CN106989984A - Detect the preprocess method of object and the method for detecting object in sample in sample - Google Patents
Detect the preprocess method of object and the method for detecting object in sample in sample Download PDFInfo
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- CN106989984A CN106989984A CN201710362470.6A CN201710362470A CN106989984A CN 106989984 A CN106989984 A CN 106989984A CN 201710362470 A CN201710362470 A CN 201710362470A CN 106989984 A CN106989984 A CN 106989984A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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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
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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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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Abstract
The present invention proposes the preprocess method of object in detection sample, the method for object and the method for detecting nitrate and nitrite in cheese product in detection sample.The preprocess method of object includes in the detection sample：The sample is subjected to freezing processing, to obtain frozen product, wherein, the sample is cheese product.The preprocess method of object can effectively improve the water solubility of cheese product in the detection sample of the present invention, in order to late detection, improve the accuracy of testing result, and easy to operate.
Description
Technical field
The present invention relates to field of food.In particular it relates to detect the preprocess method of object and inspection in sample
The method of object in test sample product.More particularly it relates to detect the preprocess method of object in sample, detection sample
The method of nitrate and nitrite in the method and detection cheese product of middle object.
Background technology
Cheese product is primarily referred to as cheese or the class dairy products containing cheese.Cheese product rich in a large amount of protein,
The nutrients of the needed by human body such as calcium, phosphorus, nutritive value is higher.
However, the detection method for cheese product still has much room for improvement at present.
The content of the invention
It is contemplated that at least solving at least one technical problem present in prior art to a certain extent.Therefore,
The present invention proposes the preprocess method of object in detection sample, detects the method for object and detection cheese system in sample
The method of nitrate and nitrite in product.Thus, the pretreatment side for detecting object in sample according to embodiments of the present invention
Method can effectively improve the water solubility of cheese product, in order to late detection, improve the accuracy of testing result, and operation letter
Just.
It should be noted that the present invention is the following discovery based on inventor and completed：
When being detected to cheese product, it usually needs in advance dissolved cheese product.But, due to cheese product
Usually contain higher fatty acid high protein and viscosity is larger, so being difficult to be completely dissolved in water, even being boiled in boiling water
Do not reach and be completely dissolved, be that subsequent detection brings difficulty, reduce the accuracy of testing result.
In view of this, inventor is had found by many experiments, and cheese product is carried out into freezing processing in advance, destroys its knot
Structure, reduces viscosity.Product after chilled processing has preferable water solubility, is easy to subsequent detection, improves the standard of testing result
True property, and it is easy to operate.
In one aspect of the invention, the present invention proposes a kind of preprocess method for detecting object in sample.According to
Embodiments of the invention, methods described includes：The sample is subjected to freezing processing, to obtain frozen product, wherein, it is described
Sample is cheese product.Inventor is had found by many experiments, and cheese product is carried out into freezing processing in advance, its structure is destroyed,
Reduce viscosity.Product after chilled processing has preferable water solubility, is easy to subsequent detection, improves the accurate of testing result
Property, and it is easy to operate.
The preprocess method of object can also have following additional in embodiments in accordance with the present invention, above-mentioned detection sample
Technical characteristic：
Embodiments in accordance with the present invention, the freezing processing is that the sample is cooled into -150~-200 in 10 minutes
DEG C, and kept for 1~3 hour.Inventor has found that freezing processing condition can influence the dissolubility of cheese product, if freezing processing temperature
Spend the high or time too short, it is impossible to destroy its structure completely, make it that still there is higher viscosity, cause water-soluble poor；If
Freezing processing temperature is too low or overlong time, and object excessively distils in sample, causes the rate of recovery of detection relatively low, accuracy
It is relatively low, it can also increase testing cost.Inventor has found that freezing processing is freezed 1~3 hour under -150~-200 degrees Celsius,
Enable to cheese product rapidly to distil to dry out, reduce viscosity, so that with preferably water solubility, and to object to be measured
Influence is smaller.Thus, cheese product can be effectively improved according to the preprocess method of object in the detection sample of the present invention
Water solubility, in order to late detection, improve the accuracy of testing result, and easy to operate.
Embodiments in accordance with the present invention, the freezing processing is that the sample was cooled into -180 DEG C in 10 minutes, and
Kept for 2 hours.Inventor has found, enables to cheese product rapidly to distil on this condition and dries out, and reduces viscosity, so that
With preferably water-soluble and smaller on object to be measured influence.Thus, according to the present invention detection sample in object it is pre-
Processing method can effectively improve the water solubility of cheese product, in order to late detection, improve the accuracy of testing result, and
It is easy to operate.
It should be noted that the present invention does not do considered critical for object to be measured, it can be selected according to actual needs
Select.Embodiments in accordance with the present invention, the object is selected from least one of NO3-N and NO2-N.Thus, according to this hair
The preprocess method of object can effectively improve the water solubility of cheese product in bright detection sample, in order to which the later stage is examined
Survey, improve the accuracy of testing result, and it is easy to operate.
In another aspect of this invention, the present invention proposes a kind of method for detecting object.According to the implementation of the present invention
Example, methods described includes：The preprocess method of object is pre-processed to sample in detection sample as described above, so as to
Obtain pretreatment product；And object described in the pretreatment product is detected, to determine that the object contains
Amount.Thus, the water solubility of cheese product can be effectively improved according to the method for the detection object of the present invention, in order to mesh
Mark thing is detected, improves the accuracy of testing result, and easy to operate.
It will be appreciated to those of skill in the art that above for described by the preprocess method of object in detection sample
Feature and advantage, the method for being equally applicable to the detection object will not be repeated here.
In still another aspect of the invention, the present invention proposes a kind of side for detecting nitrate and nitrite in cheese product
Method.Embodiments in accordance with the present invention, it is described including：The cheese product was cooled to -150~-200 DEG C in 10 minutes, and
Kept for 1~3 hour, to obtain pretreatment product；The pretreatment product is subjected to isolating protein and fat processing, the is obtained
One treatment fluid；Reduction treatment is carried out to first treatment fluid with copper facing cadmium grain, to obtain second processing liquid；By described second
Treatment fluid carries out mixed processing with sulfanilamide (SN) and N-1- naphthyls-ethylendiamine dihydrochloride, to obtain the 3rd treatment fluid；And to institute
State the 3rd treatment fluid and carry out absorbance detection, and determine that nitrate and nitrite contain in the cheese product based on testing result
Amount.Thus, the method for nitrate and nitrite can be determined exactly in detection cheese product according to embodiments of the present invention
Go out nitrate and content of nitrite, and it is easy to operate, accuracy is higher.
Embodiments in accordance with the present invention, were cooled to -180 DEG C, and kept for 2 hours by the cheese product in 10 minutes.
Thus, the method for nitrate and nitrite can determine nitre exactly in detection cheese product according to embodiments of the present invention
Hydrochlorate and content of nitrite, and it is easy to operate, accuracy is higher.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Embodiment
Embodiments of the invention are described below in detail.The embodiments described below is exemplary, is only used for explaining this hair
It is bright, and be not considered as limiting the invention.
The solution of the present invention is explained below in conjunction with embodiment.It will be understood to those of skill in the art that following
Embodiment is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Unreceipted particular technique or bar in embodiment
Part, carried out according to the technology or condition described by document in the art or according to product description.Agents useful for same or instrument
The unreceipted production firm person of device, being can be by the conventional products of acquisition purchased in market.
Embodiment 1
In this embodiment, nitrate content in cheese is detected in following manner：
(1) precise 10g cheese sample is placed in superfreeze bottle, connects sample port, opens superfreeze
Instrument, makes cheese in freezing bottle be cooled to -180 DEG C in 10 minutes, and is kept for 2 hours, obtains frozen product.
(2) frozen product is transferred in 250ml triangular flasks with 110ml moisture, mixed.
(3) 24mL solution of zinc sulfate (53.5g/100mL), 24mL potassium ferrocyanide solutions are sequentially added into triangular flask
(17.2g/100mL) and 40mL cushioning liquid, wants side edged to shake during addition, often adding a kind of solution will fully shake up.Stand
15min~1h.Then filtered with filter paper, filtrate is collected with 250mL conical flasks.
(4) 20mL filtrates are pipetted in 100mL small beakers, 5mL cushioning liquid (2mol/L hydrochloric acid) is added, shakes up, pour into
In the cistern of cadmium column top, post is crossed with the flow velocity less than 6mL/min.Elutriant (liquid crossed after post) access 100mL capacity
In bottle.When cistern is soon emptied, small beaker is rinsed with 15mL water, then pour into cistern.After flushing current are complete, then use
15mL water is repeated once.When second of flushing water flows to end soon, cistern is filled into water, post is crossed with Peak Flow Rate.Work as volumetric flask
In elutriant close to 100mL when, take out volumetric flask, use water constant volume, mix.
(5) 20mL elutriants and 20mL filtrates are pipetted respectively in 100mL volumetric flasks, add water to about 60mL.Hold each
6mL nitrite ions 1 are first added in measuring bottle, and (volume ratio is 450：550 water-hydrochloric acid solution), side edged is mixed；Add 5mL nitrite ions
2 (5g/L sulfanilamide (SN) solution).Careful mixed solution, makes it stand 5min at room temperature, it is to avoid direct sunlight.Add 2mL colour developings
Liquid 3 (1g/L N-1- naphthyls-ethylendiamine dihydrochloride solution), careful mixing, makes it stand 5min at room temperature, it is to avoid direct projection
Sunlight.Scale is settled to water, is mixed.538nm wavelength is used in 15min, using blank test liquid as the above-mentioned sample of blank determination
The absorbance of product solution.
(6) it is sub- that (or being released with buret) 0mL, 2mL, 4mL, 6mL, 8mL, 10mL, 12mL, 16mL and 20mL is pipetted respectively
Nitric acid sodium standard solution is in 9 100mL volumetric flasks.Added water in each volumetric flask, make its volume about 60mL.Hold each
6mL nitrite ions 1 are first added in measuring bottle, side edged is mixed；Add 5mL nitrite ions 2.Careful mixed solution, makes it quiet at room temperature
Put 5min, it is to avoid direct sunlight.2mL nitrite ions 3 are added, careful mixing makes it stand 5min at room temperature, it is to avoid direct projection sun
Light.Scale is settled to water, is mixed.In 15min, 538nm wavelength is used, with first solution (being free of natrium nitrosum) for control
Determine the absorbance of other eight solution.The absorbance measured is mapped to nitrite anions mass concentration.The quality of nitrite anions
Concentration can be calculated according to the gauge of the natrium nitrosum standard liquid of addition.The mass concentration of nitrite anions is abscissa, absorbance
For ordinate.The mass concentration of nitrite anions is represented with μ g/100mL.
Nitrate (in terms of nitrate anion) cubage formula is as follows：
X=1.35 × [100000 × c2/(m×V2)-W(NO2 -)]
In formula：
X --- nitrate radical content (mg/kg) in sample；
c2--- according to the absorbance of elutriant, the nitrite ion concentration read from standard curve, unit is micro-
Gram every hundred milliliters (μ g/100mL)；
The quality of m --- sample, unit is gram (g)；
V2--- the volume of elutriant is taken, unit is milliliter (mL)；
W(NO2 -) --- the nitrite anions content calculated according to following formula：
X=20000 × c1/(m×V1)
In formula：
X --- sample Nitrite content, unit is milligrams per kilogram (mg/kg)；
c1--- according to the absorbance of filtrate, the NO read from standard curve2 -Concentration, unit be every hundred milliliters of microgram
(μg/100mL)；
The quality of m --- sample, unit is gram (g)；
V1--- the volume of filtrate is taken, unit is milliliter (mL).
Embodiment 2 determines the rate of recovery
In this embodiment, the rate of recovery is determined in following manner：
(1) the cheese sample without nitrate is mixed with nitrate standard items, obtains mark-on sample, wherein mark-on
Nitrate in sample is denoted as theoretical content；
(2) nitrate content in mark-on sample is determined according to the method for embodiment 1, is denoted as actual content；
(3) rate of recovery is calculated based on following equation：
The rate of recovery (the %)=÷ theoretical contents of (actual content-theoretical content) × 100%
As a result it is as shown in table 1.As can be seen that the rate of recovery of the method for the present invention is 85~110%, meet national standard,
Illustrate that the testing result accuracy of the present invention is higher.
The rate of recovery of table 1
Comparative example 1
In the comparative example, the rate of recovery is determined according to the method for embodiment 2, difference is, in embodiment 1, makes freezing bottle
Interior cheese was cooled to -120 DEG C in 10 minutes, and was kept for 2 hours.
As a result it is as shown in table 2.As can be seen that the rate of recovery of this method is relatively low, testing result accuracy is relatively low.Main cause
Be probably at this temperature cheese do not destroy its structure completely, make it that still there is higher viscosity, cause it is water-soluble poor, from
And influence testing result accuracy.
The rate of recovery of table 2
Comparative example 2
In the comparative example, the rate of recovery is determined according to the method for embodiment 2, difference is, in embodiment 1, makes freezing bottle
Interior cheese was cooled to -220 DEG C in 10 minutes, and was kept for 2 hours.
As a result it is as shown in table 3.As can be seen that the rate of recovery of this method is relatively low, testing result accuracy is relatively low.Main cause
It is probably that composition excessively distils in sample at this temperature, causes that the rate of recovery of detection is relatively low, accuracy is relatively low.
The rate of recovery of table 3
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means to combine specific features, structure, material or the spy that the embodiment or example are described
Point is contained at least one embodiment of the present invention or example.In this manual, to the schematic representation of above-mentioned term not
Identical embodiment or example must be directed to.Moreover, specific features, structure, material or the feature of description can be with office
Combined in an appropriate manner in one or more embodiments or example.In addition, in the case of not conflicting, the skill of this area
Art personnel can be tied the not be the same as Example or the feature of example and non-be the same as Example or example described in this specification
Close and combine.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changed, replacing and modification.
Claims (7)
1. a kind of preprocess method for detecting object in sample, it is characterised in that including：
The sample is subjected to freezing processing, to obtain frozen product,
Wherein, the sample is cheese product.
2. according to the method described in claim 1, it is characterised in that the freezing processing be by the sample in 10 minutes it is cold
But to -150~-200 DEG C, and kept for 1~3 hour.
3. according to the method described in claim 1, it is characterised in that the freezing processing be by the sample in 10 minutes it is cold
But to -180 DEG C, and kept for 2 hours.
4. according to the method described in claim 1, it is characterised in that the object is selected from NO3-N and NO2-N at least
One of.
5. a kind of method for detecting object, it is characterised in that including：
Preprocess method according to object in any one of Claims 1 to 4 detection sample is pre-processed to sample, with
Just pretreatment product is obtained；And
Object described in the pretreatment product is detected, to determine the object content.
6. a kind of method for detecting nitrate and nitrite in cheese product, it is characterised in that including：
The cheese product was cooled to -150~-200 DEG C in 10 minutes, and kept for 1~3 hour, to be pre-processed
Product；
The pretreatment product is subjected to isolating protein and fat processing, the first treatment fluid is obtained；
Reduction treatment is carried out to first treatment fluid with copper facing cadmium grain, to obtain second processing liquid；
The second processing liquid and sulfanilamide (SN) and N-1- naphthyls-ethylendiamine dihydrochloride are subjected to mixed processing, to obtain the 3rd
Treatment fluid；And
Absorbance detection is carried out to the 3rd treatment fluid, and nitrate and Asia in the cheese product are determined based on testing result
Nitrate content.
7. method according to claim 6, it is characterised in that the cheese product was cooled to -180 in 10 minutes
DEG C, and kept for 2 hours.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103018232A (en) * | 2011-09-20 | 2013-04-03 | 内蒙古蒙牛乳业（集团）股份有限公司 | Detection method for sulfite in milk |
| CN105651768A (en) * | 2015-12-29 | 2016-06-08 | 内蒙古蒙牛乳业（集团）股份有限公司 | Color developing agent composition and application thereof as well as method for detecting nitritein sample |
| CN105929044A (en) * | 2016-04-14 | 2016-09-07 | 宁波出入境检验检疫局检验检疫技术中心 | Method for rapidly detecting hydroxy proline content of milk and dairy products |
-
2017
- 2017-05-22 CN CN201710362470.6A patent/CN106989984B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103018232A (en) * | 2011-09-20 | 2013-04-03 | 内蒙古蒙牛乳业（集团）股份有限公司 | Detection method for sulfite in milk |
| CN105651768A (en) * | 2015-12-29 | 2016-06-08 | 内蒙古蒙牛乳业（集团）股份有限公司 | Color developing agent composition and application thereof as well as method for detecting nitritein sample |
| CN105929044A (en) * | 2016-04-14 | 2016-09-07 | 宁波出入境检验检疫局检验检疫技术中心 | Method for rapidly detecting hydroxy proline content of milk and dairy products |
Non-Patent Citations (3)
| Title |
|---|
| DAVID S. REID，HONG YAN，ET AL.: "RHEOLOGICAL, MELTING AND MICROSTRUCTURAL PROPERTIES OF CHEDDAR AND MOZZARELLA CHEESES AFFECTED BY DIFFERENT FREEZING METHODS", 《JOURNAL OF FOOD QUALITY》 * |
| 曾庆祝，余以刚，战宇: "《食品质量与安全检测》", 30 September 2015, 中国质检出版社 * |
| 陈健，吴国杰，赵谋明: "《食品化学原理》", 28 February 2015, 华南理工大学出版社 * |
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