, multiple standard solution that the step (i) is obtained successively with bromine
It is stood after water, sodium formate and the mixing of starch-iodide cadmium solution, obtains standard items prepare liquid；
(iii) gained standard items prepare liquid is measured with spectrophotometer, is drawn according to the light absorption value measured dense
Degree-light absorption value standard curve.
In the present invention, the polyacrylamide is preferably cationic-type polyacrylamide, point of the polyacrylamide
Son amount preferably 8,000,000~12,000,000.
In the present invention, it is preferably 50mg/L, 70mg/ that concentration, which is the concentration of standard solution of gradient, in the step (i)
L, 90mg/L, 110mg/L, 130mg/L, 150mg/L and 170mg/L.
In the present invention, by standard solution obtain the processing method of standard items prepare liquid preferably in above scheme by preceding
The processing method that reason liquid obtains prepare liquid is identical, and details are not described herein.
The present invention tests the absorbance value of prepare liquid, in the present invention, the spectrophotometer using spectrophotometer
Test wavelength is preferably 550nm.Test wavelength is preferably 550nm by the present invention, and method provided by the invention is tested
Polyacrylamide-type be cationic, the polyacrylamide that molecular weight is 8,000,000~12,000,000.Method provided by the invention
Under other test wavelengths, it can not accurately test to obtain cationic, polyacrylamide that molecular weight is 8,000,000~12,000,000
Content.
Below in conjunction with the embodiment in the present invention, the technical solution in the present invention is clearly and completely described.
Sample to be tested in the present embodiment 1 is the noodles for being added to polyacrylamide, detection method packet described in the present embodiment
Include following steps:
S1: after polyacrylamide standard items are diluted with deionized water, being stirred with blender, and mixing speed is
500rpm, mixing time 6h.Then constant volume be following concentration gradient standard solution: 50mg/L, 70mg/L, 90mg/L,
110mg/L、130mg/L、150mg/L、170mg/L。
S2: match sodium acetate-aluminum sulfate buffer solution.25g sodium acetate trihydrate crystal is put into 1L beaker, is added
0.75g hydrazine aluminum sulfate is added after mixing evenly in 800mL water；Then this buffer solution is measured with corrected acidometer
PH, with acetic acid tune pH value to 5.0；The above-mentioned buffer of 25ml is pipetted in 50mL volumetric flask, 2mL standard solution is added, mixing is equal
After even, 2ml is added to be saturated bromine water, shakes up and place 5min.Adding mass concentration is 1.0% sodium formate solution 5mL, shakes up and stands 4min.
5mL starch-cadmium iodine liquid is added, is diluted to scale with pure water, shakes up and stands 5min, obtain standard items prepare liquid.
S3: with spectrophotometer at 550nm wavelength, standard items prepare liquid is detected, obtains standard items in 50mg/
The concentration of L~170mg/L-absorbance value standard curve；In 50mg/L~170mg/L concentration range, the line of polyacrylamide
Property regression equation be y=0.00027821x+0.033629, R2=0.0996 (y: polyacrylamide absorbance value, x: polypropylene
Amide concentration).
S4: precise 20g noodles sample after being crushed to 80 mesh, is placed in 500ml beaker, and 200mL pure water is added,
It is stirred with the speed of 600rpm, is stood overnight after stirring 7h, take supernatant.15U/ml amylase is added in supernatant, 50
80min is reacted in DEG C shaker water bath case, obtains pretreatment liquid.
S5: pipetting the sodium acetate-aluminum sulfate buffer 25ml prepared in S2 in 50mL volumetric flask, and 2mL pre-treatment is added
Liquid adds 2mL to be saturated bromine water after mixing, shakes up and places 5min；Adding mass concentration is 1.0% sodium formate solution 5mL, is shaken up
Stand 4min.5mL starch-cadmium iodine liquid is added, is diluted to scale with pure water, shakes up and stands 5min, prepare liquid.
S6: with spectrophotometer at 550nm wavelength, prepare liquid is detected, obtain prepare liquid 50mg/L~
Then the absorbance value of 170mg/L calculates polyacrylamide amine content in noodles sample by equation of linear regression.
The precision and the rate of recovery of above-mentioned test method are tested, test method are as follows:
The mark-on into above-mentioned noodles sample, the horizontal mark-on of low concentration select 10mg/L, the selection of intermediate concentration level's mark-on
50mg/L, the horizontally selected 100mg/L of high concentration.Concentrations above level is handled and is surveyed according to the experimental procedure and condition
It is fixed, it is repeated 3 times, the calculation method rate of recovery and standard deviation.The results are shown in Table 1.
1 recovery of standard addition of table and precision result
By 1 test result of table it is found that the recovery of standard addition result of method provided by the invention is 102.9%~109.3%,
Precision is 3.8%~5.1%.It follows that method accuracy provided by the invention and precision are higher.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of detection method of polyacrylamide, comprising the following steps:
(1) it is stood after mixing sample to be tested with water, takes supernatant；The sample to be tested is Flour product and/or rice made products；
(2) amylase is added in the supernatant that Xiang Suoshu step (1) obtains, and is heated, obtain pretreatment liquid；
(3) in sodium acetate-aluminum sulfate buffer, the pretreatment liquid that the step (2) is obtained successively with bromine water, sodium formate and
It is stood after the mixing of starch-iodide cadmium solution, obtains prepare liquid；
(4) using the absorbance value of spectrophotometer test prepare liquid, then according to the concentration of polyacrylamide-absorbance value mark
The content of polyacrylamide in sample to be tested is calculated in directrix curve.
2. detection method according to claim 1, which is characterized in that sample to be tested includes flour, rice in the step (1)
One of powder, noodles, vermicelli, steamed bun and rice cake are a variety of.
3. detection method according to claim 1, which is characterized in that the temperature heated in the step (2) is 50
DEG C, time 80min.
4. detection method according to claim 1, which is characterized in that sodium acetate-aluminum sulfate buffer in the step (3)
PH value be 5.0.
5. detection method according to claim 1 or 4, which is characterized in that sodium formate is sodium formate water in the step (3)
Solution, the mass concentration of the aqueous sodium formate solution are 1.0%.
6. detection method according to claim 1, which is characterized in that the test waves of spectrophotometer in the step (4)
A length of 550nm.
7. detection method according to claim 1 or 6, which is characterized in that polyacrylamide is dense in the step (4)
Degree-absorbance value standard curve is y=0.00027821x+0.033629, and x is concentration of polyacrylamide, and y is polyacrylamide
Absorbance value, the R of standard curve2=0.0996.
8. according to claim 1, detection method described in 2,3,4 or 6, which is characterized in that the type of the polyacrylamide is
Cationic, the polyacrylamide that molecular weight is 8,000,000~12,000,000.
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Application publication date: 20190405 |
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