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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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 |
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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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| CN2009100253413A CN101509901B (en) | 2009-03-11 | 2009-03-11 | Method for analyzing origin of amino acid in brewed sauce |
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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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