CN108918793A - The detection method of amino acid in feed - Google Patents
The detection method of amino acid in feed Download PDFInfo
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- CN108918793A CN108918793A CN201810885368.9A CN201810885368A CN108918793A CN 108918793 A CN108918793 A CN 108918793A CN 201810885368 A CN201810885368 A CN 201810885368A CN 108918793 A CN108918793 A CN 108918793A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/02—Food
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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
- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
- G01N2001/386—Other diluting or mixing processes
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Abstract
The present invention relates to the preparation method of amino acid extracting solution in feed, this method includes mixing, hydrolysis, evaporation and dilution processing under conditions of temperature is 50~60 DEG C.Detection method of the invention is made compared with prior art using the extracting method, accuracy, precision and the rate of recovery greatly improve, precision is up to 0.58-11.15%, the rate of recovery is up to 89-103.2%, and is capable of the content of disposable 17 kind hydrolysis amino acid of the Accurate Determining including methionine, cysteine, tyrosine, phenylalanine and histidine etc..
Description
Technical field
The present invention relates to field of food, in particular it relates in feed amino acid detection method, more specifically,
The present invention relates to the methods of amino acid in the preparation method of amino acid extracting solution in feed and detection feed.
Background technique
The detection method of amino acid is currently with national standard in feed《Amino acid in GB/T 18246-2000 feed
Measurement》Based on, but the pretreatment process step in the national standard method is comparatively laborious.
Therefore, the good measuring method of step simplicity, strong operability, detection effect also needs further to study.
Summary of the invention
The application is to be made based on inventor to the discovery of following facts and problem and understanding：
Inventors have found that national standard method《The measurement of amino acid in GB/T 18246-2000 feed》The sour water solution of middle record
There is only tryptophans to be unable to measure for method, and methionine, cysteine, tyrosine, phenylalanine and histidine cannot survey quasi- ask
Topic；And the accuracy of this method, precision and the rate of recovery are lower, and precision is only 5.05~16.17%, and the rate of recovery is only
51.3-91.7%.
Based on the above issues, it has furthermore been found that reason is following side after inventor is groped by countless experiments
Face：First, the ampoule bottle sealability in national standard method is not good enough, and the condition vacuumized in actual operation at all can not be real
It applies, causes tryptophan to be all oxidized destruction and be unable to measure, cysteine and methionine part are oxidized and can not survey standard.Its
Two, national standard method is evaporated using rotary evaporator, and there are the following problems, firstly, rotary evaporation need by sample by
It is a to be concentrated, cause thickening efficiency low, time-consuming, and about sample needs to carry out 15~20min；Secondly, rotary evaporation
The general volume of the evaporative flask used is larger, causes sample loss in transfer process more；Finally, due to include salt in hydrolyzate
Acid, therefore the hydrochloric acid to volatilize during rotary evaporation will certainly cause Rotary Evaporators to corrode and influence Rotary Evaporators
Leakproofness causes evaporation efficiency to reduce.Third, the inspissator that national standard method uses is that speed is concentrated in the case where determining boiling point
Comparatively fast, and the hydrolysis solution composition of the application is complicated, boiling point is different, cause the application sample hydrolyze after if dense with inspissator
Contracting, time-consuming, and thickening efficiency is low, and a collection of sample can not necessarily meet the requirements concentration one hour or more.
Finally, inventor, which passes through, replaces ampoule bottle with hydrolyzing pipe, while inflated with nitrogen is protected, phenol as indicator into
Row detection, and triangular flask is placed on electric hot plate and carries out heating evaporation at a suitable temperature, the above problem is overcome, into
And compared with prior art, accuracy, precision and the rate of recovery of detection method greatly improve, and precision is up to 0.58-
11.15%, the rate of recovery is up to 89-103.2%, and detection method of the invention can Accurate Determining include disposably egg ammonia
The content of 17 kinds of hydrolysis amino acids including acid, cysteine, tyrosine, phenylalanine and histidine etc..
For this purpose, the invention proposes a kind of preparation methods of amino acid extracting solution in feed in the first aspect of the present invention.
According to an embodiment of the invention, the method includes：
(1) the HCL solution of feed to be measured and 6mol/L is placed in hydrolysis pipe and carries out mixed processing；
3~4 drop phenol are added dropwise in the mixed material in hydrolysis pipe, backward hydrolysis pipe in be full of nitrogen, it is subsequent by
It hydrolyzes pipe and carries out sealing treatment；
Mixed material in the hydrolysis pipe of sealing is hydrolyzed；
(2) it will be filtered after hydrolysis process product pure water constant volume, filtrate be placed in triangular flask, the 5 of filtrate will be contained with
~50mL, if the triangular flask of 10mL or 25mL are placed on electric hot plate, by the filtrate in the triangular flask temperature be 50~60 DEG C
Under conditions of be evaporated processing；
(3) evaporation process product is diluted processing, the dilution processing is by being added into evaporation process product
What the HCL solution of 0.02mol/L carried out, to obtain the extracting solution.
In preparing feed in the method for amino acid extracting solution, inventors have found that the capacity and evaporation process of triangular flask
Temperature and the testing result relationship of hydrolysis amino acid in final sample are very big, if the capacity of triangular flask is too big, although sample liquid is volatilized
Speed is fast, but dilution when will lead to machine can not all dissolve residue in bottle well, to give sample detection result
Bring very big deviation.If the temperature of evaporation process is excessively high, part sample liquid can be made to burn in triangular flask bottom, destroy ammonia to be measured
The structure of base acid, causes the loss of sample, and the accuracy of detection method and the rate of recovery is caused to reduce；If evaporation process
Temperature is too low, and the detection efficiency of detection method can be made too low.Made using extracting method according to an embodiment of the present invention
Compared with prior art, accuracy, precision and the rate of recovery greatly improve detection method of the invention, and precision is up to 0.58-
11.15%, the rate of recovery is up to 89-103.2%, and can Accurate Determining include disposably methionine, cysteine, junket ammonia
The content of 17 kinds of hydrolysis amino acids including acid, phenylalanine and histidine etc..
According to an embodiment of the invention, the above method can also further comprise at least one following additional technical feature：
According to an embodiment of the invention, the hydrolysis process is to carry out 22~24 under conditions of temperature is 109~111 DEG C
Hour.Inventors have found that hydrolyzing under this condition more sufficiently, in turn, subsequent detection effect is more preferable.
According to an embodiment of the invention, further comprising before the dilution processing：It is added into evaporation process product pure
Water, repeated evaporation 2~3 times.Inventors have found that repeated evaporation can make hydrochloric acid evaporation completely, reduce the interference to subsequent detection,
In turn, detection effect is more preferable.
According to an embodiment of the invention, the feed to be measured is 30~50mg, the volume of the HCL solution of the 6mol/L is
10~15mL, the volume after the constant volume are 50mL, and the filtrate is 2~3mL.Inventors have found that each capacity and extraction step
It cooperates, in turn, subsequent detection effect is more preferable.
In the second aspect of the present invention, the invention proposes a kind of preparation methods of amino acid extracting solution in feed.According to
The embodiment of the present invention, the method includes：
(1) the HCL solution of 30~50mg feed to be measured and 10~15mL 6mol/L is placed in hydrolysis pipe and is mixed
Processing；
3~4 drop phenol are added dropwise in the mixed material in hydrolysis pipe, backward hydrolysis pipe in be full of nitrogen, it is subsequent by
It hydrolyzes pipe and carries out sealing treatment；
Mixed material in the hydrolysis pipe of sealing is carried out 22~24 hours under conditions of temperature is 109~111 DEG C
Hydrolysis process；
(2) it is filtered after hydrolysis process product being settled to 50mL with pure water, 2~3mL filtrate is taken to be placed in the triangle of 5~50mL
In bottle, the triangular flask for being contained with filtrate is placed on electric hot plate, in temperature is 50~60 DEG C by the filtrate in the triangular flask
Under the conditions of be evaporated processing；
(3) evaporation process product is diluted processing, the dilution processing is by being added into evaporation process product
What the HCL solution of 0.02mol/L carried out, to obtain the extracting solution.
Inventors have found that making detection method of the invention compared to existing skill using extracting method according to an embodiment of the present invention
Art, accuracy, precision and the rate of recovery greatly improve, and precision is up to 0.58-11.15%, and the rate of recovery is up to 89-103.2%,
And it being capable of 17 kinds including methionine, cysteine, tyrosine, phenylalanine and histidine etc. of disposable Accurate Determining
The content of hydrolysis amino acid.
According to an embodiment of the invention, the above method can also further comprise at least one following additional technical feature：
According to an embodiment of the invention, further comprising before the dilution processing：It is added into evaporation process product pure
Water, repeated evaporation 2~3 times.Inventors have found that repeated evaporation can make hydrochloric acid evaporation completely, reduce the interference to subsequent detection,
In turn, detection effect is more preferable.
In the third aspect of the present invention, the invention proposes a kind of methods of amino acid in detection feed.According to the present invention
Embodiment, the method includes：
Extracting solution is obtained using method described in any of the above embodiments；And
It is detected based on the extracting solution, to obtain the type and content of the amino acid in the feed.
Detection method step according to an embodiment of the present invention is easy, understandable, strong operability, while compared with prior art,
Accuracy, precision and the rate of recovery greatly improve, and precision is up to 0.58-11.15%, and the rate of recovery is up to 89-103.2%, and
And it being capable of disposable 17 kind water of the Accurate Determining including methionine, cysteine, tyrosine, phenylalanine and histidine etc.
Solve the content of amino acid.
According to an embodiment of the invention, the above method can also further comprise at least one following additional technical feature：
According to an embodiment of the invention, the detection is carried out by amino-acid analyzer.Inventors have found that using ammonia
Base acid analysis instrument is detected, and detection effect is more preferable, and instrument detection limit reaches 3P mol/uL.
According to an embodiment of the invention, the amino-acid analyzer uses Na+Exchange column, column temperature are 135 DEG C.Invention human hair
Existing, when amino-acid analyzer uses the condition, detection effect is more preferable.
Detailed description of the invention
Fig. 1 is the upper machine testing map schematic diagram of amino acid hybrid standard liquid according to an embodiment of the present invention；
Fig. 2 is that detection method according to an embodiment of the present invention shows the detected upper machine testing map of Feed Sample progress
It is intended to；And
Fig. 3 is to carry out detected upper machine testing map schematic diagram to Feed Sample according to national standard method.
Specific embodiment
The embodiment of the present invention is described below in detail, examples of the embodiments are shown in the accompanying drawings.Below with reference to
The embodiment of attached drawing description is exemplary, it is intended to is used to explain the present invention, and is not considered as limiting the invention.
It should be noted that extracting method and detection method of the invention is not only suitable for mixed feed, concentrated feed, addition
The extraction and measurement of total amino acid content in agent premixed feed, single feed and premix are also applied for lysozyme, iron zinc amino
The extraction and measurement of total amino acid content in the organic matters containing amino acid or protein such as sour Analysis of Nutritive Composition standard substance.
It should be noted that unless otherwise instructed, " hydrolysis amino acid " described herein, which refers to, passes through Feed Sample
The amino acid obtained after above-mentioned hydrolysis process, such as 17 kinds of hydrolysis amino acids that the detection method of the application can determine, i.e. day
L-aminobutanedioic acid, threonine, serine, glutamic acid, glycine, alanine, cysteine, valine, methionine, isoleucine,
Leucine, tyrosine, phenylalanine, lysine, histidine, arginine and proline.
Embodiment 1
The detection method of amino acid content is as follows in feed：
1) acid-hydrolysis method：Sample (mixed feed) is after sour hydrolysis process, constant volume, filtering, take filtered fluid a certain amount of into
Row catches up with acid, selects the extension rate of appropriate samples, is uniformly mixed using ultrasonic wave, through 0.22um membrane filtration, for use, direct machine
Upper measurement.
2) it takes amino acid mixing standard liquid 0.4mL (Japanese aginomoto company production, content 5ml), it is molten with 0.02mol/L hydrochloric acid
Liquid dissolves and is settled to 10mL, that is, being configured to 2nmol/20uL amino acid hybrid standard working solution, (wherein only proline is
4nmol/20uL), it measures and uses as upper machine, test map schematic diagram is referring to Fig. 1.It is automatically analyzed with Hitachi L-8900 type amino acid
(with the amino acid Sample series equivalent of known different content, sample introduction is analyzed, then responds signal and content with external standard method for instrument
Between relation curve calculate containing for sample automatically by instrument in the case where surveying calibration curve the same terms into the sample to be tested of equivalent
Amount) detection sample to be tested in each amino acid content.
3) machine measures and uses Na+ exchange post separation on the full-automatic instrument of amino acid, and 135 DEG C of column temperature, by instrument specification requirement
It prepares standard analysis and elutes solution and ninhydrin solution and ninhydrin buffer with pH1, pH2, pH3, pH4, pH6.Carry out ladder
Degree elution, is quantified, instrument detection limit reaches 3P mol/uL using multiple-reaction monitoring mode.
Above-mentioned steps 1) in sample (mixed feed) processing method it is specific as follows：
A) claim sample (30-50mg) to be added in hydrolysis pipe, after the HCL solution of the 6mol/L of (10-15) mL is added, mix, after
Continue and 3-4 drop phenol is added into hydrolysis pipe.Quick seal after inflated with nitrogen 1 minute, the constant temperature for pipe will be hydrolyzed being placed on (110 scholar 1) DEG C
In drying box, hydrolyze 22-24 hours.
B) finish it is cooling after, open pipe, the filtrate for being settled to 50mL with high purity water, filtering, take 2-3mL are placed in triangular flask
In (triangular flask of 10mL), it is evaporated under conditions of on electric hot plate at 50-60 DEG C and closely does, it is few to triangular flask Nei Kejia when necessary
Xu Shui repeats to be evaporated 2-3 times, and after natural cooling, sample is diluted to required concentration, utilization by the HCL solution that 0.02mol/L is added
Ultrasonic wave is uniformly mixed, through 0.22um membrane filtration, for use.
C) the standard solution that accurate compound concentration is 2.00nmol/20uL, measures as upper machine and uses, divided automatically with amino acid
Analyzer is with the amino acid content of external standard method Specimen Determination liquid.
Testing result is as follows：
The test map schematic diagram that detection method obtains is referring to fig. 2.The test map schematic diagram that National Standard Method obtains
Referring to Fig. 3.
For same Feed Sample, because pre-treatment extracting method is different, the precision of testing result can also differ widely.This
Invention detection method and National Standard Method see below the testing result of amino acid precision and type comparison in the mixed feed of embodiment 1
Table 1.
Table 1：Detection method and National Standard Method are to the testing result pair of amino acid precision and type in mixed feed
Than
It is analyzed by upper 1 data of table it is found that detection method is compared with National Standard Method, accuracy greatly improves, and detects
Amino acid classes are very comprehensive.Detection method step simplicity, understandable, strong operability, while comparing existing national standard side
Method, accuracy, precision and the rate of recovery greatly improve, and the precision of this method is between 0.58-11.15%, the essence of National Standard Method
Density is between 5.05~16.17%.And detection method can Accurate Determining include disposably methionine, half Guang ammonia
The content of 17 kinds of hydrolysis amino acids including acid, tyrosine, phenylalanine and histidine etc..
Because of the particularity of amino acid project, can not implement with the method for the tradition measurement rate of recovery, in order to verify the present invention
The accuracy of detection method, by detection method and National Standard Method to amino acid in the lysozyme of known amino acid theoretical content
Content and the detection comparing result of type be listed in the table below in 2.
Table 2：Detection method and National Standard Method compare the testing result of amino acid content in lysozyme and type
It is analyzed by upper 2 data of table it is found that detection method is compared with National Standard Method, accuracy greatly improves, and detects
Amino acid classes are very comprehensive.Detection method step simplicity, understandable, strong operability, while comparing existing national standard side
Method, accuracy, precision and the rate of recovery greatly improve, and the rate of recovery of this method is between 89-103.2%, the recycling of National Standard Method
Rate is between 51.3~91.7%.And detection method of the invention can Accurate Determining include disposably methionine, half Guang ammonia
The content of 17 kinds of hydrolysis amino acids including acid, tyrosine, phenylalanine and histidine etc..
Comparative example 1
The difference of detection method and embodiment 1 is only that：The sample surveyed is iron-zinc and amino-acids Analysis of Nutritive Composition standard
Substance is evaporated under conditions of on electric hot plate being 40 DEG C and closely does, and triangular flask used is respectively 50mL and 100mL, is consumed
Time and testing result it is as shown in table 3 below.
Table 3：Parameter and experiment result list used when being extracted in comparative example 1
The pre-treatment before upper machine measurement is carried out under the above conditions to same a sample it can be seen from the result of upper table 3
Process, used evaporation utensil is different, not only results in evaporation time and differs nearly 20min, it is often more important that, due to 100mL
Triangular flask for sample size volume it is too big, upper machine liquid cannot add again it is too many (otherwise influence sample finally dilute again
Several and result), so eventually leading to total amino acid precision deviation there are the halfway phenomenon of residual amino acid dissolution and reaching
12.7%, have exceeded detection method requirement.
Since test sample is by iron-zinc and amino-acids Analysis of Nutritive Composition standard substance (State center for standard matter is purchased), ammonia
Base acid total amount standard value is 25.5g/100g, so using the triangle of the triangular flask ratio 100mL of 50mL under the conditions of above-mentioned 40 DEG C
The total amino acid content rate of recovery that bottle obtains will be higher by very much.Therefore, it is preferred to use capacity is that the triangular flask of 5~50mL is heated
Evaporation.
In addition, heating evaporation under the conditions of temperature is 40 DEG C, the influence to the rate of recovery and precision of final detection result
Less, mainly detection efficiency will be greatly reduced.
Comparative example 2
The difference of detection method and embodiment 1 is only that：The sample surveyed is iron-zinc and amino-acids Analysis of Nutritive Composition standard
Substance is evaporated under conditions of on electric hot plate being 70 DEG C and closely does, and triangular flask used is respectively 50mL and 100mL, is consumed
Time and testing result it is as shown in table 4 below.
Table 4：Parameter and experiment result list used when being extracted in comparative example 2
The pre-treatment before upper machine measurement is carried out under the above conditions to same a sample it can be seen from the result of upper table 4
Process, used evaporation utensil is different, and the influence caused by evaporation time is simultaneously little.Importantly, in 70 DEG C of condition
Under when being evaporated, evaporating temperature is excessively high, so that sample segment is inevitably present the burnt phenomenon of paste, and then leads to whole detection
Accuracy is all greatly reduced.
Since test sample is by iron-zinc and amino-acids Analysis of Nutritive Composition standard substance (State center for standard matter is purchased), ammonia
Base acid total amount standard value is 25.5g/100g, so the triangular flask of 50mL and the triangular flask of 100mL obtain under the conditions of above-mentioned 70 DEG C
The total amino acid content rate of recovery arrived is all very low, only 60% hereinafter, seriously affecting the accuracy of testing result.Therefore, most
Fortunately it is evaporated under conditions of 50~60 DEG C, if the temperature of evaporation process is excessively high, the accuracy of detection method and the rate of recovery will
It is greatly reduced.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It can be combined in any suitable manner in one or more embodiment or examples.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples
It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (9)
1. the preparation method of amino acid extracting solution in a kind of feed, which is characterized in that including：
(1) the HCL solution of feed to be measured and 6mol/L is placed in hydrolysis pipe and carries out mixed processing；
By 3~4 drop phenol be added dropwise hydrolysis pipe in mixed material in, backward hydrolysis pipe in be full of nitrogen, then will hydrolyze
Pipe carries out sealing treatment；
Mixed material in the hydrolysis pipe of sealing is hydrolyzed；
(2) will be filtered after hydrolysis process product pure water constant volume, filtrate be placed in triangular flask, by be contained with filtrate 5~
The triangular flask of 50mL is placed on electric hot plate, and the filtrate in the triangular flask is evaporated under conditions of temperature is 50~60 DEG C
Processing；
(3) evaporation process product is diluted processing, the dilution processing is by being added into evaporation process product
What the HCL solution of 0.02mol/L carried out, to obtain the extracting solution.
2. the method according to claim 1, wherein the hydrolysis process is the item for being 109~111 DEG C in temperature
It is carried out 22~24 hours under part.
3. the method according to claim 1, wherein further comprising before dilution processing：
It is added pure water into evaporation process product, repeated evaporation 2~3 times.
4. the method according to claim 1, wherein the feed to be measured be 30~50mg, the 6mol/L's
The volume of HCL solution is 10~15mL, and the volume after the constant volume is 50mL, and the filtrate is 2~3mL.
5. the preparation method of amino acid extracting solution in a kind of feed, which is characterized in that including：
(1) the HCL solution of 30~50mg feed to be measured and 10~15mL 6mol/L is placed in hydrolysis pipe and is carried out at mixing
Reason；
By 3~4 drop phenol be added dropwise hydrolysis pipe in mixed material in, backward hydrolysis pipe in be full of nitrogen, then will hydrolyze
Pipe carries out sealing treatment；
Mixed material in the hydrolysis pipe of sealing is carried out to hydrolysis in 22~24 hours under conditions of temperature is 109~111 DEG C
Processing；
(2) it is filtered after hydrolysis process product being settled to 50mL with pure water, 2~3mL filtrate is taken to be placed in the triangular flask of 5~50mL
In, the triangular flask for being contained with filtrate is placed on electric hot plate, the item for being 50~60 DEG C in temperature by the filtrate in the triangular flask
Processing is evaporated under part；
(3) evaporation process product is diluted processing, the dilution processing is by being added into evaporation process product
What the HCL solution of 0.02mol/L carried out, to obtain the extracting solution.
6. according to the method described in claim 5, it is characterized in that：Before the dilution processing, further comprise：
It is added pure water into evaporation process product, repeated evaporation 2~3 times.
7. a kind of method of amino acid in detection feed, which is characterized in that including：
Extracting solution is obtained using the described in any item methods of claim 1~6；And
It is detected based on the extracting solution, to obtain the type and content of amino acid in the feed.
8. the method according to the description of claim 7 is characterized in that the detection is carried out by amino-acid analyzer.
9. according to the method described in claim 8, it is characterized in that, the amino-acid analyzer uses Na+Exchange column, column temperature are
135℃。
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| CN110426262A (en) * | 2019-09-04 | 2019-11-08 | 四川轻化工大学 | Amino acid sample treatment equipment and detection method |
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