CN101561423A - Method for measuring content of polyphosphate in meat products - Google Patents
Method for measuring content of polyphosphate in meat products Download PDFInfo
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- CN101561423A CN101561423A CNA2009101436036A CN200910143603A CN101561423A CN 101561423 A CN101561423 A CN 101561423A CN A2009101436036 A CNA2009101436036 A CN A2009101436036A CN 200910143603 A CN200910143603 A CN 200910143603A CN 101561423 A CN101561423 A CN 101561423A
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Abstract
The invention relates to a method for detecting the content of polyphosphate in meat products and particularly relates to a method which can be used as a technology for detecting the specific form and content of the polyphosphate added in aquatic livestock food. The principle of the method is as follows: trifluoroacetic acid is used as a protein precipitant and a series of other pre-processing steps are also conducted to the sample of the meat products. An AS11-HC anion-exchange column is selected for matching with a GP40 pump to generate sodium hydroxide with different concentrations according to the proportion, to carry out gradient separation. Inhibitory-type electrical conductivity detection can accurately fix the quantity of the concentrations of pyrophosphate, tripolyphosphate and trimetaphosphate in different products. The method can be applied to the quantitative detection of pyrophosphate, tripolyphosphate and trimetaphosphate in aquatic food and meat products.
Description
Technical field
The present invention relates to the method for content of polyphosphate in the meat products, particularly relate to the concrete form that can be used as the polyphosphate that adds in the aquatic livestock property food and the detection technique of content.
Background technology
Polyphosphate is widely used in the processing of aquatic products processes such as fish as water-loss reducer and quality improver, play the effect that keeps moisture to improve mouthfeel, but in some aquatic products, ban use of, use as forbidding in the scallop process: European Union and Czech use polyphosphate to the cod fillet and the strict restriction of artificial crab meat of its import, and Poland does not allow to use.Under the situation about allow using in process, polyphosphate allows to limit the quantity of and is 0.5g/kg in the general frozen fish.Content of polyphosphate in the control aquatic products becomes the problem that people pay close attention to.
At present, people require the content of the polyphosphate in the control cod for the consideration of safety and Health.The method of conventional mensuration content of polyphosphate is that polyphosphate is converted into orthophosphate, uses phosphomolybdic acid quinoline method, gravimetric method or colorimetric method for determining then, but can't distinguish the form of polyphosphate.Because the existence of water-soluble phosphate in cod and scallop post and other aquatic products, differentiate with the method for routine whether to have added polyphosphate in cod and scallop post process be very difficult, at present, domestic Hai No has the effective ways of polyphosphate in the check aquatic products.Chromatography of ions is the anionic method of a kind of good mensuration, has the multiple anionic characteristics of separation determination simultaneously.By forming of the polyphosphate of human ion-chromatographic determination chemicals.This work is studied the method for polyphosphate in ion-chromatographic determination cod and the scallop post, adopts polyphosphate in deionized water ultrasonic extraction cod and the scallop post, and protein and fat are removed in sedimentation, and the ion chromatograph conductance detecting device detects.This research provides phosphatic quantitative detecting method in the detection aquatic food, guarantees that for supervision and inspection institute the security of aquatic products meat products provides reference frame.
Summary of the invention
The object of the invention provides a kind of polyphosphate concrete form that adds in the marine product and method of content of detecting.The step of this method is: earlier sample is smashed to pieces, taken by weighing the sample of certain mass, add the certain volume deionized water, place the supersonic wave cleaning machine ultrasonic extraction.And then in the hydro-extractor of 6000rpm centrifugal 10 minutes, with 0.22 μ m membrane filtration, add trifluoroacetic acid solution sedimentation protein in the filtrate, put into 0-4 ℃ of refrigerator and preserved 30 minutes, centrifugal again, filter, filtrate is crossed the RP post, dilute 100 times after sample introduction.
The present invention finally selects for use trifluoroacetic acid as protein precipitant, and the marine product sample is carried out a series of other pre-treatment steps through a large amount of experiments.Select for use the AS11-HC anion-exchange column to cooperate the GP40 pump to produce variable concentrations NaOH in proportion and carry out gradient separations, inhibition type electricity is led detection, can accurately quantitative different marine product samples in the concentration of pyrophosphate, tripolyphosphate and trimetaphosphate.
Embodiment
Embodiment: composite phosphate assay in the cod fillet
Sample pre-treatments
The cod fillet sample is smashed to pieces, taking by weighing the 10.0g sample enters in the 250mL flask, add the 50mL deionized water, flask is put into supersonic wave cleaning machine ultrasonic extraction 10min, in the hydro-extractor of 6000rpm centrifugal 10 minutes, filter (with 0.22 μ m nylon membrane), add 5mL20% trifluoroacetic acid solution sedimentation protein in the filtrate, putting into 0-4 ℃ of refrigerator preserved 30 minutes, in the hydro-extractor of 6000rpm centrifugal 10 minutes again, after the filtration filtrate is crossed OnGuard RP post, dilute in 100 times of laggard sample introduction bottles stand-by.
The mensuration of method precision: basic, normal, high three samples are respectively got 6 times respectively measure by method.The actual sample of parallel processing is measured under basic, normal, high concentration, relative standard deviation＜2%.Analysis result sees Table 1-1:
Table 1-1: the mensuration of sample precision
The mensuration of method accuracy:, in the sample solution of same concentration, add certain density pure standard solution and carry out six mark-ons recovery experiments in order further to investigate the accuracy of this method.Actual recovery of standard addition meets laboratory macro-analysis requirement between 86%～96%.Analysis result sees Table 1-3:
Table 1-3: the mensuration of recovery of standard addition
| Sample | The sample determination value, % | Sample determination value behind the mark-on, % | Add standard volume, % | The recovery, % |
| The 1st time | 1.23 | 2.15 | 1.00 | 96.4 |
| The 2nd time | 1.25 | 2.09 | 1.00 | 92.9 |
| The 3rd time | 1.20 | 2.01 | 1.00 | 91.4 |
| The 4th | 1.30 | 1.98 | 1.00 | 86.1 |
| The 5th | 1.35 | 2.03 | 1.00 | 86.4 |
| The 6th time | 1.39 | 2.09 | 1.00 | 87.4 |
Obviously, those skilled in the art can come the content of composite phosphate in the quantitative measurement marine product with the chromatography of ions of the present invention.
The foregoing description is only for the usefulness that the present invention is described; and be not to be limitation of the present invention; the those of ordinary skill in relevant technologies field; under the situation that does not break away from the scope of application of the present invention; can also make various variations and modification; therefore all technical schemes that are equal to also should belong to category of the present invention, and scope of patent protection of the present invention should be limited by each claim.
Claims (3)
1. the assay method of content of polyphosphate in the meat products, it is characterized in that: the step of this method is: earlier the phosphatic sample that contains to be determined is smashed to pieces, take by weighing the sample of certain mass, add the certain volume deionized water, place the supersonic wave cleaning machine ultrasonic extraction.And then in the hydro-extractor of 6000rpm centrifugal 10 minutes, with 0.22 μ m membrane filtration, add reagent solution sedimentation protein in the filtrate, put into 0～4 ℃ of refrigerator and preserved 30 minutes, centrifugal again, to filter, filtrate is crossed the RP post, dilution back sample introduction.Come quantification of phosphate content according to typical curve.
2. according to the assay method of content of polyphosphate in the described meat products of claim 1, it is characterized in that the employing protein precipitant is a trifluoroacetic acid.
3. according to the assay method of content of polyphosphate in the described meat products of claim 1, it is characterized in that, use polyphosphate concrete form that ion chromatography adds in can the qualitative detection meat products and the further phosphatic content of various forms that adds of quantitative measurement.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009101436036A CN101561423A (en) | 2009-05-27 | 2009-05-27 | Method for measuring content of polyphosphate in meat products |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009101436036A CN101561423A (en) | 2009-05-27 | 2009-05-27 | Method for measuring content of polyphosphate in meat products |
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| CN101561423A true CN101561423A (en) | 2009-10-21 |
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| CNA2009101436036A Pending CN101561423A (en) | 2009-05-27 | 2009-05-27 | Method for measuring content of polyphosphate in meat products |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103698448A (en) * | 2013-12-05 | 2014-04-02 | 华南农业大学 | Method for fast separation and determination of phosphates in different forms in ammonium polyphosphate |
| CN104007190A (en) * | 2014-03-21 | 2014-08-27 | 舟山出入境检验检疫局综合技术服务中心 | Method for simultaneously detecting propionate, citrate and polyphosphate in aquatic product |
-
2009
- 2009-05-27 CN CNA2009101436036A patent/CN101561423A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103698448A (en) * | 2013-12-05 | 2014-04-02 | 华南农业大学 | Method for fast separation and determination of phosphates in different forms in ammonium polyphosphate |
| CN103698448B (en) * | 2013-12-05 | 2015-06-17 | 华南农业大学 | Method for fast separation and determination of phosphates in different forms in ammonium polyphosphate |
| CN104007190A (en) * | 2014-03-21 | 2014-08-27 | 舟山出入境检验检疫局综合技术服务中心 | Method for simultaneously detecting propionate, citrate and polyphosphate in aquatic product |
| CN104007190B (en) * | 2014-03-21 | 2015-04-22 | 舟山出入境检验检疫局综合技术服务中心 | Method for simultaneously detecting propionate, citrate and polyphosphate in aquatic product |
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Open date: 20091021 |