CN103743688A - Method for measuring content of magnesium in fruits - Google Patents
Method for measuring content of magnesium in fruits Download PDFInfo
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- CN103743688A CN103743688A CN201310745150.0A CN201310745150A CN103743688A CN 103743688 A CN103743688 A CN 103743688A CN 201310745150 A CN201310745150 A CN 201310745150A CN 103743688 A CN103743688 A CN 103743688A
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Abstract
The invention provides a method for measuring the content of magnesium in fruits. The method comprises the following steps: after digestive treatment of the fruits, measuring the content of magnesium in the fruits by a flame atomic absorption spectroscopy method under the optimum conditions that the incident light-absorbing wavelength is 285nm, the quantity of a releasing agent strontium liquor is 2mL, the flow of acetylene is 1.25L/min, and the height of a combustor is 7mm. The method is high in precision, visual, simple and good in operability.
Description
Technical field
The invention belongs to food inspection technical field, be specifically related to the assay method of content of magnesium in a kind of fruit.
Background technology
Magnesium is the trace element of needed by human, it is micro-the same with calcium, iron etc., participates in the health engineering of human body, and appropriate Mg supplementation can improve bone mineral content of material, improve bone strength, magnesium is stored in the foods such as vegetables, fruit, coarse food grain, beans, potato class more.
The mensuration of content of magnesium is all to use conventional certain methods at present, but the interference factor that existing assay method is subject to when measuring content of magnesium is more, is difficult for observing terminal, and measurement result error is larger.
Summary of the invention
The object of the present invention is to provide the assay method of content of magnesium in a kind of fruit.
For achieving the above object, the present invention has adopted following technical scheme.
This assay method comprises the following steps:
1) the edible part water of fruit is rinsed, after flushing, suck the moisture of edible part surface, then edible part is made to homogenate with homogenizer, by the mixed liquid dipping of nitric acid and the perchloric acid composition potpourri that spends the night to obtain for homogenate, potpourri is heated on electric hot plate homogenate digestion completely digestive juice;
2) after adding sub-boiling water in digestive juice, again heat, when being heated to just to emit Bai Yanhou to proceed in volumetric flask, then with sub-boiling water constant volume, obtain sample liquid;
3) deionized water for sample liquid (with reference to content range and the absorbance typical curve of magnesium in fruit) is diluted to obtain to test specimens, in dilution, in sample liquid, add strontium chloride aqueous solution, adopt atomic absorption spectrophotometer (AAS) to detect the absorbance of test specimens, then according to absorbance typical curve, obtain the magnesium density corresponding to absorbance of test specimens, according to magnesium density, calculate the content of magnesium in fruit.
In described mixed liquor, the volume ratio of nitric acid and perchloric acid is (4～5): (1～2).
The concentration of described nitric acid is 14.4～15.2mol/L, and the concentration of described perchloric acid is 11.7～12.0mol/L.
In described step 1), the temperature range of heating is 100～120 ℃.
The dosage of described strontium chloride aqueous solution is for being less than or equal to 3mL, and the strontium concentration of strontium chloride aqueous solution is 10mgmL
-1.
During detection, atomic absorption spectrophotometer (AAS) adopts 270～290nm lambda1-wavelength.
In described atomic absorption spectrophotometer (AAS), the height of burner is 6～7mm.
Flow 1.25～the 1.50L/min of acetylene in described atomic absorption spectrophotometer (AAS).
The method for production of described typical curve is: to filling, in the 50mL volumetric flask of 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL magnesium standard solution, to add respectively 2mL strontium concentration be 10mgmL
-1strontium chloride aqueous solution, then be settled to respectively 50mL and obtain standard sample, adopt the atomic absorption spectrophotometer (AAS) absorbance of examination criteria sample respectively, then draw the curve of magnesium density and absorbance, magnesium standard solution dilutes and obtains after magnesium is dissolved in hydrochloric acid, and the magnesium density of magnesium standard solution is 10.0 μ gmL
-1.
Described assay method specifically comprises the following steps:
1) the banana edible part water of 2～3 grams is rinsed, after flushing, suck the moisture of banana edible part surface, then banana edible part is made to homogenate with homogenizer, by 8～10 milliliters of mixed liquid dippings of nitric acid and perchloric acid composition potpourri that spends the night to obtain for 5mL homogenate, in mixed liquor, the volume ratio of nitric acid and perchloric acid is 4:1, within 30 minutes, makes homogenate digestion obtain digestive juice completely in potpourri on electric hot plate in 100 ℃ of heating;
2) after adding sub-boiling water in digestive juice, again heat, when being heated to just to emit Bai Yanhou to proceed in 250 milliliters of volumetric flasks, then with sub-boiling water constant volume, obtain sample liquid;
3) 5mL sample liquid being added in 50mL volumetric flask, is then 10mgmL to adding 2mL strontium concentration in described 50mL volumetric flask
-1strontium chloride aqueous solution, then with deionized water constant volume, obtain test specimens, adopt atomic absorption spectrophotometer (AAS) to detect the absorbance of test specimens, then according to absorbance typical curve, obtain the magnesium density corresponding to absorbance of test specimens, according to magnesium density, calculate the content of magnesium in banana, during detection, the lambda1-wavelength of atomic absorption spectrophotometer (AAS) is 285nm, and in atomic absorption spectrophotometer (AAS), the flow of acetylene is 1.25L/min, and in atomic absorption spectrophotometer (AAS), the height of burner is 7mm.
Beneficial effect of the present invention is embodied in:
The present invention carries out fruit after digestion process, adopts the content of magnesium in aas determination fruit, and Absolute analysis is highly sensitive, and has the advantages such as directly perceived, succinct, operability is good, can be used as the assay method of content of magnesium in fruit; Meanwhile, the present invention is without the observation of carrying out titration end-point, and disturbing factor is less, can overcome the larger deficiency of existing titration method measurement result error; In addition, the process that the present invention carries out digestion process to fruit sample is simple, and the reagent type that digestion process adds is few, has reduced the disturbing factor in measuring.
Accompanying drawing explanation
Fig. 1 is absorbance typical curve; Y=0.6695x+0.007, R
2=0.997.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
1.1 reagent, material and instrument:
Magnesium standard reserving solution (100 μ gmL
-1): accurately take simple metal magnesium 0.025g, be placed in 100mL beaker, cover surface plate, drip 5mL1molL from beaker mouth to beaker
-1dissolving with hydrochloric acid magnesium metal, then transfers to solution in 250mL volumetric flask, is diluted to scale with the hydrochloric acid that volume fraction is 1%, shakes up.
Magnesium standard solution (10.0 μ gmL
-1): accurately draw 10.0mL magnesium standard reserving solution in 100mL volumetric flask, be diluted with water to scale, shake up.
10mgmL
-1strontium solution: take 30.4g SrCl
26H
2o is soluble in water, then is diluted with water to 1000mL.
1+1 hydrochloric acid: 6mol/L hydrochloric acid.
SP-3803AA type atomic absorption spectrophotometer (AAS); Magnesium hollow cathode lamp; High purity acetylene; Air compressor; Volumetric flask 50mL7 props up, and 100mL2 props up; Pipette 5mL1 props up; The fresh banana of market sale.
1.2 experimental techniques:
That atomic absorption spectrography (AAS) has is highly sensitive, selectivity good, interference is few, and measures accurately, analyzes the features such as quick, easy and simple to handle.For the analysis of the magnesium in banana, only need, through suitably processing dilution, just can directly measure.While entering ethyne-air flame after test solution is atomized, metallic ion, by atomization, produces ground state atom steam.This steam can absorb the radiation energy of the ejection values line that respective metal element hollow cathode lamp emits, and its absorbing state is obeyed Beer law.By the absorbance recording, can on typical curve, find corresponding concentration, can try to achieve the content of magnesium in banana, its Absolute analysis sensitivity can reach 10
-9g.
In banana, except magnesium ion, also contain aluminium, sulfate, phosphate and silicate etc., they can suppress the atomization of magnesium, produce and disturb, and make to record Lower result.Add strontium ion to make interference inhibitor, can obtain correct result.
1.2.1 sample preparation: by banana peeling, after getting 2-3 gram of edible part water and rinsing 3 times, with gauze, absorb water, then chopping, and make homogenate (can store in plastic bottle, put in refrigerator and save backup) with homogenizer.
5 milliliters of homogenate are moved in high pin beaker, then to the mixed liquor (8～10 milliliters) that adds 14.4～15.2mol/L nitric acid and 11.7～12.0mol/L perchloric acid in high pin beaker, soaked overnight (nitric acid: the volume ratio of perchloric acid is 4:1), make digestion (solid content all disappears i.e. digestion completely) completely for 30 minutes in 100 ℃ of hot digestions next day on electric hot plate, then in high pin beaker, add again the sub-boiling water of 25mL, be heated to again move in 250 milliliters of volumetric flasks after Mao Baiyan, then use sub-boiling water constant volume, as sample.
1.2.2 the drafting of typical curve: accurately draw 0.00mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL10.0 μ gmL
-1magnesium standard solution, is placed in respectively 6 50mL volumetric flasks, adds 2mL10mgmL in every volumetric flask again
-1strontium solution, deionized water constant volume.Under selected instrumentation condition, take blank sample (containing 0.00mL magnesium standard solution) as reference zeroing, measure corresponding absorbance at every turn.Take content of magnesium as horizontal ordinate, absorbance is ordinate, drawing standard curve (referring to Fig. 1).
1.2.3 the mensuration of magnesium in sample: the 5mL sample of accurately drawing is placed in to 50mL volumetric flask, then adds 2mL10mgmL
-1strontium solution, finally with deionized water, be diluted to scale, shake up.By selected operating conditions, (lambda1-wavelength of described atomic absorption spectrophotometer (AAS) is 285nm, in atomic absorption spectrophotometer (AAS), the flow of acetylene is 1.25L/min, the height of burner is 7mm), the zeroing take blank sample as reference, then measure absorbance, by typical curve, found again the content of magnesium in sample, and by volume of sample, calculated the content of magnesium in sample.
1.2.4 the mensuration of the recovery: accurately absorption has recorded the sample 5mL of content of magnesium, is placed in 50mL volumetric flask, adds the magnesium standard solution (total magnesium amount should drop in the range of linearity of typical curve) of known quantity, then adds 2mL10mgmL
-1strontium solution, be diluted with water to scale, shake up.By described selected operating conditions, with blank sample, do reference and return to zero, measure absorbance, and by typical curve, found the content of magnesium.Then by following formula, calculate the recovery:
Magnesium amount × 100% of the recovery=(recording magnesium amount in total magnesium amount-sample)/add
The recovery is 95.7%～99.9%, and recovery standard deviation is 0.10%～2.46%, meets the requirement of the recovery, proves that the method is feasible, and simple to operate, can carry out mass detection, improves detection efficiency.
1.2.5 influence factor: lambda1-wavelength (nm), strontium solution addition (mL), acetylene flow (L/min
-1) and burner height (mm).
1) lambda1-wavelength
Get the clean volumetric flask of 2 50mL, with pipette, draw 5.0mL10.0 μ g/mL magnesium standard solution in one of them volumetric flask, then in two volumetric flasks, add 2mL10mgmL
-1strontium solution,, shakes up to scale with distilled water diluting.Take blank sample as reference is between 270～290nm, every 5nm, measure absorbance.Along with the increase of wavelength, absorbance also increases, but when wavelength is increased to 285nm, its absorbance reaches maximal value, and its maximum absorption wavelength is 285nm.Under normal circumstances, the light that should select the maximum absorption wavelength of measured matter is incident light, and sensitivity and the accuracy of measuring are like this high.
2) selection of strontium solution addition
Draw 6 parts of 5mL magnesium samples (referring to magnesium standard reserving solution), be placed in respectively 6 50mL volumetric flasks, add 1+1 hydrochloric acid 2mL in every bottle, then add respectively 10mgmL
-1strontium solution 0mL, 1mL, 2mL, 3mL, 4mL, 5mL, be diluted to scale with deionized water, shakes up.Take deionized water as reference, return to zero, measure the absorbance of each bottle of sample, make the relation curve of absorbance-strontium solution addition.When strontium solution addition is less than 3mL, absorbance increases along with the increase of addition, and when exceeding 3mL, absorbance is almost constant.
3) acetylene flow
Pipette magnesium standard solution 4.0mL in 100mL volumetric flask, add 4mL10mgmL
-1strontium solution, is diluted with water to scale, shakes up.The instructions of pressing atomic absorption spectrophotometer (AAS) starts instrument, wavelength is transferred to 285nm place, lamp current 3mA, spectral band-width 0.2nm.Acetylene-air flame is lighted in operation in accordance with regulations.Carry out the selection of following operating conditions:
The pressure (0.2MPa) and the flow that before mensuration, first mix up air, make atomizer in best spray pattern.Fixing acetylene pressure is 0.05Mpa, changes acetylene flow (1.0～2.0L/min), by blank reagent, does reference zeroing, carries out the measurement of above-mentioned magnesium solution absorbance.From test findings, can find out when acetylene flow is 1.25～1.50L/min, absorbance good stability and value are larger, so 1.25～1.50L/min is as acetylene flowrate optimization condition.
4) selection of burner height
Pipette 4.0mL magnesium standard solution in 100mL volumetric flask, add 4mL10mgmL
-1strontium solution, is diluted with water to scale, shakes up.The instructions of pressing atomic absorption spectrophotometer (AAS) starts instrument, wavelength is transferred to 285nm place, lamp current 3mA, spectral band-width 0.2nm.Acetylene-air flame is lighted in operation in accordance with regulations.Carry out the selection of following operating conditions:
Under the pressure and flow condition of selected air-acetylene, change burner height (3～7mm), to go blank sample to return to zero as reference, measure the absorbance of above-mentioned magnesium solution.When burner height is 6～7mm, good stability and absorbance are larger.So 6～7mm can be used as the burner height of mensuration.
By range analysis result, can draw top condition: incident extinction wavelength 285nm, strontium solution addition 2mL, acetylene flow 1.25L/min, the height 7mm of burner.In the homogenate of test banana, the content of magnesium is 17.38mg/100mL.
Claims (10)
1. an assay method for content of magnesium in fruit, is characterized in that: this assay method comprises the following steps:
1) the edible part water of fruit is rinsed, after flushing, suck the moisture of edible part surface, then edible part is made to homogenate with homogenizer, by the mixed liquid dipping of nitric acid and the perchloric acid composition potpourri that spends the night to obtain for homogenate, potpourri is heated on electric hot plate homogenate digestion completely digestive juice;
2) after adding sub-boiling water in digestive juice, again heat, when being heated to just to emit Bai Yanhou to proceed in volumetric flask, then with sub-boiling water constant volume, obtain sample liquid;
3) sample liquid is diluted to obtain to test specimens with deionized water, in dilution, in sample liquid, add strontium chloride aqueous solution, adopt atomic absorption spectrophotometer (AAS) to detect the absorbance of test specimens, then according to absorbance typical curve, obtain the magnesium density corresponding to absorbance of test specimens, according to magnesium density, calculate the content of magnesium in fruit.
2. the assay method of content of magnesium in a kind of fruit according to claim 1, is characterized in that: in described mixed liquor, the volume ratio of nitric acid and perchloric acid is (4～5): (1～2).
3. the assay method of content of magnesium in a kind of fruit according to claim 1, is characterized in that: the concentration of described nitric acid is 14.4～15.2mol/L, the concentration of described perchloric acid is 11.7～12.0mol/L.
4. the assay method of content of magnesium in a kind of fruit according to claim 1, is characterized in that: in described step 1), the temperature range of heating is 100～120 ℃.
5. the assay method of content of magnesium in a kind of fruit according to claim 1, is characterized in that: the dosage of described strontium chloride aqueous solution is for being less than or equal to 3mL, and the strontium concentration of strontium chloride aqueous solution is 10mgmL
-1.
6. the assay method of content of magnesium in a kind of fruit according to claim 1, is characterized in that: during detection, atomic absorption spectrophotometer (AAS) adopts 270～290nm lambda1-wavelength.
7. the assay method of content of magnesium in a kind of fruit according to claim 1, is characterized in that: in described atomic absorption spectrophotometer (AAS), the height of burner is 6～7mm.
8. the assay method of content of magnesium in a kind of fruit according to claim 1, is characterized in that: the flow 1.25～1.50L/min of acetylene in described atomic absorption spectrophotometer (AAS).
9. the assay method of content of magnesium in a kind of fruit according to claim 1, is characterized in that: the method for production of described typical curve is: to filling, in the 50mL volumetric flask of 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL magnesium standard solution, to add respectively 2mL strontium concentration be 10mgmL
-1strontium chloride aqueous solution, then be settled to respectively 50mL and obtain standard sample, adopt the atomic absorption spectrophotometer (AAS) absorbance of examination criteria sample respectively, then draw the curve of magnesium density and absorbance, magnesium standard solution dilutes and obtains after magnesium is dissolved in hydrochloric acid, and the magnesium density of magnesium standard solution is 10.0 μ gmL
-1.
10. the assay method of content of magnesium in a kind of fruit according to claim 1, is characterized in that: described assay method specifically comprises the following steps:
1) the banana edible part water of 2～3 grams is rinsed, after flushing, suck the moisture of banana edible part surface, then banana edible part is made to homogenate with homogenizer, by 8～10 milliliters of mixed liquid dippings of nitric acid and perchloric acid composition potpourri that spends the night to obtain for 5mL homogenate, in mixed liquor, the volume ratio of nitric acid and perchloric acid is 4:1, within 30 minutes, makes homogenate digestion obtain digestive juice completely in potpourri on electric hot plate in 100 ℃ of heating;
2) after adding sub-boiling water in digestive juice, again heat, when being heated to just to emit Bai Yanhou to proceed in 250 milliliters of volumetric flasks, then with sub-boiling water constant volume, obtain sample liquid;
3) 5mL sample liquid being added in 50mL volumetric flask, is then 10mgmL to adding 2mL strontium concentration in described 50mL volumetric flask
-1strontium chloride aqueous solution, then with deionized water constant volume, obtain test specimens, adopt atomic absorption spectrophotometer (AAS) to detect the absorbance of test specimens, then according to absorbance typical curve, obtain the magnesium density corresponding to absorbance of test specimens, according to magnesium density, calculate the content of magnesium in banana, during detection, the lambda1-wavelength of atomic absorption spectrophotometer (AAS) is 285nm, and in atomic absorption spectrophotometer (AAS), the flow of acetylene is 1.25L/min, and in atomic absorption spectrophotometer (AAS), the height of burner is 7mm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106442356A (en) * | 2016-09-30 | 2017-02-22 | 营口康辉石化有限公司 | Detection method of magnesium content in polymer film slices |
| CN107192707A (en) * | 2017-05-11 | 2017-09-22 | 金花企业(集团)股份有限公司西安金花制药厂 | Arsenic, cadmium, copper, mercury, the method for the Heavy Metallic Elements of lead five in Bionic tiger bone powder are determined simultaneously |
| CN109709050A (en) * | 2018-11-28 | 2019-05-03 | 广东中京环境监测有限公司 | A kind of detection method of metallic element |
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| CN103175802A (en) * | 2011-12-20 | 2013-06-26 | 四川科伦药物研究有限公司 | Method for determining content of magnesium element in hydroxyethyl starch injection preparation |
| CN103196858A (en) * | 2013-04-24 | 2013-07-10 | 吉林化工学院 | Atomic absorption spectrometry for determining element magnesium in polygonum cuspidatum |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103175802A (en) * | 2011-12-20 | 2013-06-26 | 四川科伦药物研究有限公司 | Method for determining content of magnesium element in hydroxyethyl starch injection preparation |
| CN103196858A (en) * | 2013-04-24 | 2013-07-10 | 吉林化工学院 | Atomic absorption spectrometry for determining element magnesium in polygonum cuspidatum |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106442356A (en) * | 2016-09-30 | 2017-02-22 | 营口康辉石化有限公司 | Detection method of magnesium content in polymer film slices |
| CN107192707A (en) * | 2017-05-11 | 2017-09-22 | 金花企业(集团)股份有限公司西安金花制药厂 | Arsenic, cadmium, copper, mercury, the method for the Heavy Metallic Elements of lead five in Bionic tiger bone powder are determined simultaneously |
| CN109709050A (en) * | 2018-11-28 | 2019-05-03 | 广东中京环境监测有限公司 | A kind of detection method of metallic element |
| CN109709050B (en) * | 2018-11-28 | 2021-06-08 | 广东中京环境监测有限公司 | Method for detecting metal elements |
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Application publication date: 20140423 |