CN104359877A - Resonance Rayleigh scattering spectrometry for quickly determining sodium hexametaphosphate - Google Patents
Resonance Rayleigh scattering spectrometry for quickly determining sodium hexametaphosphate Download PDFInfo
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- CN104359877A CN104359877A CN201410613268.2A CN201410613268A CN104359877A CN 104359877 A CN104359877 A CN 104359877A CN 201410613268 A CN201410613268 A CN 201410613268A CN 104359877 A CN104359877 A CN 104359877A
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- sodium hexametaphosphate
- rayleigh scattering
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Abstract
The invention discloses a resonance Rayleigh scattering spectrometry for simply and quickly determining sodium hexametaphosphate. The resonance Rayleigh scattering spectrometry comprises the steps: (1) preparing a sodium hexametaphosphate standard solution system; (2) preparing a blank contrast solution system; (3) respectively determining resonance Rayleigh scattering peak strength values I standard and I blank of the sodium hexametaphosphate standard solution system and the blank contrast solution system, and performing the formula: delta I = I standard - I blank; (4) drafting a working curve of the concentration relation of the sodium hexametaphosphate by using the delta I; (5) determining a sample of an object to be determined, and performing the formula: delta I sample = I sample - I blank; (6) checking the working curve draft in step (4) according to the obtained delta I sample, and calculating the content of the sodium hexametaphosphate in the object to be determined. The resonance Rayleigh scattering spectrometry for simply and quickly determining the sodium hexametaphosphate has the advantages that the utilized devices are simple, the operations are quick, the sensitivity is high, and the selectivity is excellent.
Description
Technical field
The present invention relates to analytical chemistry field, specifically measure the Resonance Rayleigh Scattering Spectral Method of sodium hexametaphosphate.
Background technology
A kind of traditional, conventional food quality modifying agent of sodium hexametaphosphate.Be usually used in the food industry improving the retentiveness of meat product and being knotted property, prevent fat oxidation; Improve crushing juice rate and the viscosity of fruit beverage, suppress ascorbic decomposition; In addition, it is also for stablizing the natural colouring matter and color and luster etc. in other food.But excessive interpolation can destroy the various nutrients in food, and in human body, long time integration can cause as various diseases such as neoplastic lesion, fluorosis of bone, osteosclerosis and osteoporosises, damages people's liver function.Therefore, clear and definite regulation has been done to the allowance of sodium hexametaphosphate in varieties of food items by China, must not more than 0.5g/kg.At present, the main method measuring sodium hexametaphosphate has the chromatography of ions, Pulse sample introduction device, the precipitation method and spectrophotometric method.But the chromatography of ions and Pulse sample introduction device operate more complicated loaded down with trivial details, and precipitation method portion of reagent used has toxicity or corrosivity, although spectrophotometric method sensitivity simple to operate is lower.Therefore, a kind of method that is simple, that detect hexa metaphosphoric acid sodium content in food additives is fast set up significant.
Resonance Rayleigh Scattering Spectral Method is the spectral analysis technique that a kind of selectivity is good, highly sensitive, food, health, safety, clinical etc. in all have application.Although Resonance Rayleigh Scattering Spectral Method detection technique report is more, the Resonance Rayleigh Scattering Spectral Method analytical approach research of sodium hexametaphosphate has no report.
Summary of the invention
The object of the invention is the Resonance Rayleigh Scattering Spectral Method that a kind of simple and quick mensuration sodium hexametaphosphate will be provided.
Use Resonance Rayleigh Scattering Spectral Method for Determination sodium hexametaphosphate, comprise the steps:
(1) prepare hexa metaphosphoric acid sodium standard solution system: get scale test tube, pipette 5 ~ 800 μ L 1.00 × 10 successively
-5moL/L hexa metaphosphoric acid sodium standard solution, the NaAc_HAc buffer solution of 200 ~ 280 μ L pH 2.6,100 ~ 200 μ L 9.9 × 10
-6moL/L VBB solution, shakes up, and reacts 20 min, then adds 400 ~ 550 μ L4.0 × 10
-4moL/L Silver nanorod colloidal sol, is settled to 2.0 mL with redistilled water, mixing;
(2) placebo solution system is prepared: do not add sodium hexametaphosphate titer by the method for step (1) and prepare placebo solution system;
(3) get the hexa metaphosphoric acid sodium standard solution system prepared by step (1), (2) respectively and placebo solution system appropriate, be placed in cuvette, on fluorospectrophotometer, synchronous scanning excitation wavelength and emission wavelength, the Resonance Rayleigh Scattering Spectra of acquisition system, measures the Resonance Rayleigh Scattering peak intensity value of system maximum wavelength 370 nm place hexa metaphosphoric acid sodium standard solution system
i, and measure the Resonance Rayleigh Scattering peak intensity value of placebo solution system
i 0, calculate Δ
i=
i-
i 0;
(4) with Δ
ithe concentration relationship of sodium hexametaphosphate is worked curve;
(5) measured object sample determination: get the testing sample containing sodium hexametaphosphate, operates by step (1) ~ (3).Calculate the Δ of measured object
i sample=
i sample-
i 0;
(6) Δ recorded per sample
i sample, look into the working curve of step (4), calculate the concentration of sodium hexametaphosphate in measured object.
The preparation method of described Silver nanorod colloidal sol is: in Erlenmeyer flask, add redistilled water 45mL, 2.0 mL 10 mmoL/L liquor argenti nitratis ophthalmicuses are sequentially added under magnetic agitation, 3.0 mL 60 mmoL/L citric acid three sodium solutions, finally add 150 μ L 0.38 moL/L hydrazine hydrate solutions, Keep agitation 10 min, be settled to 50 mL, namely obtain the Silver nanorod colloidal sol of Chinese red.This Silver nanorod collosol concentration is 4.0 × 10
-4moL/L Ag.
Realizing principle of the present invention is: in the NaAc_HAc buffer solution of pH 2.6, when not adding VBB probe, system along with the increase Resonance Rayleigh Scattering value of hexa metaphosphoric acid na concn unchanged; When not adding Silver nanorod colloidal sol, along with the change of the increase Resonance Rayleigh Scattering value of hexa metaphosphoric acid na concn is irregular, only has Acetic acid-sodium acetate damping fluid-VBB-Ag-sodium hexametaphosphate system, along with the increase system of hexa metaphosphoric acid na concn strengthens gradually in the Resonance Rayleigh Scattering intensity at 370nm place, and linear relation, establish the Resonance Rayleigh Scattering Spectral Method measuring sodium hexametaphosphate accordingly.
Advantage of the present invention is: compared with existing method, this assay method is easy and simple to handle, highly sensitive, selectivity good, stable system.
Accompanying drawing explanation
Fig. 1 is the partial resonance Rayleigh scattering light spectrogram that the embodiment of the present invention measures sodium hexametaphosphate.
In figure: (a) pH 2.6 HAc-NaAc+0.792 μm of oL/L VBB+0.1 mmoL/L Ag; (b) a+0.025 μm of oL/L sodium hexametaphosphate; (c) a+0.5 μm of oL/L sodium hexametaphosphate; (d) a+3.0 μm of oL/L sodium hexametaphosphate; (e) a+4.0 μm of oL/L sodium hexametaphosphate.
Embodiment
Embodiment:
Application Resonance Rayleigh Scattering Spectral Method for Determination sodium hexametaphosphate, comprises the steps:
(1) hexa metaphosphoric acid sodium standard solution system is prepared: get scale test tube, move 5,100,400,600,800 μ L 1.00 × 10
-5moL/L hexa metaphosphoric acid sodium standard solution joins in different test tubes respectively, then in each test tube, adds the NaAc_HAc buffer solution of 250 μ L pH 2.6 successively, 160 μ L 9.9 × 10
-6moL/L VBB solution, shakes up, and reacts 20 min, then adds 500 μ L4.0 × 10
-4moL/L Silver nanorod colloidal sol, is settled to 2.0 mL with redistilled water, and mixing, makes multiple hexa metaphosphoric acid sodium standard solution system;
(2) placebo solution system is prepared: do not add sodium hexametaphosphate titer by the method for step (1) and prepare placebo solution system;
(3) get the hexa metaphosphoric acid sodium standard solution system prepared by step (1), (2) respectively and placebo solution system appropriate, be placed in cuvette, on fluorospectrophotometer, synchronous scanning excitation wavelength and emission wavelength, the Resonance Rayleigh Scattering Spectra of acquisition system, measures the Resonance Rayleigh Scattering peak intensity value of system maximum wavelength 370 nm place hexa metaphosphoric acid sodium standard solution system
i, and measure the Resonance Rayleigh Scattering peak intensity value of placebo solution system
i 0, calculate Δ
i=
i-
i 0;
(4) with Δ
ithe concentration relationship of sodium hexametaphosphate is worked curve;
(5) measured object sample determination: get commercially available Wahaha green tea, Chef Kang's green tea, Tongyi icy black tea sample, get 100 respectively
μl sample redistilled water is diluted to 10mL, namely obtains sample solution, operates by step (1) ~ (3).Calculate the Δ of measured object
i sample=
i sample-
i 0;
(6) Δ recorded per sample
i sample, look into the working curve of step (4), calculate the content of sodium hexametaphosphate in measured object and be respectively 020 g/kg, 0.18 g/kg, 0.14 g/kg.Measurement result all meets " Food Hygiene Law of the People's Republic of China " and in " food additives administration of health way ", the maximum use amount of food additives sodium hexametaphosphate in tea beverage is the regulation of 0.5g/Kg.
It is within the scope of 0.025 ~ 4.0 μm of oL/L and resonance Rayleigh scattering light intensity Δ that the embodiment of the present invention measures sodium hexametaphosphate content range
i 370nmlinear, equation of linear regression is equation is Δ
i 370nm=470.46C+226.7, detects and is limited to 0.01 μm of ol/L.
The recovery test: to 3 samples respectively replicate determination carry out recovery testu 5 times, the recovery is between 98.2 ~ 101.3%, and relative standard deviation is 1.2% ~ 3.6%.Illustrate that the method is correctly reliable.
Claims (1)
1. a Resonance Rayleigh Scattering Spectral Method for simple and quick mensuration sodium hexametaphosphate, is characterized in that: comprise the steps:
(1) prepare hexa metaphosphoric acid sodium standard solution system: get scale test tube, pipette 5 ~ 800 μ L 1.00 × 10 successively
-5moL/L hexa metaphosphoric acid sodium standard solution, the NaAc_HAc buffer solution of 200 ~ 280 μ L pH 2.6,100 ~ 200 μ L 9.9 × 10
-6moL/L VBB solution, shakes up, and reacts 20 min, then adds 400 ~ 550 μ L4.0 × 10
-4moL/L Silver nanorod colloidal sol, is settled to 2.0 mL with redistilled water, mixing;
(2) placebo solution system is prepared: do not add sodium hexametaphosphate titer by the method for step (1) and prepare placebo solution system;
(3) get the hexa metaphosphoric acid sodium standard solution system prepared by step (1), (2) respectively and placebo solution system appropriate, be placed in cuvette, on fluorospectrophotometer, synchronous scanning excitation wavelength and emission wavelength, the Resonance Rayleigh Scattering Spectra of acquisition system, measures the Resonance Rayleigh Scattering peak intensity value of system maximum wavelength 370 nm place hexa metaphosphoric acid sodium standard solution system
i, and measure the Resonance Rayleigh Scattering peak intensity value of placebo solution system
i 0, calculate Δ
i=
i-
i 0;
(4) with Δ
ithe concentration relationship of sodium hexametaphosphate is worked curve;
(5) measured object sample determination: get the testing sample containing sodium hexametaphosphate, operates by step (1) ~ (3); Calculate the Δ of measured object
i sample=
i sample-
i 0;
(6) Δ recorded per sample
i sample, look into the working curve of step (4), calculate the concentration of sodium hexametaphosphate in measured object.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106680062A (en) * | 2017-01-06 | 2017-05-17 | 广东药科大学 | Method for determining content of anionic surfactant by utilizing resonance rayleigh scattering method |
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|---|---|---|---|---|
| CN103604756B (en) * | 2013-11-29 | 2016-02-03 | 广西师范大学 | A kind of Resonance Rayleigh Scattering Technique measuring azides ion |
| CN103604792A (en) * | 2013-11-29 | 2014-02-26 | 广西师范大学 | Resonance Rayleigh scattering (RRS) method for measuring bromide ion |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106680062A (en) * | 2017-01-06 | 2017-05-17 | 广东药科大学 | Method for determining content of anionic surfactant by utilizing resonance rayleigh scattering method |
| CN106680062B (en) * | 2017-01-06 | 2019-04-16 | 广东药科大学 | Utilize the method for resonance rayleigh light scattering method measurement anionic surfactant concentration |
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