CN101509901B - Method for analyzing origin of amino acid in brewed sauce - Google Patents
Method for analyzing origin of amino acid in brewed sauce Download PDFInfo
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- CN101509901B CN101509901B CN2009100253413A CN200910025341A CN101509901B CN 101509901 B CN101509901 B CN 101509901B CN 2009100253413 A CN2009100253413 A CN 2009100253413A CN 200910025341 A CN200910025341 A CN 200910025341A CN 101509901 B CN101509901 B CN 101509901B
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- 150000001413 amino acids Chemical class 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 16
- 235000015067 sauces Nutrition 0.000 title 1
- 235000013555 soy sauce Nutrition 0.000 claims abstract description 30
- 238000004458 analytical method Methods 0.000 claims abstract description 23
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 11
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 11
- 238000005516 engineering process Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000012545 processing Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- ONIBWKKTOPOVIA-UHFFFAOYSA-N Proline Natural products OC(=O)C1CCCN1 ONIBWKKTOPOVIA-UHFFFAOYSA-N 0.000 claims description 6
- 238000000825 ultraviolet detection Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- QEVHRUUCFGRFIF-MDEJGZGSSA-N reserpine Chemical compound O([C@H]1[C@@H]([C@H]([C@H]2C[C@@H]3C4=C(C5=CC=C(OC)C=C5N4)CCN3C[C@H]2C1)C(=O)OC)OC)C(=O)C1=CC(OC)=C(OC)C(OC)=C1 QEVHRUUCFGRFIF-MDEJGZGSSA-N 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 238000004364 calculation method Methods 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 6
- 238000011084 recovery Methods 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 235000011194 food seasoning agent Nutrition 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 7
- 235000010469 Glycine max Nutrition 0.000 description 3
- 244000068988 Glycine max Species 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 1
- 239000004472 Lysine Substances 0.000 description 1
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- 230000000739 chaotic effect Effects 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 235000021107 fermented food Nutrition 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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Abstract
The invention discloses a method for analyzing the source of amino acid in brewed soy sauce, belonging to an analysis method of seasoning quality. The proportions between various amino acids and the total amino acids are established by selecting a sample, reasonably processing the sample, and adopting an amino acid analysis technology, thereby determining the source of protein. The method has the beneficial effects that: the addition of non-brewing compositions can be effectively found by detecting the content of the amino acid in the soy sauce, which is far from being solved only by detecting amino acid nitrogen; and the processing technology of the sample improves the determination accuracy and the recovery rate of the sample. The analysis method has lower detection limit and higher sensitivity.
Description
Technical field
The present invention relates to seasoning class attributional analysis method, specifically is the method for origin of amino acid during a kind of analysis makes soy sauce.
Background technology
Protein raw material is the important source material that makes soy sauce and produce, and Chinese over the past thousands of years traditional dregs of beans that rolls behind the oil with soybean or soybean that makes soy sauce always is a raw material, undergoes microbial fermentation and produces the fermented food with strong color, smell and taste characteristic.But continuing to bring out along with amino acid and Related product in recent years; Protein source in the soy sauce takes place chaotic; Only measure in existing determining N of amino acid method under the situation of amino-acid nitrogen (GB18186-2000 " making soy sauce "), the quality that makes soy sauce is difficult to control.
The amino acid analysis technology; Be to be used for the technical skill that working sample amino acid is formed after liquid chromatography separation and the detection technique development; In a lot of food service industrys and fine chemistry industry industry, be able to use; It is modal to be to use post-column derivation technology, but the application in soy sauce manufacture and quality control is also rarely found, does not appear in the newspapers as yet in particular for the judgement of protein source.
Summary of the invention
The method that the present invention provides a kind of analysis to make soy sauce middle origin of amino acid; Purpose is the otherness of forming to amino acid in the protein source in the commercial soy sauce; The characteristics that amino acid is formed in confirming to make soy sauce through the amino acid analysis technology, and judge the rationality of protein source in the different samples as comparison.
The present invention realizes with following technical scheme: the method for protein source during a kind of analysis makes soy sauce; Through selection to sample, the reasonable processing of sample, and adopt the amino acid analysis technology; Set up the proportionate relationship of each seed amino acid and total amino acid, confirm protein source; Specifically:
1) selection of sample: the benchmark raw material selects for use hair oil in the production run as sample, and other sample markets sampling are sampled from market, comprise the soy sauce that national most of areas is produced, and have certain general character to guarantee the result;
2) processing of sample: mix with isopyknic soy sample with 5% trichloroacetic acid, precipitate centrifugally after 1 hour, get supernatant, filter subsequent use;
3) amino acid analysis: use deriving technology; Equipment choosing Agilent 1100 liquid chromatographs, the operation of equipment condition is: Agilent 1100 liquid chromatograph analyses, hypersil ODS C184.6 * 250mm post OPA derives automatically; 40 ℃ of column temperatures; Flow velocity 1.0ml/min, ultraviolet detection 338nm automatically switches to 262nm and is used to detect proline during 22.5min;
The amino acid analysis condition:
(1) chromatographic column: Agilent 1100 liquid chromatograph analyses, hypersil ODS C184.6 * 250mm post OPA derives automatically, 40 ℃ of column temperatures, flow velocity 1.0ml/min, ultraviolet detection 338nm automatically switches to 262nm and is used to detect proline during 22.5min.The gradient elution program is seen table 1.
I. table 1
(2) elution requirement and moving phase
(A)：0.05mol/L?NaAc+0.5％THF；
(B): methyl alcohol
The processing of data: Agilent workstation
The method validation verification:
The typical curve correlation test is example with lysine: as horizontal ordinate, peak face area score value Y carries out linear regression as ordinate with amino acid content X (mg/mL), gets typical curve.Equation of linear regression is Y=5337.9X+4761.9, R
2=0.999, the range of linearity is 0.05～5mg/mL.
Recovery experiment: in sample solution, add a certain amount of amino acid standard items, dilute behind the suitable multiple, measure its content, calculate average recovery by above-mentioned chromatographic condition sample introduction, recovery average out to 98.85%, the result is shown in chart 2.
The mensuration of the table 2 method recovery
The precision experiment:
Get variable concentrations 17 in mixed standard solution, after deriving by selected method, in a few days measure 5 times; In 5 days every day measure in 17 the variable concentrations mixed standard solution each once, the average coefficient of variation of gained (CV): in a few days 4.01%, 3.50%; 2.98%, 2.50%, 4.03%; In the daytime be: 7.67%, 9.84%, 5.88%, 2.62%, 5.09%, The above results shows that the precision of this method is better.
The invention has the beneficial effects as follows: can effectively find to add the non-composition of brewageing through content of amino acids in the detection soy sauce, and this point is to be indeterminable through detecting amino-acid nitrogen only far away.The treatment technology of sample has improved the accuracy and the recovery of sample determination.This method detection limit is lower, and higher sensitivity is arranged.
Description of drawings
The amino acid collection of illustrative plates of Fig. 1 hair oil;
The amino acid collection of illustrative plates of Fig. 2 commodity soy sauce 1;
The amino acid collection of illustrative plates of Fig. 3 commodity soy sauce 2.
Embodiment
Below in conjunction with specific embodiment the present invention is further specified.
Embodiment
Further specify method of the present invention and effect below in conjunction with embodiment.
Embodiment 1
With the permanent isopyknic soy sauce hair oil sample mix of 5% trichloroacetic acid and Xuzhou along ten thousand logical fermentation food company limiteds; Precipitate centrifugally after 1 hour, get supernatant, filter subsequent use.Use Agilent 1100 liquid chromatograph analyses then, hypersilODS C184.6 * 250mm post OPA derives automatically, 40 ℃ of column temperatures, and flow velocity 1.0ml/min, ultraviolet detection 338nm automatically switches to 262nm and is used to detect proline during 22.5min.The gradient elution program is carried out by last table 1.The amino acid collection of illustrative plates of its hair oil is seen Fig. 1.The testing result of hair oil is seen table 3.
The testing result of table 3 hair oil
Embodiment 2
Mix with isopyknic commodity soy sauce 2 with 5% trichloroacetic acid, precipitate centrifugally after 1 hour, get supernatant, filter subsequent use.Use Agilent 1100 liquid chromatograph analyses then, hypersil ODS C18 4.6 * 250mm post OPA derives automatically, 40 ℃ of column temperatures, and flow velocity 1.0ml/min, ultraviolet detection 338nm automatically switches to 262nm and is used to detect proline during 22.5min.The gradient elution program is carried out by last table 1.The amino acid collection of illustrative plates of commodity soy sauce 1 is seen Fig. 2.The testing result of commodity soy sauce 1 is seen table 4.
The testing result of table 4 commodity soy sauce 1
Embodiment 3
Mix with isopyknic commodity soy sauce 2 with 5% trichloroacetic acid, precipitate centrifugally after 1 hour, get supernatant, filter subsequent use.Use Agilent 1100 liquid chromatograph analyses then, hypersil ODS C184.6 * 250mm post OPA derives automatically, 40 ℃ of column temperatures, and flow velocity 1.0ml/min, ultraviolet detection 338nm automatically switches to 262nm and is used to detect proline during 22.5min.The gradient elution program is carried out by last table 1.Fig. 3 between the amino acid collection of illustrative plates of commodity soy sauce 2.Table 5. between the testing result of commodity soy sauce 2
The testing result of table 5 commodity soy sauce 2
Claims (1)
1. the method in free amino acid source during an analysis makes soy sauce; It is characterized in that utilizing the method for amino acid analysis; Amino acid composition in the product is analyzed, and compares and use the protein raw material production that makes soy sauce always and the amino acid composition that gets, thereby judges the protein source of product; Concrete grammar is following:
1) select sample: the benchmark raw material selects for use hair oil in the production run as sample, and other sample markets sampling are sampled from market, comprise the soy sauce that national most of areas is produced, and have certain general character to guarantee the result;
2) processing of sample: mix with isopyknic soy sample with 5% trichloroacetic acid, precipitate centrifugally after 1 hour, get supernatant, filter subsequent use;
3) amino acid analysis: use deriving technology, select Agilent 1100 liquid chromatographs for use, the amino acid analysis condition is:
(1) chromatographic column: Agilent 1100 liquid chromatograph analyses, hypersil ODS C184.6 * 250mm post OPA derives automatically, 40 ℃ of column temperatures, flow velocity 1.0ml/min, ultraviolet detection 338nm automatically switches to 262nm and is used to detect proline during 22.5min;
(2) elution requirement and moving phase; Moving phase is made up of A and B, and A is 0.05mol/L NaAc+0.5%THF; B is a methyl alcohol;
The gradient elution program is seen table 1
Table 1
4) processing of data: Agilent workstation; Draw amino acid component law wherein through data processing, be very easy to find, and tabulate according to the ratio calculation of every seed amino acid content and total amino acid content if added the protein source of other types in process of production.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100253413A CN101509901B (en) | 2009-03-11 | 2009-03-11 | Method for analyzing origin of amino acid in brewed sauce |
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| CN2009100253413A CN101509901B (en) | 2009-03-11 | 2009-03-11 | Method for analyzing origin of amino acid in brewed sauce |
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| CN101509901B true CN101509901B (en) | 2012-01-25 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101793642B (en) * | 2009-12-17 | 2011-09-07 | 东北农业大学 | Separation and liquid chromatography column pre-column derivatization method of biogenic amine in soybean paste |
| CN103163249B (en) * | 2013-03-21 | 2014-04-16 | 佛山市海天调味食品股份有限公司 | Method for fast identifying fermented soy sauce and blended soy sauce |
| CN103207251B (en) * | 2013-03-21 | 2014-08-27 | 佛山市海天调味食品股份有限公司 | Quick blended soy sauce judging method |
| CN103163248B (en) * | 2013-03-21 | 2014-05-28 | 佛山市海天调味食品股份有限公司 | Method for identifying blended soy sauce |
| CN103163269B (en) * | 2013-03-21 | 2014-12-17 | 佛山市海天调味食品股份有限公司 | Method for fast identifying fermented soy sauce and blended soy sauce |
| CN110632227B (en) * | 2019-09-12 | 2022-03-18 | 中南林业科技大学 | Method for distinguishing Liuyang fermented soya beans, Yangjiang fermented soya beans and Yongchuan fermented soya beans |
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