CN103411911B - The method of aluminium content in Fast Measurement flour-made food - Google Patents
The method of aluminium content in Fast Measurement flour-made food Download PDFInfo
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Abstract
The invention provides the method for aluminium content in a kind of Fast Measurement flour-made food, prepare six kinds of aluminum standard solutions with aluminium standard reserving solution; Draw aluminum standard solution in color comparison tube with a scale, add chrome azurol S solution, polyoxyethylene nonylphenol ether solution, bromide sixteen alkyls pyridine solution and ethylenediamine-hydrochloride buffer respectively, constant volume, after shaking up placement, measure absorbance; Draw the working curve of series aluminum titer; Take tested surface goods, dry, grind, sieve, make butt sample; In butt sample, add distilled water and acid solution, after ultrasound wave extracts, filter, obtain sample preparation liquid; Sample preparation liquid and above-mentioned agents useful for same are added color comparison tube, is settled to scale, shakes up placement, measure absorbance, make blank assay simultaneously; According to the aluminium content in formulae discovery tested surface goods.This rapid assay methods can shorten the sample cycle, save the energy, and stability, reappearance and stability are better, and the recovery is higher, can meet the testing requirement in laboratory.
Description
Technical field
The invention belongs to technical field of food safety detection, relate to a kind of method measuring certain element-specific content in flour-made food, particularly a kind of method of aluminium content in Fast Measurement flour-made food.
Background technology
Aluminium is not human essential elements, when up to the present also not finding that human body lacks, anything can be brought to damage to health, otherwise aluminium salt is taken in and human body formation accumulation property too much can be made poisoning, and affect child's bone growth, intelligence also can be subject to certain impact; Degradation harmfulness disease under senile dementia, encephalopathic, osteopathy, ephrosis, non-iron deficiency anemia, body's immunity can be caused.
In flour-made food the largest source of aluminium be artificial over range, Use out of range containing aluminium food additives (such as: using 12 hydrazine aluminum sulfate potassium as leavening agent), aluminium composition in flour-made food is obviously increased.In the flour-made food such as steamed bun, deep-fried twisted dough sticks, to exceed the situation of national standard very serious for the content of aluminium.Therefore, the content detecting aluminum in food ion is enforced in state food security fields.In flour-made food, Al-single crystal method mainly performs the spectrophotometer method specified in GB GB/T5009.182-2003.In addition, atomic absorption spectrography (AAS) (А А S), inductively coupled plasma emission spectrography (Ι CP-OES) etc. are also had.All adopt nitric acid in these detection methods, perchloric acid cleared up, Microwave Digestion and dry ashing method processing sample, sample preparation length consuming time, inefficiency, testing cost are higher.
Prior art compares with assay method of the present invention:
When adopting dry method to carry out pre-treatment to sample, 4h and ashing 4h need be carbonized, process consuming time longer.When adopting Wet to carry out pre-treatment to sample, sample is cleared up after needing acid adding soaked overnight, clears up and at least needs 4 hours, consuming time longer; And digestion solution is generally the higher perchloric acid of concentration, nitric acid, the acid mist that digestion process produces is large to human injury, and reagent dosage is comparatively large, and testing cost is higher.And assay method of the present invention adopts ultrasonic extraction, only need 5 ~ 30min, shorten the processing time, save the energy, increase work efficiency.
Summary of the invention
The object of this invention is to provide that a kind of sample processing time is short, work efficiency is high, the method for aluminium content in the Fast Measurement flour-made food that testing cost is low.
For achieving the above object, the technical solution adopted in the present invention is: a kind of method of aluminium content in Fast Measurement flour-made food, specifically carries out according to the following steps:
Step 1: the six kinds of aluminum standard solutions being respectively 0.5 μ g/mL, 1.0 μ g/mL, 2.0 μ g/mL, 3.0 μ g/mL, 4.0 μ g/mL and 5.0 μ g/mL with the aluminium standard reserving solution preparation mass body volume concentrations of mass body volume concentrations 1.0mg/mL; Each aluminum standard solution is handled as follows respectively: draw 100 μ L aluminum standard solutions in the color comparison tube that 5mL is with a scale, add 300 μ L chrome azurol S solution, 100 μ L polyoxyethylene nonylphenol ether solution, 200 μ L bromide sixteen alkyls pyridine solution and 300 μ L ethylenediamine-hydrochloride buffers respectively, distilled water is settled to 2.5mL, shake up after placing 15min, under 620nm wavelength, measure absorbance; Then take absorbance as ordinate, in aluminium titer, the quality of aluminium is horizontal ordinate, draws the working curve of series aluminum titer; Make blank assay simultaneously, make reference with blank;
Step 2: take the uniform tested surface goods of 10g as sample, dries 3 ~ 6h, grinds, sieve, make butt sample at 100 ± 3 DEG C of temperature;
Step 3: take 0.1g butt sample, be placed in 50mL beaker, adds 18mL distilled water and 2.0mL acid solution, and ultrasound wave extracts 5 ~ 30min, filters extract, obtains sample preparation liquid;
Step 4: get 100 μ L sample preparation liquid in 5mL color comparison tube with a scale, add 300 μ L chrome azurol S solution, 100 μ L polyoxyethylene nonylphenol ether solution, 200 μ L bromide sixteen alkyls pyridine solution and 300 μ L ethylenediamine-hydrochloride buffers respectively, 2.5mL scale is settled to distilled water, shake up placement 15 ~ 120min, with UV2300 twin-beam ultraviolet scene photometer, under 620nm wavelength, measure absorbance, make blank assay simultaneously;
Step 5: according to the absorbance of the sample preparation liquid that step 4 records, finds the quality of the aluminium that this absorbance is corresponding, is calculated as follows the aluminium content X in tested surface goods from the working curve of the series aluminum titer of step 1 drafting:
In formula: X represents the aluminium content in sample, unit mg/kg; C
1represent the quality of the aluminium corresponding to absorbance of the sample preparation liquid that step 5 records, unit μ g; C
0represent the quality of aluminium in sample blank liquid, unit μ g; M represents sample mass, unit g; V
1represent the cumulative volume of sample preparation liquid in step 4, Unit/mL; V
2represent the volume of liquid after constant volume in step 5, Unit/mL.
Reagent used in above-mentioned steps 1 and step 5:
Take 0.1g chrome azurol S, be dissolved in 100mL ethanolic solution (1+1), mixing, obtains the chrome azurol S solution that mass body volume concentrations is 1g/L;
3.0mL polyoxyethylene nonylphenol ether is dissolved in 100mL water, is made into polyoxyethylene nonylphenol ether solution;
Take 0.6g bromide sixteen alkyls pyridine, be dissolved in 30mL ethanol, be diluted with water to 200mL, obtain bromide sixteen alkyls pyridine solution;
Get anhydrous ethylenediamine 100mL, add pure water 200mL, adding 190mL mass body volume concentrations after cooling is the hydrochloric acid of 1.19g/mL, stirs evenly, and adjust ph is 6.7 ~ 7.0, obtained ethylenediamine-hydrochloride buffer;
Rapid assay methods of the present invention uses the aluminium in ultrasound wave extraction flour-made food, sample is without dry method or wet digesting process, detection speed accelerated greatly, shortens the sample cycle, save the energy, and there is good stability, reappearance and stability, and the recovery is higher, the testing requirement in laboratory can be met.
Accompanying drawing explanation
Fig. 1 is the working curve diagram of the series aluminum titer drawn in the inventive method.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
In flour-made food, Al-single crystal method mainly performs the spectrophotometer method specified in GB GB/T5009.182-2003.In addition, atomic absorption spectrography (AAS) (А А S), inductively coupled plasma emission spectrography (Ι CP-OES) etc. are also had.But all adopt nitric acid in these detection methods, perchloric acid cleared up, Microwave Digestion and dry ashing method processing sample, sample preparation length consuming time, inefficiency, testing cost are higher.In order to overcome above-mentioned problems of the prior art, the invention provides the method for aluminium content in a kind of Fast Measurement flour-made food, such that sample processing time is short, work efficiency is high, testing cost is low.This rapid assay methods is specifically carried out according to the following steps:
Step 1: take 0.1g chrome azurol S (C
23h
13o
9sC
l2na
3), be dissolved in 100mL ethanolic solution (1+1), mixing, obtains the chrome azurol S solution that mass body volume concentrations is 1g/L;
3.0mL polyoxyethylene nonylphenol ether is dissolved in 100mL water, is made into polyoxyethylene nonylphenol ether solution;
Take 0.6g bromide sixteen alkyls pyridine (CPB), be dissolved in 30mL ethanol (φ (C
2h
5oH)=95%) in, be diluted with water to 200mL, obtain bromide sixteen alkyls pyridine solution;
Get anhydrous ethylenediamine (C
2h
8n
2) 100mL, add pure water 200mL, slowly adding 190mL mass body volume concentrations after cooling is the hydrochloric acid of 1.19g/mL, stirs evenly, and is 6.7 ~ 7.0 by acidometer adjust ph, obtained ethylenediamine-hydrochloride buffer; If pH>7, then slowly drip hydrochloric acid, if pH<6.7, ethylenediamine solution (1+2) can be added;
Step 2: prepare six kinds of aluminum standard solutions that mass body volume concentrations is respectively 0.5 μ g/mL, 1.0 μ g/mL, 2.0 μ g/mL, 3.0 μ g/mL, 4.0 μ g/mL and 5.0 μ g/mL with the aluminium standard reserving solution (purchased from China National Measuring Science Research Inst.: Beijing) of mass body volume concentrations 1.0mg/mL; Each aluminum standard solution is handled as follows respectively: draw 100 μ L aluminum standard solutions in the color comparison tube that 5mL is with a scale, add 300 μ L chrome azurol S solution, 100 μ L polyoxyethylene nonylphenol ether solution, 200 μ L bromide sixteen alkyls pyridine solution and 300 μ L ethylenediamine-hydrochloride buffers respectively, 2.5mL scale is settled to distilled water, shake up after placing 15min, with UV2300 twin-beam ultraviolet scene photometer, under 620nm wavelength, measure absorbance; Then take absorbance as ordinate, in aluminium titer, the quality of aluminium is horizontal ordinate, draws the working curve of series aluminum titer as shown in Figure 1; The regression equation of this typical curve is:
y=0.13038x-0.0101,R
2=0.9994。
Make blank assay simultaneously, make reference with blank;
Step 3: take the uniform tested surface goods of 10g as sample, dries 3 ~ 6h, grinds at 100 ± 3 DEG C of temperature, crosses 40 mesh sieves, makes butt sample, is kept in dry ground glass stoppered bottle for subsequent use;
Step 4: take 0.1g(and be accurate to 0.0001g) butt sample, be placed in 50mL beaker, add 18mL distilled water and 2.0mL acid solution, beaker is placed in ultrasonic generator, continual ultrasonic ripple extracts 5 ~ 30min, filters extract, obtains sample preparation liquid;
Acid solution adopt volumetric concentration be 10% hydrochloric acid solution, volumetric concentration be 10% sulfuric acid solution or volumetric concentration be the salpeter solution of 10%.
Step 5: get 100 μ L sample preparation liquid in 5mL color comparison tube with a scale, add 300 μ L chrome azurol S solution, 100 μ L polyoxyethylene nonylphenol ether solution, 200 μ L bromide sixteen alkyls pyridine solution and 300 μ L ethylenediamine-hydrochloride buffers respectively, 2.5mL scale is settled to distilled water, shake up placement 15 ~ 120min, with UV2300 twin-beam ultraviolet scene photometer, under 620nm wavelength, measure absorbance, make blank assay simultaneously;
Step 6: according to the absorbance of the sample preparation liquid that step 5 records, finds the quality of the aluminium that this absorbance is corresponding, is calculated as follows the aluminium content X in tested surface goods from the working curve of the series aluminum titer of step 2 drafting:
In formula: X represents the aluminium content in sample, unit mg/kg; C
1represent the quality of the aluminium corresponding to absorbance of the sample preparation liquid that step 5 records, unit μ g; C
0represent the quality of aluminium in sample blank liquid, unit μ g; M represents sample mass, unit g; V
1represent the cumulative volume of sample preparation liquid in step 4, Unit/mL; V
2represent the volume of liquid after constant volume in step 5, Unit/mL.
Below rapid assay methods of the present invention is verified:
1) ultrasound wave extraction time
Prepare six kinds of sample preparation liquid by above-mentioned steps 3 and step 4, the ultrasound wave extraction time in these six kinds of sample preparation liquid preparation process is respectively 5min, 10min, 15min, 20min, 25min or 30min; Get six 5mL color comparison tubes with a scale, often prop up color comparison tube with a scale and add a kind of sample preparation liquid 100 μ L, and then all add by the obtained chrome azurol S solution 300 μ L of step 1 method, polyoxyethylene nonylphenol ether solution 100 μ L, bromide sixteen alkyls pyridine solution 200 μ L and ethylenediamine-hydrochloride buffer 300 μ L often propping up in color comparison tube with a scale, distilled water is settled to 2.5mL, shake up after placing 15min, with UV2300 twin-beam ultraviolet scene photometer, under 620nm wavelength, measure absorbance, make blank assay simultaneously.Analysis result is as shown in table 1.
Table 1 different ultrasound wave extraction time is on the impact of sample absorbance
Table 1 shows: ultrasound wave extraction time is in the interval of 5min to 30min, the absorbance no significant difference of sample, illustrates in the inventive method step 4, when sample being carried out to the ultrasound wave extraction of 5 ~ 30min, can not affect the absorbance of sample, this time interval is reasonable.In practical work process, in order to shorten the sample cycle, save the energy, in time interval, ultrasound wave extraction time can be selected arbitrarily.
2) Precision Experiment
The mass body volume concentrations that accurate aspiration step 2 is prepared be the aluminum standard solution 100 μ L of 2.0 μ g/mL in the color comparison tube that 5.0mL is with a scale, measure as stated above.METHOD FOR CONTINUOUS DETERMINATION 6 times, absorbance is respectively: 0.245,0.238,0.252,0.242,0.241,0.247, and precision is estimated with its relative standard deviation RSD, and RSD is 2.03%.Experimental result shows, uses the inventive method to measure the absorbance of same sample, and the change of absorbance is little, and stability is better, and the method can meet the testing requirement in laboratory.
3) repeated experiment
Butt sample is prepared by the method for step 3, take 6 parts, this butt sample, six parts of sample preparation liquid are made by the method for step 4, as stated above these six parts of sample preparation liquid are measured respectively, the content recording this six increments product aluminium is respectively: 293.56mg/kg, 294.98mg/kg, 298.78mg/kg, 291.25mg/kg, 283.77mg/kg, 293.90mg/kg, repeatability is estimated with its RSD, and RSD is 1.72%.Experimental result shows, measures the content of aluminium in same sample by the inventive method, and results change is little, and the method has good reappearance.
4) stability experiment
Take " 3) repeated experiment " middle six parts, the butt sample prepared, six parts of sample preparation liquid are made by the method for step 4, as stated above after process, respectively shake up place 15min, 30min, 45min, 60min, 90min, 120min measure, the absorbance recorded is respectively 0.235,0.238,0.233,0.223,0.210,0.198.Experimental result shows, sample preparation liquid is stable in 45min, and measure best at 15min ~ 45min, absorbance prolongation in time diminishes gradually.
5) recovery experiment
Take " 3) repeated experiment " middle 6 parts, the butt sample prepared, wherein add the aluminium standard substance of 25mg/kg in two parts of butt samples respectively, 50mg/kg is added respectively in other two parts of butt samples, the aluminium standard substance of 100mg/kg is added respectively in remaining two parts of butt samples, then by the obtained six parts of sample preparation liquid of the method for step 4, these six parts of sample preparation liquid are measured respectively, and calculates the recovery, the results are shown in Table 2.
Table 2 recovery experimental result
Table 2 shows: after adopting the inventive method processing sample, in sample, the recovery of aluminium is 82.08 ~ 97.02%.Experimental result shows, uses the content of aluminium in the inventive method working sample, and result reappearance is better, and the method has good accuracy and reliability, can meet the testing requirement in laboratory.
By Precision Experiment, repeated experiment, stability experiment and recovery experimental verification, result shows that method for quick of the present invention has stability and reliability well.
The pH value of the mixed liquor formed after sample preparation liquid, chrome azurol S solution, polyoxyethylene nonylphenol ether solution, bromide sixteen alkyls pyridine solution and ethylenediamine-hydrochloride buffer mixing is still that 6.7 ~ 7.0(measures the pH of this mixed liquor by experiment also in 6.7 ~ 7.0 scopes, the effect of ethylenediamine-hydrochloride buffer is exactly regulate solution ph), aluminium reacts with chrome azurol S and generates blue quaternary mixed micelle, colorimetric estimation under the existence of polyglycol octyl group phenylate (OP) and bromide sixteen alkyls pyridine (CPB).
embodiment 1
Take 0.1g chrome azurol S, be dissolved in 100mL ethanolic solution (1+1), mixing, obtains the chrome azurol S solution that mass body volume concentrations is 1g/L; 3.0mL polyoxyethylene nonylphenol ether is dissolved in 100mL water, is made into polyoxyethylene nonylphenol ether solution; Take 0.6g bromide sixteen alkyls pyridine, be dissolved in 30mL ethanol (φ (C
2h
5oH)=95%) in, be diluted with water to 200mL, obtain bromide sixteen alkyls pyridine solution; Get anhydrous ethylenediamine 100mL, add pure water 200mL, slowly adding 190mL mass body volume concentrations after cooling is the hydrochloric acid of 1.19g/mL, stirs evenly, and adjust ph is 6.7 ~ 7.0, obtained ethylenediamine-hydrochloride buffer; Six kinds of aluminum standard solutions of 0.5 μ g/mL, 1.0 μ g/mL, 2.0 μ g/mL, 3.0 μ g/mL, 4.0 μ g/mL and 5.0 μ g/mL are respectively with the aluminium standard reserving solution preparation mass body volume concentrations of mass body volume concentrations 1.0mg/mL; Each aluminum standard solution is handled as follows respectively: draw 100 μ L aluminum standard solutions in the color comparison tube that 5mL is with a scale, add 300 μ L chrome azurol S solution, 100 μ L polyoxyethylene nonylphenol ether solution, 200 μ L bromide sixteen alkyls pyridine solution and 300 μ L ethylenediamine-hydrochloride buffers respectively, 2.5mL scale is settled to distilled water, shake up after placing 15min, with UV2300 twin-beam ultraviolet scene photometer, under 620nm wavelength, measure absorbance; Then take absorbance as ordinate, in aluminium titer, the quality of aluminium is horizontal ordinate, draws the working curve of series aluminum titer; Make blank assay simultaneously, make reference with blank; Take the uniform tested surface goods of 10g as sample, at 97 DEG C of temperature, dry 6h, grind, cross 40 mesh sieves, make butt sample; Take 0.1g(and be accurate to 0.0001g) butt sample, be placed in 50mL beaker, add 18mL distilled water and 2.0mL volumetric concentration is the sulfuric acid solution of 10%, beaker is placed in ultrasonic generator, continual ultrasonic ripple extracts 5min, filters extract, obtains sample preparation liquid; Get 100 μ L sample preparation liquid in 5mL color comparison tube with a scale, add 300 μ L chrome azurol S solution, 100 μ L polyoxyethylene nonylphenol ether solution, 200 μ L bromide sixteen alkyls pyridine solution and 300 μ L ethylenediamine-hydrochloride buffers respectively, 2.5mL is settled to distilled water, shake up and place 150min, with UV2300 twin-beam ultraviolet scene photometer, under 620nm wavelength, measure absorbance, make blank assay simultaneously; According to the absorbance of the sample preparation liquid recorded, find the quality of the aluminium that this absorbance is corresponding from the working curve of the series aluminum titer drawn, be calculated as follows the aluminium content X in tested surface goods:
In formula: X represents the aluminium content in sample, unit mg/kg; C
1represent the quality of the aluminium corresponding to absorbance of the sample preparation liquid recorded, unit μ g; C
0represent the quality of aluminium in sample blank liquid, unit μ g; M represents sample mass, unit g; V
1represent the cumulative volume of sample preparation liquid, Unit/mL; V
2the volume of liquid after expression sample preparation liquid constant volume, Unit/mL.
embodiment 2
Take 0.1g chrome azurol S, be dissolved in 100mL ethanolic solution (1+1), mixing, obtains the chrome azurol S solution that mass body volume concentrations is 1g/L; 3.0mL polyoxyethylene nonylphenol ether is dissolved in 100mL water, is made into polyoxyethylene nonylphenol ether solution; Take 0.6g bromide sixteen alkyls pyridine, be dissolved in 30mL ethanol (φ (C
2h
5oH)=95%) in, be diluted with water to 200mL, obtain bromide sixteen alkyls pyridine solution; Get anhydrous ethylenediamine 100mL, add pure water 200mL, slowly adding 190mL mass body volume concentrations after cooling is the hydrochloric acid of 1.19g/mL, stirs evenly, and is 6.7 ~ 7.0 by acidometer adjust ph, obtained ethylenediamine-hydrochloride buffer; Six kinds of aluminum standard solutions of 0.5 μ g/mL, 1.0 μ g/mL, 2.0 μ g/mL, 3.0 μ g/mL, 4.0 μ g/mL and 5.0 μ g/mL are respectively with the aluminium standard reserving solution preparation mass body volume concentrations of mass body volume concentrations 1.0mg/mL; Each aluminum standard solution is handled as follows respectively: draw 100 μ L aluminum standard solutions in the color comparison tube that 5mL is with a scale, add 300 μ L chrome azurol S solution, 100 μ L polyoxyethylene nonylphenol ether solution, 200 μ L bromide sixteen alkyls pyridine solution and 300 μ L ethylenediamine-hydrochloride buffers respectively, 2.5mL scale is settled to distilled water, shake up after placing 15min, with UV2300 twin-beam ultraviolet scene photometer, under 620nm wavelength, measure absorbance; Then take absorbance as ordinate, in aluminium titer, the quality of aluminium is horizontal ordinate, draws the working curve of series aluminum titer; Make blank assay simultaneously, make reference with blank; Take the uniform tested surface goods of 10g as sample, at 100 DEG C of temperature, dry 4.5h, grind, cross 40 mesh sieves, make butt sample; Take 0.1g(and be accurate to 0.0001g) butt sample, be placed in 50mL beaker, add 18mL distilled water and 2.0mL volumetric concentration is the hydrochloric acid solution of 10%, beaker is placed in ultrasonic generator, continual ultrasonic ripple extracts 30min, filters extract, obtains sample preparation liquid; Get 100 μ L sample preparation liquid in 5mL color comparison tube with a scale, add 300 μ L chrome azurol S solution, 100 μ L polyoxyethylene nonylphenol ether solution, 200 μ L bromide sixteen alkyls pyridine solution and 300 μ L ethylenediamine-hydrochloride buffers respectively, 2.5mL scale is settled to distilled water, shake up and place 120min, with UV2300 twin-beam ultraviolet scene photometer, under 620nm wavelength, measure absorbance, make blank assay simultaneously; According to the absorbance of the sample preparation liquid recorded, find the quality of the aluminium that this absorbance is corresponding from the working curve of the series aluminum titer drawn, be calculated as follows the aluminium content X in tested surface goods:
In formula: X represents the aluminium content in sample, unit mg/kg; C
1represent the quality of the aluminium corresponding to absorbance of the sample preparation liquid recorded, unit μ g; C
0represent the quality of aluminium in sample blank liquid, unit μ g; M represents sample mass, unit g; V
1represent the cumulative volume of sample preparation liquid, Unit/mL; V
2the volume of liquid after expression sample preparation liquid constant volume, Unit/mL.
embodiment 3
Take 0.1g chrome azurol S, be dissolved in 100mL ethanolic solution (1+1), mixing, obtains the chrome azurol S solution that mass body volume concentrations is 1g/L; 3.0mL polyoxyethylene nonylphenol ether is dissolved in 100mL water, is made into polyoxyethylene nonylphenol ether solution; Take 0.6g bromide sixteen alkyls pyridine (CPB), be dissolved in 30mL ethanol (φ (C
2h
5oH)=95%) in, be diluted with water to 200mL, obtain bromide sixteen alkyls pyridine solution; Get anhydrous ethylenediamine 100mL, add pure water 200mL, slowly adding 190mL mass body volume concentrations after cooling is the hydrochloric acid of 1.19g/mL, stirs evenly, and adjust ph is 6.7 ~ 7.0, obtained ethylenediamine-hydrochloride buffer; Six kinds of aluminum standard solutions of 0.5 μ g/mL, 1.0 μ g/mL, 2.0 μ g/mL, 3.0 μ g/mL, 4.0 μ g/mL and 5.0 μ g/mL are respectively with the aluminium standard reserving solution preparation mass body volume concentrations of mass body volume concentrations 1.0mg/mL; Each aluminum standard solution is handled as follows respectively: draw 100 μ L aluminum standard solutions in the color comparison tube that 5mL is with a scale, add 300 μ L chrome azurol S solution, 100 μ L polyoxyethylene nonylphenol ether solution, 200 μ L bromide sixteen alkyls pyridine solution and 300 μ L ethylenediamine-hydrochloride buffers respectively, 2.5mL scale is settled to distilled water, shake up after placing 15min, with UV2300 twin-beam ultraviolet scene photometer, under 620nm wavelength, measure absorbance; Then take absorbance as ordinate, in aluminium titer, the quality of aluminium is horizontal ordinate, draws the working curve of series aluminum titer; Make blank assay simultaneously, make reference with blank; Take the uniform tested surface goods of 10g as sample, at 103 DEG C of temperature, dry 3h, grind, cross 40 mesh sieves, make butt sample; Take 0.1g(and be accurate to 0.0001g) butt sample, be placed in 50mL beaker, add 18mL distilled water and 2.0mL volumetric concentration is the salpeter solution of 10%, beaker is placed in ultrasonic generator, continual ultrasonic ripple extracts 17.5min, filters extract, obtains sample preparation liquid; Get 100 μ L sample preparation liquid in 5mL color comparison tube with a scale, add 300 μ L chrome azurol S solution, 100 μ L polyoxyethylene nonylphenol ether solution, 200 μ L bromide sixteen alkyls pyridine solution and 300 μ L ethylenediamine-hydrochloride buffers respectively, 2.5mL scale is settled to distilled water, shake up and place 67.5min, with UV2300 twin-beam ultraviolet scene photometer, under 620nm wavelength, measure absorbance, make blank assay simultaneously; According to the absorbance of the sample preparation liquid recorded, find the quality of the aluminium that this absorbance is corresponding from the working curve of the series aluminum titer drawn, be calculated as follows the aluminium content X in tested surface goods:
In formula: X represents the aluminium content in sample, unit mg/kg; C
1represent the quality of the aluminium corresponding to absorbance of the sample preparation liquid recorded, unit μ g; C
0represent the quality of aluminium in sample blank liquid, unit μ g; M represents sample mass, unit g; V
1represent the cumulative volume of sample preparation liquid, Unit/mL; V
2the volume of liquid after expression sample preparation liquid constant volume, Unit/mL.
Claims (4)
1. the method for aluminium content in Fast Measurement flour-made food, it is characterized in that, this rapid assay methods is specifically carried out according to the following steps:
Step 1: the six kinds of aluminum standard solutions being respectively 0.5 μ g/mL, 1.0 μ g/mL, 2.0 μ g/mL, 3.0 μ g/mL, 4.0 μ g/mL and 5.0 μ g/mL with the aluminium standard reserving solution preparation mass body volume concentrations of mass body volume concentrations 1.0mg/mL; Each aluminum standard solution is handled as follows respectively: draw 100 μ L aluminum standard solutions in the color comparison tube that 5mL is with a scale, add 300 μ L chrome azurol S solution, 100 μ L polyoxyethylene nonylphenol ether solution, 200 μ L bromide sixteen alkyls pyridine solution and 300 μ L ethylenediamine-hydrochloride buffers respectively, distilled water is settled to 2.5mL, shake up after placing 15min, under 620nm wavelength, measure absorbance; Then take absorbance as ordinate, in aluminium titer, the quality of aluminium is horizontal ordinate, draws the working curve of series aluminum titer; Make blank assay simultaneously, make reference with blank;
Step 2: take the uniform tested surface goods of 10g as sample, dries 3 ~ 6h, grinds at 100 ± 3 DEG C of temperature, crosses 40 mesh sieves, makes butt sample;
Step 3: take 0.1g butt sample, be placed in 50mL beaker, adds 18mL distilled water and 2.0mL acid solution, and ultrasound wave extracts 5 ~ 30min, filters extract, obtains sample preparation liquid;
Step 4: get 100 μ L sample preparation liquid in 5mL color comparison tube with a scale, add 300 μ L chrome azurol S solution, 100 μ L polyoxyethylene nonylphenol ether solution, 200 μ L bromide sixteen alkyls pyridine solution and 300 μ L ethylenediamine-hydrochloride buffers respectively, 2.5mL scale is settled to distilled water, shake up placement 15 ~ 120min, with UV2300 twin-beam ultraviolet spectrophotometer, under 620nm wavelength, measure absorbance, make blank assay simultaneously;
Step 5: according to the absorbance of the sample preparation liquid that step 4 records, finds the quality of the aluminium that this absorbance is corresponding, is calculated as follows the aluminium content X in tested surface goods from the working curve of the series aluminum titer of step 1 drafting:
In formula: X represents the aluminium content in sample, unit mg/kg; C
1represent the absorbance of the sample preparation liquid recorded according to step 4, find the quality of the aluminium that this absorbance is corresponding from the working curve of the series aluminum titer of step 1 drafting, unit μ g; C
0represent the quality of aluminium in sample blank liquid, unit μ g; M represents the quality of butt sample in step 3, unit g; V
1represent the cumulative volume of sample preparation liquid in step 3, Unit/mL; V
2represent in step 4 volume measuring absorbance time institute sample thief and prepare liquid, Unit/mL.
2. the method for aluminium content in Fast Measurement flour-made food according to claim 1, is characterized in that, reagent used in described step 1 and step 4:
Take 0.1g chrome azurol S, be dissolved in 100mL ethanolic solution (1+1), mixing, obtains the chrome azurol S solution that mass body volume concentrations is 1g/L;
3.0mL polyoxyethylene nonylphenol ether is dissolved in 100mL water, is made into polyoxyethylene nonylphenol ether solution;
Take 0.6g bromide sixteen alkyls pyridine, be dissolved in 30mL ethanol, be diluted with water to 200mL, obtain bromide sixteen alkyls pyridine solution;
Get anhydrous ethylenediamine 100mL, add pure water 200mL, adding 190mL mass body volume concentrations after cooling is the hydrochloric acid of 1.19g/mL, stirs evenly, and adjust ph is 6.7 ~ 7.0, obtained ethylenediamine-hydrochloride buffer.
3. the method for aluminium content in Fast Measurement flour-made food according to claim 1, it is characterized in that, the regression equation of the working curve drawn in described step 1 is:
y=0.13038x-0.0101,R
2=0.9994。
4. the method for aluminium content in Fast Measurement flour-made food according to claim 1, is characterized in that, the acid solution in described step 3 adopt volumetric concentration be 10% hydrochloric acid solution, volumetric concentration be 10% sulfuric acid solution or volumetric concentration be the salpeter solution of 10%.
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| CN103994981B (en) * | 2014-04-28 | 2016-08-31 | 中国农业科学院兰州畜牧与兽药研究所 | A kind of method of aluminium composition in quick mensuration bee product |
| CN103994980B (en) * | 2014-04-28 | 2016-06-29 | 中国农业科学院兰州畜牧与兽药研究所 | A kind of alizarin red S chelating reaction-spectrophotometry measures the method for aluminium composition |
| CN105738323B (en) * | 2016-02-26 | 2018-08-28 | 长春美泰仪器有限公司 | The detection method and field quick detection instrument of the food additives containing aluminium in a kind of Flour product |
| CN105973880B (en) * | 2016-04-25 | 2019-02-12 | 天津科技大学 | The instant test paper and its application method of a kind of rapid evaluation aluminum in food constituent content and application |
| CN106680210A (en) * | 2016-12-09 | 2017-05-17 | 防城港市质量技术监督局 | Kit for detecting content of aluminum in food |
| CN108333125A (en) * | 2017-12-04 | 2018-07-27 | 上海仪电科学仪器股份有限公司 | A kind of Chrome azurol s colorimetry measurement aluminium ion method |
| CN108037219A (en) * | 2018-01-24 | 2018-05-15 | 辽宁大学 | A kind of method of aluminium content in high effective liquid chromatography for measuring parched food |
| US10794883B2 (en) * | 2019-02-15 | 2020-10-06 | Hach Company | Colorimetric detection of aluminum in an aqueous sample |
| CN110243771A (en) * | 2019-06-28 | 2019-09-17 | 百杰瑞(荆门)新材料有限公司 | The detection method of aluminium content in a kind of lithium fluoride raw material |
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