CN110455731A - Composite phosphate detection method in a kind of meat products - Google Patents
Composite phosphate detection method in a kind of meat products Download PDFInfo
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- CN110455731A CN110455731A CN201910799701.9A CN201910799701A CN110455731A CN 110455731 A CN110455731 A CN 110455731A CN 201910799701 A CN201910799701 A CN 201910799701A CN 110455731 A CN110455731 A CN 110455731A
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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
Abstract
The invention discloses composite phosphate detection methods in a kind of meat products, including carrying out reagent configuration, Specification Curve of Increasing, sample measurement and calculating phosphate content in sample, the present invention is by prepare liquid under certain acidity, phosphate anion therein reacts to form yellow ternary heteropoly acid with metavanadic acid and molybdic acid, within the scope of a certain concentration, the absorbance and phosphorus content direct proportionality of yellow solution, with spectrophotometric quantitative analysis phosphorus content, composite phosphate detection method in the meat products that the present invention establishes, sensitivity and accuracy stable and with higher.
Description
Technical field:
The invention belongs to composite phosphate detection methods in composite phosphate detection technique field more particularly to a kind of meat products.
Background technique:
Occur in existing national standard composite phosphate detection method molybdenum blue color pipe colour developing it is unobvious, absorbance is small, sensitive
Low problem is spent, placing to hydroquinone solution can change colour for a period of time, and sodium sulfite solution also needs Extemporaneous, otherwise may make
Muddiness occurs for molybdenum blue solution, causes absorbance change.
The present invention selects low toxicity and composite phosphate in stable reducing agent measurement meat products, reaches good experiment effect
Fruit.
Summary of the invention:
In view of the above-mentioned problems, the technical problem to be solved in the present invention is to provide composite phosphate detection methods in a kind of meat products.
Composite phosphate detection method in a kind of meat products of the invention, comprising the following steps:
A. reagent configuration is carried out:
(1) vanadium ammonium molybdate solution:
A liquid: it weighs 25.0g ammonium molybdate and is dissolved in 400ml water；
B liquid: weighing 1.25g ammonium metavanadate and be dissolved in 300ml hot water, and 250ml nitric acid is added after cooling, cooling；
A liquid is slowly injected in b liquid under stiring, is diluted with water to 1L, mixes, stores in brown bottle；
(2) sodium hydroxide solution: the solution of mass concentration 10%；
(3) sulfuric acid solution: the solution of volume fraction 5%；
(4) phosphorus standard solution: 50ug/ml weighs the potassium dihydrogen phosphate (standard reagent) that 0.2195g dries 2h through 105 DEG C, uses water
It after dissolution, is transferred in 1L volumetric flask, 5ml sulfuric acid is added, is settled to scale with water after cooling；
(5) 2,4(or 2,6)-dinitrophenol dinitrophenolate indicator: the solution of mass concentration 0.2%；
B. Specification Curve of Increasing:
Pipette respectively 0.0 ml of phosphorus standard solution, 1.0 ml, 2.0 ml, 3.0 ml, 4.0ml, 5.0ml, 6.0ml, 8.0ml,
9.0ml is placed in 50ml volumetric flask, adds water to 15~20ml, sequentially adds 2,4-dinitrophenol dinitrophenolate indicator 2 drop, uses hydroxide
Sodium solution and sulfuric acid solution adjust PH to solution be just in it is yellowish, using zero pipe of standard curve as reference, 10.00ml vanadium molybdic acid is added
Ammonium salt solution adds distilled water to be diluted to scale, shakes up, and after static 30min, 2cm optical path ratio is used at spectrophotometer wavelength 440nm
Color ware is carried out colorimetric, is measured the absorbance of each standard solution, and draw standard with zero pipe solutions as controls conditioning instrumentation zero point
Curve；
C. sample measures:
Appropriate amount of sample is weighed, is placed in 150 ml stuffed conical flasks, 80 ml water of addition, 80 DEG C of ultrasonic extraction 30min, every
5min shaking is primary, is kept fixed and is mutually completely dispersed, after being cooled to room temperature, is settled in 100ml volumetric flask, shakes up, and filters, takes
Portion filtrate is at 4 DEG C, and 8000r/min is centrifuged 10min, and supernatant is spare, and supernatant 5ml is taken to be placed in 50ml volumetric flask, with
The zeroing of blank test solutions as controls is read absorbance and is drawn with standard liquid series with condition colour developing, colorimetric.
D. phosphate content in sample, calculation formula are calculated are as follows:
X= m1*v1*3.066*10-4 /m*v2, in formula:
X: phosphate content in sample, unit are gram every hectogram (%)；
m1: checked in by standard curve or regression equation calculate in Specimen Determination liquid the quality of phosphorus, unit be milligram (ug)；
v1: sample digestive juice constant volume total volume, unit are milliliter (mL)；
v2: the volume of measurement sample digestive juice, unit are milliliter (mL)；
M: the quality of sample, unit are gram (g)；
3.066: the conversion coefficient of phosphate (PO43-) and phosphorus (P).
The invention has the advantages that: the detection technique that the present invention establishes composite phosphate in meat products, stablizes and have higher
Sensitivity and accuracy substituted to quinhydrones and sodium sulfite, no using ammonium metavanadate, molybdic acid and ascorbic acid collective effect
Only low toxic and environment-friendly, and it is obvious to develop the color, and absorbance is big, high sensitivity, easy to operate；Reproducibility, accuracy and precision all compared with
It is good；Spectrophotometry measures the method for inspection of composite phosphate in meat products, and instrument and equipment is simple, and common lab can match
It sets.
Specific embodiment:
In order to make the objectives, technical solutions and advantages of the present invention clearer, this hair is described below by specific embodiment
It is bright.However, it should be understood that these descriptions are merely illustrative, and it is not intended to limit the scope of the invention.In addition, in following explanation
In, descriptions of well-known structures and technologies are omitted, so as not to unnecessarily obscure the concept of the present invention.
Composite phosphate detection method in a kind of meat products of the present embodiment, comprising the following steps:
A. reagent configuration is carried out:
(1) vanadium ammonium molybdate solution:
A liquid: it weighs 25.0g ammonium molybdate and is dissolved in 400ml water；
B liquid: weighing 1.25g ammonium metavanadate and be dissolved in 300ml hot water, and 250ml nitric acid is added after cooling, cooling；
A liquid is slowly injected in b liquid under stiring, is diluted with water to 1L, mixes, stores in brown bottle；
(2) sodium hydroxide solution: the solution of mass concentration 10%；
(3) sulfuric acid solution: the solution of volume fraction 5%；
(4) phosphorus standard solution: 50ug/ml weighs the potassium dihydrogen phosphate (standard reagent) that 0.2195g dries 2h through 105 DEG C, uses water
It after dissolution, is transferred in 1L volumetric flask, 5ml sulfuric acid is added, is settled to scale with water after cooling；
(5) 2,4(or 2,6)-dinitrophenol dinitrophenolate indicator: the solution of mass concentration 0.2%；
B. Specification Curve of Increasing:
Pipette respectively 0.0 ml of phosphorus standard solution, 1.0 ml, 2.0 ml, 3.0 ml, 4.0ml, 5.0ml, 6.0ml, 8.0ml,
9.0ml is placed in 50ml volumetric flask, adds water to 15~20ml, sequentially adds 2,4-dinitrophenol dinitrophenolate indicator 2 drop, uses hydroxide
Sodium solution and sulfuric acid solution adjust PH to solution be just in it is yellowish, using zero pipe of standard curve as reference, 10.00ml vanadium molybdic acid is added
Ammonium salt solution adds distilled water to be diluted to scale, shakes up, and after static 30min, 2cm optical path ratio is used at spectrophotometer wavelength 440nm
Color ware is carried out colorimetric, is measured the absorbance of each standard solution, and draw standard with zero pipe solutions as controls conditioning instrumentation zero point
Curve；
C. sample measures:
Appropriate amount of sample is weighed, is placed in 150 ml stuffed conical flasks, 80 ml water of addition, 80 DEG C of ultrasonic extraction 30min, every
5min shaking is primary, is kept fixed and is mutually completely dispersed, after being cooled to room temperature, is settled in 100ml volumetric flask, shakes up, and filters, takes
Portion filtrate is at 4 DEG C, and 8000r/min is centrifuged 10min, and supernatant is spare, and supernatant 5ml is taken to be placed in 50ml volumetric flask, with
The zeroing of blank test solutions as controls is read absorbance and is drawn with standard liquid series with condition colour developing, colorimetric.
D. phosphate content in sample, calculation formula are calculated are as follows:
X= m1*v1*3.066*10-4 /m*v2, in formula:
X: phosphate content in sample, unit are gram every hectogram (%)；
m1: checked in by standard curve or regression equation calculate in Specimen Determination liquid the quality of phosphorus, unit be milligram (ug)；
v1: sample digestive juice constant volume total volume, unit are milliliter (mL)；
v2: the volume of measurement sample digestive juice, unit are milliliter (mL)；
M: the quality of sample, unit are gram (g)；
3.066: the conversion coefficient of phosphate (PO43-) and phosphorus (P).
The method of the present invention principle: under certain acidity, phosphate anion therein reacts prepare liquid with metavanadic acid and molybdic acid
Form yellow ternary heteropoly acid.In a certain concentration range [ 1ug/mL~20ug/mL ], the absorbance and phosphorus content of yellow solution
Direct proportionality, with spectrophotometric quantitative analysis phosphorus content.
Embodiment 1:
Phosphorus standard curve series is done with this law, measurement result is shown in Table 1.
Table 1: the standard series that this method is surveyed
| Concentration c (ug) | 0.00 | 50.00 | 100.0 | 150.0 | 200.0 | 300.0 | 400.0 | 450.0 |
| Absorbance (A) | 0.000 | 0.068 | 0.135 | 0.207 | 0.276 | 0.413 | 0.542 | 0.610 |
Note: r=0.9999.
Embodiment 2:
National Standard Reference substance prawn (GWB10050) is weighed respectively, carries out sample detection according to this law, 6 measurements are averaged
Value is consistent with standard reference value, the results are shown in Table 2.
Table 2: the measurement result (n=6) of P elements in standard substance
Note: in upper table, laterally indicate that same sample has taken 6 groups of Duplicate Samples in number 1,2,3,4,5,6.
Embodiment 3:
It chooses authorized by state and carries out recovery testu as sample in standard quality control sample, add low, high 2 in every part of sample
The phosphorus standard solution of a different content is measured 2 its contents respectively by this law and calculates the rate of recovery, the results are shown in Table 3.
Table 3: sample recovery of standard addition test
Thus table finds out average recovery rate between the % of 94 % ~ 97, meets analysis method requirement.
In conclusion accuracy height the experimental results showed that, is agreed in precision using the method for the present invention by 3 two groups of table 2 and table,
Recovery of standard addition is average between the % of 94 % ~ 97, it was demonstrated that the method for the present invention science is feasible.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (1)
1. composite phosphate detection method in a kind of meat products, it is characterised in that: the following steps are included:
A. reagent configuration is carried out:
(1) vanadium ammonium molybdate solution:
A liquid: it weighs 25.0g ammonium molybdate and is dissolved in 400ml water；
B liquid: weighing 1.25g ammonium metavanadate and be dissolved in 300ml hot water, and 250ml nitric acid is added after cooling, cooling；
A liquid is slowly injected in b liquid under stiring, is diluted with water to 1L, mixes, stores in brown bottle；
(2) sodium hydroxide solution: the solution of mass concentration 10%；
(3) sulfuric acid solution: the solution of volume fraction 5%；
(4) phosphorus standard solution: 50ug/ml weighs the potassium dihydrogen phosphate (standard reagent) that 0.2195g dries 2h through 105 DEG C or so,
It after being dissolved with water, is transferred in 1L volumetric flask, 5ml sulfuric acid is added, is settled to scale with water after cooling；
(5) 2,4(or 2,6)-dinitrophenol dinitrophenolate indicator: the solution of mass concentration 0.2%；
B. Specification Curve of Increasing:
Pipette respectively 0.0 ml of phosphorus standard solution, 1.0 ml, 2.0 ml, 3.0 ml, 4.0ml, 5.0ml, 6.0ml, 8.0ml,
9.0ml is placed in 50ml volumetric flask, adds water to 15~20ml, sequentially adds 2,4-dinitrophenol dinitrophenolate indicator 2 drop, uses hydroxide
Sodium solution and sulfuric acid solution adjust PH to solution be just in it is yellowish, using zero pipe of standard curve as reference, 10.00ml vanadium molybdic acid is added
Ammonium salt solution adds distilled water to be diluted to scale, shakes up, after static 30min or so, with 2cm light at spectrophotometer wavelength 440nm
Diameter cuvette is carried out colorimetric, is measured the absorbance of each standard solution, and draw with zero pipe solutions as controls conditioning instrumentation zero point
Standard curve；
C. sample measures:
Appropriate amount of sample is weighed, is placed in 150 ml stuffed conical flasks, 80 ml water of addition, 80 DEG C of ultrasonic extraction 30min, every
5min or so shaking is primary, is kept fixed and is mutually completely dispersed, after being cooled to room temperature, is settled in 100ml volumetric flask, shakes up, mistake
Filter, takes portion filtrate at 4 DEG C, and 8000r/min is centrifuged 10min, and supernatant is spare, and supernatant 5ml is taken to be placed in 50ml volumetric flask
In, it reads absorbance with standard liquid series with condition colour developing, colorimetric with the zeroing of blank test solutions as controls and draws.
D. phosphate content in sample, calculation formula are calculated are as follows:
X= m1*v1*3.066*10-4 /m*v2, in formula:
X: phosphate content in sample, unit are gram every hectogram (%)；
m1: checked in by standard curve or regression equation calculate in Specimen Determination liquid the quality of phosphorus, unit be milligram (ug)；
v1: sample digestive juice constant volume total volume, unit are milliliter (mL)；
v2: the volume of measurement sample digestive juice, unit are milliliter (mL)；
M: the quality of sample, unit are gram (g)；
3.066: the conversion coefficient of phosphate (PO43-) and phosphorus (P).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112285039A (en) * | 2020-09-15 | 2021-01-29 | 青海西矿同鑫化工有限公司 | Method for determining phosphate radical in fluosilicic acid |
| CN112683818A (en) * | 2020-12-08 | 2021-04-20 | 山东祥通橡塑科技有限公司 | Method for measuring total phosphorus content in ammonium polyphosphate |
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| CN1664567A (en) * | 2005-03-14 | 2005-09-07 | 陕西师范大学 | Chemiluminescent organophosphorus pesticide residual analyzer and detecting method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112285039A (en) * | 2020-09-15 | 2021-01-29 | 青海西矿同鑫化工有限公司 | Method for determining phosphate radical in fluosilicic acid |
| CN112683818A (en) * | 2020-12-08 | 2021-04-20 | 山东祥通橡塑科技有限公司 | Method for measuring total phosphorus content in ammonium polyphosphate |
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Application publication date: 20191115 |