CN108037219A - A kind of method of aluminium content in high effective liquid chromatography for measuring parched food - Google Patents
A kind of method of aluminium content in high effective liquid chromatography for measuring parched food Download PDFInfo
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- CN108037219A CN108037219A CN201810066527.2A CN201810066527A CN108037219A CN 108037219 A CN108037219 A CN 108037219A CN 201810066527 A CN201810066527 A CN 201810066527A CN 108037219 A CN108037219 A CN 108037219A
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Abstract
The present invention relates to a kind of method of aluminium content in high effective liquid chromatography for measuring parched food.Standard curve is drawn first with the detection reagent of various concentrations proportioning, obtains equation of linear regression；Then sample sheared, dissolved, filtration treatment, then pre-column derivatization is carried out with sample, aluminium content in sample is calculated according to regression curve equation.Advantage is：This method operation is fast and convenient, and testing result is accurate, and reagent is cheap, easy to promote.
Description
Technical field
The invention belongs to Food Quality and Safety detection field, and in particular to a kind of quantitatively to detect aluminium content in parched food
Method.
Background technology
Aluminium is largely formed in the bodies of aminal and plant with natural environment, and is widely used in the daily life of the mankind,
Such as food additives, water treatment agent, gastric antiacids thing etc..Enjoyed due to superelevation nutritive value in the nut roasted seeds and nuts that people like
Aluminum-containing additive is usually added, prevents the moisture absorption, so as to keep the high-quality mouthfeel of roasted seeds and nuts.But also there is substantial amounts of research to show, when
When the concentration of aluminium is excessive in human body, aluminium can produce chronic toxicity and jeopardize health.Excessive aluminium intake can influence brain
Memory function causes senile dementia.Meanwhile a large amount of losses that excessive aluminium also results in internal calcium are taken in, trigger rickets.
Therefore the intake of aluminium content is necessary in control roasted seeds and nuts.What China promulgated《Food additives use sanitary standard》Regulation：Ammonium
Alum and potassium alum can be used for aquatic products, fried food (including fried class nut and roasted seeds and nuts), yeast powder, dilated food, but most
Residual quantity wants≤100mg/kg afterwards.
At present, domestic related measure parched food aluminium content has multiple standards method, mainly there is spectrophotometer method, atom
Absorption spectrometry, flame atomic absorption spectrometry, graphite furnace atomic absorption spectrometry, inductively coupled plasma mass spectrometry.But
Above-mentioned several method all more or less there are some it is obvious the shortcomings that.Wherein spectrophotometer method is highly prone in detection process
The acid-base value of the influence of some extraneous factors, such as colour temp, developing time and solution.And need to match somebody with somebody in measurement process
A series of reagents are made, its processing can affect environment；And atomic absorption spectrography (AAS) be although capable of detecting when it is a variety of
Trace element, but it limits its application in terms of aluminum content tests since big and safety problem etc. is lost in critical component；
Flame atomic absorption spectrometry needs to use various flammability hazard gases in continuous mode, and therefore, the method lacks certain peace
Quan Xing；Graphite furnace atomic absorption spectrometry easily causes the reduction of graphite tube lifetime when measuring aluminium content；Inductively coupled plasma
Although mass spectrography analytical precision is high, operation is cumbersome.Therefore, it is a kind of fast and convenient there is an urgent need to establish, accurate easily behaviour
The method of aluminium content in the measure roasted seeds and nuts of work.
The content of the invention
In order to solve the above-mentioned technical problem, the object of the present invention is to provide a kind of fast and convenient, can accurate quantitative analysis detection fry
The method of goods Aluminum Content in Food, this method is simple, convenient, reagent and of low cost, and testing result is accurate, sensitivity
Height, easy to promote.
The technical solution adopted by the present invention is：A kind of method of aluminium content in high effective liquid chromatography for measuring parched food,
Include the following steps：
1) standard curve is drawn, obtains equation of linear regression；
2) sample to be tested is handled：It is 0.5-5g samples to be tested to weigh dry weight, is put into after fully crushing in beaker, adds distillation
Water 10-15mL, is placed in Ultrasound Instrument progress ultrasound 30min by beaker, stands 15min, cool down, and first with filter paper coarse filtration 3 times, then uses
0.22 μm of membrane filtration 1 time, filtrate is transferred in the volumetric flask of 25mL, is diluted to graduation mark with distilled water, and shake up quiet
Put；
3) sample to be tested 1-5ml is taken in 10ml volumetric flasks, and it is molten to sequentially add 8-hydroxyquinoline solution, BES solution and SDS
Each 0.5mL of liquid, shakes, static 10min, scale is settled to distilled water；Peak area is detected with high performance liquid chromatograph, according to line
The content of aluminium in property regression equation calculation sample to be tested.
The method of aluminium content in a kind of above-mentioned high effective liquid chromatography for measuring parched food, step 1) are specially：Measure
0.5mL-5mL aluminum standard solutions sequentially add 8-hydroxyquinoline solution, BES solution (double (the 2- hydroxyls of N, N- in 10mL volumetric flasks
Ethyl) -2-aminoethanesulfonic acid solution), SDS solution (sodium dodecyl sulfate solution) each 0.5mL, shakes, static 10min, uses
Distilled water is settled to scale, detects peak area with high performance liquid chromatograph, draws standard curve, obtains equation of linear regression.
The method of aluminium content in a kind of above-mentioned high effective liquid chromatography for measuring parched food, high performance liquid chromatograph detection
Condition be：Chromatographic column：InertSustain C18 columns (5 μm, 250mmX4.6mm)；Mobile phase：8-hydroxyquinoline acetonitrile is molten
Liquid-SDS (30:70, v/v)；Flow velocity：1.0ml/min；Excitation wavelength：370nm, launch wavelength：516nm；Column temperature：30℃；Sample introduction
Amount：20μL.
The method of aluminium content, 8-hydroxyquinoline solution concentration in a kind of above-mentioned high effective liquid chromatography for measuring parched food
For 20mmol/l；BES solution concentrations are 2.5mol/l；SDS solution concentrations are 0.32mol/l.
The method of aluminium content in a kind of above-mentioned high effective liquid chromatography for measuring parched food, in step 1), the line
Property regression equation is：Y=12.385x-95.05, wherein x are Al3+Concentration, unit is μ g/ml；Y is absorption peak area.
The beneficial effects of the invention are as follows：
1) method of the invention, easy to operate quick, testing result is accurate, high sensitivity, and selectivity is good.
2) method of the invention, the main derivative using aluminium and 8-hydroxyquinoline have fluorescent absorption, can be in efficient liquid
Detected on the fluorescence detector of chromatography, meanwhile, good linear relationship is presented with absworption peak in aluminium ion concentration, so as to calculate
The content of aluminium in roasted seeds and nuts.Method is easy to operate, and excessive processing is not required in sample, and reagent is conveniently easy to get, while high-efficient liquid phase color
It is accurate to compose testing result, it is sensitive.
3) when detecting sample, first sample is sheared, is dissolved, filtration treatment, then, by sample and 8-hydroxyquinoline shape
Into derivative, pre-column derivatization is carried out, so that aluminium ion in measure parched food.
The present invention is a kind of simple, accurately and rapidly analysis method, is with a wide range of applications, can be used for quantitative
Detect aluminium content in roasted seeds and nuts sample.
Embodiment
Embodiment 1 detects aluminium content in sunflower seed
1st, standard curve is drawn
The Al that concentration is 200 μ g/mL is measured respectively3+Standard solution 0.5mL, 1.0mL, 1.5mL, 2.0mL, 2.5mL, in
In 10mL volumetric flasks, 0.5ml 8-hydroxyquinolines solution (20mmol/l) is sequentially added, 0.5ml BES solution (2.5mol/l),
0.5mL SDS solution (0.32mol/l), shakes, static 10min, makes it be sufficiently mixed derivatization, and quarter is settled to distilled water
Degree, rocks mixing up and down.Peak area is detected with high performance liquid chromatograph, draws standard curve, obtains equation of linear regression.
High performance liquid chromatograph detection condition be：Chromatographic column：InertSustain C18 columns (5 μm,
250mmX4.6mm)；Mobile phase：8-hydroxyquinoline acetonitrile solution-SDS (30:70, v/v)；Flow velocity：1.0ml/min；Excitation wave
It is long：370nm, launch wavelength：516nm；Column temperature：30℃；Sample size：20μL.
Absworption peak is measured in 370nm high performance liquid chromatography, gained equation of linear regression is y=12.385x-95.05 (x
For Al3+Concentration, unit is μ g/ml；Y is to absorb peak area, r=0.9996).
2nd, sample to be tested is handled
4g melon seeds (sample 1,2,3,4 and 5) are weighed respectively, are put into after shredding in 5 beakers, and are marked, and are added into beaker
Enter 10mL distilled water, 5 beakers are placed in Ultrasound Instrument and carry out ultrasound 30min.Beaker is taken out afterwards, is stood 15min, is treated that its is cold
But after, first with filter paper coarse filtration 3 times, then with 0.22 μm of membrane filtration 1 time, filtrate is transferred in the volumetric flask of 25mL, with distillation
Water is diluted to graduation mark, and shakes up standing.
3rd, the measure of detected sample
Sample to be tested 2.5ml is taken in 10ml volumetric flasks, sequentially adds 0.5ml 8-hydroxyquinolines solution (20mmol/l),
0.5ml BES solution (2.5mol/l), 0.5ml SDS solution (0.32mol/l) shake, and static 10min is sufficiently mixed it to spread out
Biochemistry, is settled to scale with distilled water, rocks mixing up and down, with high performance liquid chromatography detection peak area.
High performance liquid chromatograph detection condition be：Chromatographic column：InertSustain C18 columns (5 μm,
250mmX4.6mm)；Mobile phase：8-hydroxyquinoline acetonitrile solution-SDS (30:70, v/v)；Flow velocity：1.0ml/min；Excitation wave
It is long：370nm, launch wavelength：516nm；Column temperature：30℃；Sample size：20μL.
Absworption peak is measured in 370nm high performance liquid chromatography, is y=12.385x-95.05 according to equation of linear regression, meter
Calculate the content of aluminium in sample.
The concentration for measuring aluminium in the extracting solution of sample 4 is 51.13 μ g/mL, and the concentration of aluminium in the melon seeds is understood by calculating
For 319mg/kg, aluminium is not detected in remaining 4 sample (sample 1,2,3,5).
Sample 1,2,3,4 and 5 is detected by the inductively coupled plasma emission spectrography of the prior art, will be tied
Fruit is compared, and the results are shown in Table 1.
Aluminium content in 5 groups of samples in 1 embodiment of the present invention 1 of table
By table 1 as it can be seen that with the aluminium content that the method for the present invention measures with being surveyed using inductively coupled plasma emission spectrography
Fixed aluminium content result is coincide, and illustrates that this method result is accurate, reliable.
4th, recovery of standard addition is tested
Two parts of identical samples are taken, a copy of it adds the alum standard solution that C marks 40 μ g/mL, another is not added with.By adding
The peak area substitution standard curve for entering standard substance understands that its concentration C 1 is 87.47 μ g/mL, and the concentration C 2 of sample is 51.13 μ
G/mL, according to sample recovery rate formula：C1-C2/C mark calculate sample recovery rate be 90.85%.
It these are only the specific embodiment of the present invention, be not intended to limit the invention, for those skilled in the art
For member, the invention may be variously modified and varied.Any modification within the spirit and principles of the invention, being made,
Equivalent substitution, improvement etc., should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of method of aluminium content in high effective liquid chromatography for measuring parched food, it is characterised in that：Include the following steps：
1) standard curve is drawn, obtains equation of linear regression；
2) sample to be tested is handled：0.5-5g samples to be tested are weighed, are put into after fully crushing in beaker, add distilled water 10-15mL,
Beaker is placed in Ultrasound Instrument progress ultrasound 30min, 15min is stood, cools down, first with filter paper coarse filtration 3 times, then with 0.22 μm of filter
Membrane filtration 1 time, filtrate is transferred in the volumetric flask of 25mL, is diluted to graduation mark with distilled water, and shake up standing；
3) sample to be tested 1-5ml is taken in 10ml volumetric flasks, and it is each to sequentially add 8-hydroxyquinoline solution, BES solution and SDS solution
0.5mL, shakes, static 10min, scale is settled to distilled water；Peak area is detected with high performance liquid chromatograph, is returned according to linear
Return the content of aluminium in equation calculation sample to be tested.
2. the method for aluminium content, its feature in a kind of high effective liquid chromatography for measuring parched food according to claim 1
It is：Step 1) is specially：0.5mL-5mL aluminum standard solutions are measured in 10mL volumetric flasks, it is molten to sequentially add 8-hydroxyquinoline
Liquid, BES solution, each 0.5mL of SDS solution, shakes, static 10min, is settled to scale with distilled water, uses high performance liquid chromatograph
Peak area is detected, draws standard curve, obtains equation of linear regression.
3. the method for aluminium content in a kind of high effective liquid chromatography for measuring parched food according to claim 1 or 2, it is special
Sign is：High performance liquid chromatograph detection condition be：Chromatographic column：InertSustain C18 columns；Mobile phase：8-hydroxyquinoline
Acetonitrile solution-SDS；Flow velocity：1.0ml/min；Excitation wavelength：370nm, launch wavelength：516nm；Column temperature：30℃；Sample size：20
μL。
4. the method for aluminium content, its feature in a kind of high effective liquid chromatography for measuring parched food according to claim 3
It is：The chromatographic column is：InertSustain C18 columns, 5 μm, 250mm × 4.6mm.
5. the method for aluminium content, its feature in a kind of high effective liquid chromatography for measuring parched food according to claim 3
It is：By volume, 8-hydroxyquinoline acetonitrile solution:SDS=30:70.
6. the method for aluminium content in a kind of high effective liquid chromatography for measuring parched food according to claim 1 or 2, it is special
Sign is：8-hydroxyquinoline solution concentration is 20mmol/l；BES solution concentrations are 2.5mol/l；SDS solution concentrations are
0.32mol/l。
7. the method for aluminium content in a kind of high effective liquid chromatography for measuring parched food according to claim 1 or 2, it is special
Sign is：In step 1), the equation of linear regression is：Y=12.385x-95.05, wherein x are Al3+Concentration, unit is
μg/ml；Y is absorption peak area.
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Citations (6)
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| JPH0354458A (en) * | 1989-07-21 | 1991-03-08 | Shimadzu Corp | Analysis of metallic ion |
| CN102539606A (en) * | 2011-12-31 | 2012-07-04 | 中国水产科学研究院黄海水产研究所 | Determination method of trivalent aluminum in aquatic product and product thereof |
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2018
- 2018-01-24 CN CN201810066527.2A patent/CN108037219A/en active Pending
Patent Citations (6)
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|---|---|---|---|---|
| JPH0354458A (en) * | 1989-07-21 | 1991-03-08 | Shimadzu Corp | Analysis of metallic ion |
| CN102539606A (en) * | 2011-12-31 | 2012-07-04 | 中国水产科学研究院黄海水产研究所 | Determination method of trivalent aluminum in aquatic product and product thereof |
| CN103411911A (en) * | 2013-08-16 | 2013-11-27 | 甘肃省商业科技研究所 | Method for quickly determining content of aluminum in flour-made foods |
| CN103487446A (en) * | 2013-09-26 | 2014-01-01 | 上海海洋大学 | Rapid detection method for alum additive in fried food based on dielectric property |
| CN104359881A (en) * | 2014-11-06 | 2015-02-18 | 沈阳化工大学 | Analysis method for content of aluminum in calcium preparation |
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| MARY T KELLY ET AL.: "Validation and evaluation of a high performance liquid chromatographic method for the determination of aluminium in wine", 《JOURNAL OF CHROMATOGRAPHY A》 * |
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