CN103197022A - Method for detecting amino acid contained in table vinegar - Google Patents

Method for detecting amino acid contained in table vinegar Download PDF

Info

Publication number
CN103197022A
CN103197022A CN2013101454115A CN201310145411A CN103197022A CN 103197022 A CN103197022 A CN 103197022A CN 2013101454115 A CN2013101454115 A CN 2013101454115A CN 201310145411 A CN201310145411 A CN 201310145411A CN 103197022 A CN103197022 A CN 103197022A
Authority
CN
China
Prior art keywords
channel
amino acid
phase ratio
vinegar
accounts
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN2013101454115A
Other languages
Chinese (zh)
Inventor
梁宝爱
张素娟
姚春孝
武向勇
刘玉玲
孙丽萍
贾策
赵海霞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SHANXI INSTITUTE OF FOOD QUALITY SUPERVISION INSPECTION AND RESEARCH
Original Assignee
SHANXI INSTITUTE OF FOOD QUALITY SUPERVISION INSPECTION AND RESEARCH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SHANXI INSTITUTE OF FOOD QUALITY SUPERVISION INSPECTION AND RESEARCH filed Critical SHANXI INSTITUTE OF FOOD QUALITY SUPERVISION INSPECTION AND RESEARCH
Priority to CN2013101454115A priority Critical patent/CN103197022A/en
Publication of CN103197022A publication Critical patent/CN103197022A/en
Pending legal-status Critical Current

Links

Images

Landscapes

  • Investigating Or Analysing Biological Materials (AREA)

Abstract

The invention discloses a method for detecting amino acid contained in table vinegar. The method for detecting amino acid contained in table vinegar comprises the steps of: (1) distilling and extracting steam for a to-be-detected sample of table vinegar; (2) extracting and purifying an extractive in the step (1) by using a solid phase extraction column; (3) detecting a purified product of the step (2) by utilizing an ion chromatography-electrochemical detector, thereby obtaining the chromatogram map of the amino acid contained in the test sample of the table vinegar; (4) preparing 18 amino acid standard solutions, and carrying out ion chromatography analysis to obtain a chromatogram map of the 18 amino acid standard solutions; and (5) comparing the chromatogram maps respectively obtained in the step (3) and the step (4), thereby obtaining the types of amino acid contained in the test sample of table vinegar. The method for detecting amino acid contained in table vinegar provided by the invention has the advantages that an efficient, accurate and flexible analysis method for detecting 18 amino acid in the table vinegar by combining extraction with a distillation method, purification with a strong cation solid phase extraction column (SCX, strong cation exchanger) and an ion chromatography-electrochemical detector is established.

Description

A kind ofly detect method amino acid contained in the vinegar
Technical field
The invention belongs to the food inspection technical field, be specifically related to a kind of method amino acid contained in the vinegar that detects, relate to the method that the way of distillation, solid-phase extraction column extraction and cleaning and chromatography of ions-electrochemical detector coupling technique detects amino acid content in the vinegar more specifically.
Background technology
Vinegar is as a kind of flavouring, and is necessary by people in daily life; Along with vinegar have such as eliminating tired, anti-ageing and softening blood vessel, reducing blood lipid, the highlighting of health-care effects such as reduction cholesterol, it is more and more important that vinegar also seems in life.The protein that contains 0.05%-3% in the vinegar contains 8 kinds of amino acid/11s, and wherein 8 seed amino acids of needed by human all possess.The delicious flavour of vinegar, the smell of vinegar is mellow and full, soft, and these all are amino acid whose contributions.Several amino acids is mixed the delicious food and the organic acid tart flavour that produce vinegar and is mixed the fragrance that produces vinegar.
Vinegar has making vinegar and preparation of vinegar by the production technology branch: it is to be used alone or as a mixture various material or the alcohol that contain starch, sugar, the liquid flavoring that forms through the microbial fermentation brew that (1), making vinegar define in the GB18187-2000 national standard; Its zymotechnique is divided into two classes: a class is the solid state fermentation vinegar, and another kind of is liquid fermentation edible vinegar; (2), preparation of vinegar defines in SB10337-2000 Ministry of Commerce standard is based on making vinegar, the flavouring edible vinegar that forms with mixed preparing such as glacial acetic acid, food additives, and the ratio (with Acetometer) of making vinegar must not be less than 50% in the preparation of vinegar.
Because the making vinegar cycle is long, cost is high, the standard of China is relatively backward in addition, make some unprincipled fellows have an opportunity to take advantage of, blending into preparation of vinegar with edible ice acetic acid is used for pretending to be making vinegar to seek exorbitant profit, more hateful is, and industrial glacial acetic acid blends into this vinegar inferior of artificial vinegar (abbreviation synthetic vinegar) does not only have nutritive value, and serious harm is healthy.
According to existing national standard, the physical and chemical index of making vinegar mainly contains: total acid (in Acetometer), fixed acid (with lactic acid), soluble saltless solid can't restrict glacial acetic acid and blend into preparation of vinegar and artificial synthetic vinegar.Make the counterfeiter convert water dilution back with glacial acetic acid and add the physical and chemical index standard that a small amount of making vinegar, caramel colorant, adjuvant etc. just can reach making vinegar, the coat of put on " qualified " is sold, and supervision brings difficulty to food.
Generally by adopting high performance liquid chromatography to measuring to amino acid derived back before the post or behind the post, this method derivative reagent expense is higher for existing detection method, and test operation is complicated, poor stability.Adopt the chromatography of ions to measure amino acid and generally measure by a large amount of dilute samples, sensitivity is lower, and some micro-amino acid can't detect.
Therefore be badly in need of a kind of detection method and come accurately quantitatively to detect the content characteristics index of 18 seed amino acids in the making vinegar, in order to differentiating making vinegar and preparation of vinegar and synthetic vinegar, thereby standard vinegar industry makes its sound development, guarantees the vinegar quality safety.
Summary of the invention
In order to differentiate making vinegar and preparation of vinegar and synthetic vinegar, the objective of the invention is to disclose the method for 18 seed amino acids in a kind of analyzing and testing vinegar, provide a kind of method of utilizing way of distillation enrichment method, solid-phase extraction column extraction and cleaning and chromatography of ions-electrochemical detector coupling technique to detect amino-acid compound in the vinegar specifically, so that amino acid in the vinegar is carried out qualitative and quantitative analysis.
The objective of the invention is to be achieved through the following technical solutions:
A kind ofly detect method amino acid contained in the vinegar, comprise the steps:
(1), the vinegar testing sample is extracted with steam distillation, remove the volatile acid in the testing sample, and amino acid has been carried out enrichment method;
(2), the extract to step (1) carries out extraction and cleaning with solid-phase extraction column;
(3), the purified product of step (2) is detected with chromatography of ions-electrochemical detector, obtain chromatogram amino acid contained in the vinegar sample through after the ion chromatography;
(4), be equipped with 18 seed amino acid standard solution, through after the ion chromatography, obtain 18 seed amino acid standard solution chromatograms, the condition of the ion chromatography in the condition of described ion chromatography and the step (3) is identical;
(5), chromatogram that step (3) and step (4) are obtained respectively contrasts, namely get and contain amino acid whose kind in the vinegar sample;
The process for preparation of 18 seed amino acid standard solution is in the technical program: take by weighing 18 seed amino acid list standard specimens (0.1g) respectively and be mixed with 1000 μ mol/L standard inventory solution with ultrapure water; Measure 18 seed amino acid standard inventory solution 5.0mL respectively, be settled to 100mL with ultrapure water, shake up standbyly, be mixed with 18 seed amino acid standard solution (50 μ mol/L).
The described a kind of method amino acid contained in the vinegar that detects of technique scheme, wherein, the detailed process of step (1) is: draw vinegar sample 2mL and carry out steam distillation, when receiving liquid arrival 180mL, finish distillation, be settled to 10mL with ultrapure water, obtain extract.
The described a kind of method amino acid contained in the vinegar that detects of technique scheme, wherein, the detailed process of step (2) is: the extract of getting 1~2mL step (1) is put into solid-phase extraction column, formic acid solution drip washing pillar with 15~20mL0.02%, remove the sugar alcohol compound in the sample, discard cleansing solution; With 10mL1mol/L ammonia spirit wash-out pillar, whole Solid-Phase Extraction process flow velocity is no more than 1mL/min; Eluent dries up with nitrogen under 50 ℃, with deionized water dissolving and dilution, obtains the purified product for ion chromatography then.
The described a kind of method amino acid contained in the vinegar that detects of technique scheme, wherein, the detailed process of step (3) is: purified product chromatography of ions-electrochemical detector coupling technique that step (2) is obtained detects, and obtains chromatogram amino acid contained in the vinegar sample; Wherein the chromatography of ions condition is chromatographic column: Amino PacPA-10 (2 * 250mm); Sample size: 25 μ L; Analysis time: 52min.
The described a kind of method amino acid contained in the vinegar that detects of technique scheme, wherein, the gradient elution liquid program of described step (3) intermediate ion chromatogram is: flow rate of mobile phase is 0.25ml/min, it is deionized water mutually that A channel flows, the B channel flow is the 250mmol/L sodium hydroxide solution mutually, and it is the 1mol/L sodium acetate solution mutually that C-channel flows; From 0~6min, the mobile phase ratio of A channel accounts for 88%, B channel flow phase ratio and accounts for 12%, and the mobile phase ratio of C-channel accounts for 0, and gradient curve is 5; From 6min~12.10min, the A channel phase ratio that flows drops to 68.0%, B channel flow phase ratio gradually from 88% and rises to 32.0% gradually from 12%, and the C-channel phase ratio that flows accounts for 0, and gradient curve is 5; The phase ratio accounts for 68%, B channel flow phase ratio and accounts for 32% 12.10~16.0min, A channel flow, and the mobile phase ratio of C-channel accounts for 0, and gradient curve is 8; From 16.00min~24.00min, the A channel phase ratio that flows drops to 36.0%, B channel flow phase ratio gradually from 68% and drops to 24.0% gradually from 32%, and the C-channel phase ratio that flows rises to 40% gradually, and gradient curve is 5; From 24.00~39.00min, the mobile phase ratio of A channel accounts for 36%, B channel flow phase ratio and accounts for 24%, and the mobile phase ratio of C-channel accounts for 40%, and gradient curve is 8; From 39.00~39.10min, the A channel phase ratio that flows drops to 20.0%, B channel flow phase ratio from 36% and rises to 80.0% gradually from 24.0%, and the C-channel phase ratio that flows accounts for 0, and gradient curve is 5; From 39.10~41.10min, the mobile phase ratio of A channel accounts for 20%, B channel flow phase ratio and accounts for 80%, and the mobile phase ratio of C-channel accounts for 0, and gradient curve is 8; From 41.10~41.20min, the A channel phase ratio that flows rises to 88.0%, B channel flow phase ratio from 20% and drops to 12.0% gradually from 80.0%, and the C-channel phase ratio that flows accounts for 0, and gradient curve is 5; From 41.20~52.0min, the mobile phase ratio of A channel accounts for 88%, B channel flow phase ratio and accounts for 12%, and the mobile phase ratio of C-channel accounts for 0, and gradient curve is 5.
The present invention has following beneficial effect:
1, the present invention purifies the method that combines with chromatography of ions-electrochemical detector with way of distillation extraction, strong cation solid-phase extraction column (SCX) first, has set up the analytical approach of 18 seed amino acids in efficient, accurate, the sensitive detection vinegar.
2, compare with traditional concentration technique, the present invention adopts part micro-amino acid in the steam distillation enrichment vinegar and removes volatile acid in the vinegar testing sample, makes that final testing result is more accurate; And in the sample that traditional concentration technique is handled, still have a large amount of acetic acid and glucide produces interference to amino acid whose result.
3, the present invention adopts strong cation Solid-Phase Extraction column purification to extract, and effectively improves reappearance, sensitivity and the recovery of amino acid detection method in the vinegar; Adopt electrochemical detector-chromatography of ions in addition, this method is highly sensitive, cost is low, has overcome the many deficiencies in the analytical approach in the past.
4, amino acid whose method development and application in the vinegar disclosed by the invention will be conducive to the production of standard vinegar enterprise, the safety of improving the quality of products, and do Primary Study for discriminating making vinegar, preparation of vinegar and synthetic vinegar simultaneously.Therefore, the present invention has important practical significance for aspects such as promoting China's vinegar industry development and protection consumer's interests.
Description of drawings:
1, Fig. 1 is 18 seed amino acid standard solution chromatograms.
2, Fig. 2 is chromatogram amino acid contained in the vinegar sample.
Embodiment:
For making technical scheme of the present invention be convenient to understand, below in conjunction with concrete test example detection method of the present invention is further described.
Embodiment 1:A kind ofly detect method amino acid contained in the vinegar, comprise the steps:
(1), vinegar testing sample that market is bought extracts with steam distillation, remove the volatile acid in the testing sample, and amino acid carried out enrichment method; Concrete steps are: draw vinegar testing sample 2mL and carry out steam distillation, when receiving liquid arrival 180ml, finish distillation, be settled to 10mL with ultrapure water, obtain extract;
(2), the extract to step (1) carries out extraction and cleaning with solid-phase extraction column, concrete steps are: the extract of getting 1~2mL step (1) is put into solid-phase extraction column, with the formic acid solution drip washing pillar of 15~20mL0.02%, remove the sugar alcohol compound in the sample, discard cleansing solution; With 10mL1mol/L ammonia spirit wash-out pillar, whole Solid-Phase Extraction process flow velocity is no more than 1mL/min; Eluent dries up with nitrogen under 50 ℃, then with deionized water dissolving and be diluted to certain volume, obtains the purified product for ion chromatography;
(3), the purified product to step (2) detects with chromatography of ions-electrochemical detector, obtain chromatogram amino acid contained in the vinegar sample, concrete steps are: purified product chromatography of ions-electrochemical detector coupling technique that step (2) is obtained detects, and wherein the chromatography of ions condition is chromatographic column: Amino Pac PA-10 (2 * 250mm); Sample size: 25 μ L; Analysis time: 52min; The gradient elution liquid program of described chromatography of ions is as shown in table 1; Obtain chromatogram amino acid contained in the vinegar sample, the result as shown in Figure 2, the 1-14 crest that occurs at different time among Fig. 2 represents 14 kinds of different amino acid that contain in the vinegar testing sample respectively;
Table 1 gradient elution liquid setting program
Figure BSA00000883873600051
(4), take by weighing 18 seed amino acid list standard specimens (0.1g) respectively and be mixed with 1000 μ mol/L standard inventory solution with ultrapure water; Measure 18 seed amino acid standard inventory solution 5.0mL respectively, be settled to 100mL with ultrapure water, shake up standby, be mixed with 18 seed amino acid standard solution (50 μ mol/L), with this 18 seed amino acid standard solution through (the chromatography of ions condition is identical with chromatography of ions condition in the step (3)) after ion chromatography, obtain 18 seed amino acid standard solution chromatograms as shown in Figure 1, wherein the 1-18 crest that occurs at different time among Fig. 1 represents 18 kinds of different amino acid respectively: 1, lysine (4.584min), 2, glutamine (6.917min), 3, alanine (9.967min), 4, threonine (10.650min), 5, glycocoll (12.284min), 6, valine (13.784min), 7, serine (16.617min), 8, proline (16.984min), 9, isoleucine (19.750min), 10, leucine (21.084min), 11, methionine (22.150min), 12, histidine (27.867min), 13, phenylalanine (29.434min), 14, glutamic acid (30.52min), 15, aspartic acid (30.984min), 16, cystine (32.317min), 17, tryptophane (35.034min), 18, tyrosine (36.417min);
(5), the crest that occurs at different time among Fig. 1 and Fig. 2 is contrasted, namely get and contain amino acid whose kind in the vinegar sample, through contrasting, the amino acid that contains in the vinegar testing sample among Fig. 2 is: 1, alanine, 2, threonine, 3, glycocoll, 4, valine, 5, serine, 6, proline, 7, isoleucine, 8, leucine, 9, methionine, 10, histidine, 11, phenylalanine, 12, glutamic acid, 13, aspartic acid and 14, tyrosine.
Embodiment 2:Checking to embodiment 1 detection method reliability:
For the detection method of embodiment 1, below by doing typical curve, precision and method recovery test, what this method was described has more high sensitivity, accuracy is better arranged, and estimates to verify the reliability of detection step of the present invention by this.
(1), typical curve:
This method is that the amino acid standard solution of each concentration point with preparation carries out the drawing standard curve by stratographic analysis; Detailed process is as follows:
Take by weighing 18 seed amino acid list standard specimens (0.1g) respectively and be mixed with 1000 μ mol/L standard inventory solution with ultrapure water; Measure 18 seed amino acid standard inventory solution 5.0mL respectively, be settled to 100mL with ultrapure water, shake up standbyly, be mixed with 18 seed amino acid standard intermediate liquids (50 μ mo1/L); Measure 18 seed amino acid standard intermediate liquids and be mixed with a series of 18 seed amino acid standard solution that concentration is 0,1.0,2.0,5.0,8.0,10.0,15.0 μ mol/L respectively, measure for ion chromatograph.Be horizontal ordinate with the concentration of standard solution, peak area is ordinate drawing standard working curve.
With different gradient concentration standard 18 seed amino acid working fluids, do standard solution, be ordinate according to standard solution amino acid chromatogram peak area, amino acid concentration is that horizontal ordinate is made typical curve.
X = A × c × V 1 × 1000 AS × V × 1000 × f . . . . . . ( 1 )
In the formula (1):
Amino acid whose content in the X-sample, unit are every liter of micromole (μ mol/L);
Amino acid whose peak area in the A-sample;
Amino acid whose concentration in the c-standard solution, unit is every liter of micromole (μ mol/L);
V 1The final constant volume of-sample liquid, unit are milliliter (mL);
A sAmino acid whose peak area in the-standard solution;
The volume of V-sample, unit are milliliter (mL);
The f-extension rate.
(2), amino acid precision, determination of recovery rates test behind the adding standard amino acid in testing sample:
Draw and carry out steam distillation after vinegar sample 2.0mL adds 18 seed amino acid mixed standard solutions, 0.04 μ mol, when receiving liquid arrival 180mL, finish distillation, be settled to l0mL with ultrapure water, obtain extract.
Get the lmL extract and put into solid-phase extraction column, with the formic acid solution drip washing pillar of 15~20mL0.02%, remove the sugar alcohol compound in the sample, discard cleansing solution; With l0mLlmol/L ammonia spirit wash-out pillar, whole Solid-Phase Extraction process flow velocity is no more than lmL/min; Eluent dries up with nitrogen under 50 ℃, then with deionized water dissolving and be diluted to certain volume, obtains the purified product for ion chromatography.Carry out 6 replicate determinations, carry out precision and recovery test.
(3), method detection limit, method quantitative limit determination test;
Under above-mentioned testing procedure, the mark-on that carries out vinegar, blank sample after the standard solution serial dilution is reclaimed, sample size is 25 μ L, according to the peak response value of 3 times of noises and the peak response value of 10 times of noises, draws this method detection limit, method quantitative limit.
The linear relationship equation of method, precision and recovery test result see Table 2 respectively, shown in table 3 and the table 4, can be drawn a conclusion from the test of above-mentioned test (1), (2) and (3): 18 seed amino acid typical curve linearly dependent coefficient R 2Greater than 0.99, the method recovery reaches more than 85%; RSD<5.0%, method detection limit are all less than 0.3 μ mol/L, and the method quantitative limit is all less than 0.9 μ mol/L; Satisfy and analyze requirement.
Table 2 each seed amino acid typical curve equation and related coefficient
Sequence number Project The typical curve equation Coefficient R 2
1 Lysine Y=0.202x 0.99917
2 Glutamine Y=0.269x 0.99982
3 Alanine Y=0.446x 0.99982
4 Threonine Y=1.204x 0.99981
5 Glycocoll Y=0.285x 0.99533
6 Valine Y=0.391x 0.99835
7 Serine Y=0.942x 0.99814
8 Proline Y=1.333x 0.99969
9 Isoleucine Y=0.580x 0.99980
10 Leucine Y=0.440x 0.99907
11 Methionine Y=1.172x 0.99925
12 Histidine Y=2.714x 0.99877
13 Phenylalanine Y=0.831x 0.99822
14 Glutamic acid Y=0.056x 0.99955
15 Aspartic acid Y=0.089x 0.99979
16 Cystine Y=1.233x 0.99756
17 Tryptophane Y=0.626x 0.99768
18 Tyrosine Y=1.179x 0.99963
Amino acid precision mensuration behind the mark-on in table 3 making vinegar
Figure BSA00000883873600071
Figure BSA00000883873600081
Table 4 making vinegar recovery of standard addition
Figure BSA00000883873600082
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any formal and substantial restriction, all those skilled in the art, in not breaking away from the technical solution of the present invention scope, when can utilizing the above technology contents that discloses, and a little change of making, modify the equivalent variations with differentiation, be equivalent embodiment of the present invention; Simultaneously, the change of any equivalent variations that all foundations essence technology of the present invention is done above embodiment, modify and differentiation, all still belong in the scope of technical scheme of the present invention.

Claims (5)

1. one kind is detected method amino acid contained in the vinegar, comprises the steps:
(1), the vinegar testing sample is extracted with steam distillation, remove the volatile acid in the testing sample, and amino acid has been carried out enrichment method;
(2), the extract to step (1) carries out extraction and cleaning with solid-phase extraction column;
(3), the purified product of step (2) is detected with chromatography of ions-electrochemical detector, obtain chromatogram amino acid contained in the vinegar sample through after the ion chromatography;
(4), be equipped with 18 seed amino acid standard solution, through after the ion chromatography, obtain 18 seed amino acid standard solution chromatograms, the condition of the ion chromatography in the condition of described ion chromatography and the step (3) is identical;
(5), chromatogram that step (3) and step (4) are obtained respectively contrasts, namely get and contain amino acid whose kind in the vinegar sample.
2. a kind of method amino acid contained in the vinegar that detects according to claim 1 is characterized in that the detailed process of step (1) is: draw vinegar sample 2mL and carry out steam distillation, when receiving liquid arrival 180ml, finish distillation, be settled to 10mL with ultrapure water, obtain extract.
3. a kind of method amino acid contained in the vinegar that detects according to claim 1, it is characterized in that, the detailed process of step (2) is: the extract of getting 1~2mL step (1) is put into solid-phase extraction column, formic acid solution drip washing pillar with 15~20mL0.02%, remove the sugar alcohol compound in the sample, discard cleansing solution; With 10mL1mol/L ammonia spirit wash-out pillar, whole Solid-Phase Extraction process flow velocity is no more than 1mL/min; Eluent dries up with nitrogen under 50 ℃, with deionized water dissolving and dilution, obtains the purified product for ion chromatography then.
4. a kind of method amino acid contained in the vinegar that detects according to claim 1, it is characterized in that, the detailed process of step (3) is: purified product chromatography of ions-electrochemical detector that step (2) is obtained detects, and obtains chromatogram amino acid contained in the vinegar sample; Wherein the chromatography of ions condition is chromatographic column: Amino Pac PA-10 (2 * 250mm); Sample size: 25 μ L; Analysis time: 52min.
5. a kind of amino acid contained method of vinegar that detects according to claim 4, it is characterized in that, the gradient elution liquid program of described step (3) intermediate ion chromatogram is: flow rate of mobile phase is 0.25ml/min, it is deionized water mutually that A channel flows, the B channel flow is the 250mmol/L sodium hydroxide solution mutually, and it is the 1mol/L sodium acetate solution mutually that C-channel flows; From 0~6min, the mobile phase ratio of A channel accounts for 88%, B channel flow phase ratio and accounts for 12%, and the mobile phase ratio of C-channel accounts for 0, and gradient curve is 5; From 6min~12.10min, the A channel phase ratio that flows drops to 68.0%, B channel flow phase ratio gradually from 88% and rises to 32.0% gradually from 12%, and the C-channel phase ratio that flows accounts for 0, and gradient curve is 5; The phase ratio accounts for 68%, B channel flow phase ratio and accounts for 32% 12.10~16.0min, A channel flow, and the mobile phase ratio of C-channel accounts for 0, and gradient curve is 8; From 16.00min~24.00min, the A channel phase ratio that flows drops to 36.0%, B channel flow phase ratio gradually from 68% and drops to 24.0% gradually from 32%, and the C-channel phase ratio that flows rises to 40% gradually, and gradient curve is 5; From 24.00~39.00min, the mobile phase ratio of A channel accounts for 36%, B channel flow phase ratio and accounts for 24%, and the mobile phase ratio of C-channel accounts for 40%, and gradient curve is 8; From 39.00~39.10min, the A channel phase ratio that flows drops to 20.0%, B channel flow phase ratio from 36% and rises to 80.0% gradually from 24.0%, and the C-channel phase ratio that flows accounts for 0, and gradient curve is 5; From 39.10~41.10min, the mobile phase ratio of A channel accounts for 20%, B channel flow phase ratio and accounts for 80%, and the mobile phase ratio of C-channel accounts for 0, and gradient curve is 8; From 41.10~41.20min, the A channel phase ratio that flows rises to 88.0%, B channel flow phase ratio from 20% and drops to 12.0% gradually from 80.0%, and the C-channel phase ratio that flows accounts for 0, and gradient curve is 5; From 41.20~52.0min, the mobile phase ratio of A channel accounts for 88%, B channel flow phase ratio and accounts for 12%, and the mobile phase ratio of C-channel accounts for 0, and gradient curve is 5.
CN2013101454115A 2013-04-25 2013-04-25 Method for detecting amino acid contained in table vinegar Pending CN103197022A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2013101454115A CN103197022A (en) 2013-04-25 2013-04-25 Method for detecting amino acid contained in table vinegar

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2013101454115A CN103197022A (en) 2013-04-25 2013-04-25 Method for detecting amino acid contained in table vinegar

Publications (1)

Publication Number Publication Date
CN103197022A true CN103197022A (en) 2013-07-10

Family

ID=48719713

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2013101454115A Pending CN103197022A (en) 2013-04-25 2013-04-25 Method for detecting amino acid contained in table vinegar

Country Status (1)

Country Link
CN (1) CN103197022A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103995076A (en) * 2014-05-20 2014-08-20 浙江大学 Method for analyzing and detecting trace ammonia nitrogen in complicated matrix by combining fast distillation method with ion chromatography technology
CN105891387A (en) * 2016-05-16 2016-08-24 辽宁润生康泰生物医药科技有限公司 Enrichment method for detecting hydrophilic amino acid
CN109781923A (en) * 2018-12-13 2019-05-21 中华人民共和国日照海关 A kind of method of a variety of amino acid and sugared Rapid Simultaneous Determination in soy sauce
CN110118832A (en) * 2019-04-29 2019-08-13 山西农业大学 Construction method and the application of the organic acid and aroma volatile finger-print of Shanxi mature vinegar
CN110320287A (en) * 2018-03-31 2019-10-11 天津药业研究院有限公司 A kind of tyrosine content and the analysis method in relation to substance

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0346037A1 (en) * 1988-06-07 1989-12-13 Rohm And Haas Company Composite ion-exchange compositions for ion chromatography
US5589069A (en) * 1992-10-05 1996-12-31 Soichi Inoue Method for separating and analyzing ions by electrostatic ion chromatography and a zwitterionic stationary phase for ion chromatography and method for separating and analyzing analytes by multifunctional liquid chromatography

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0346037A1 (en) * 1988-06-07 1989-12-13 Rohm And Haas Company Composite ion-exchange compositions for ion chromatography
US5589069A (en) * 1992-10-05 1996-12-31 Soichi Inoue Method for separating and analyzing ions by electrostatic ion chromatography and a zwitterionic stationary phase for ion chromatography and method for separating and analyzing analytes by multifunctional liquid chromatography

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
国家质量技术监督局: "《中华人民共和国国家标准 酿造食醋 GB18187-2000》", 1 September 2000 *
墨淑敏等: "电化学检测-色谱法测定食醋中氨基酸含量", 《理化检验-化学分册》 *
梁宝爱: "食醋中多种氨基酸检测方法的研究-离子色谱法", 《食品工程》 *
茅端良等: "简易蒸馏装置测定食醋中不挥发酸和挥发酸", 《中国酿造》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103995076A (en) * 2014-05-20 2014-08-20 浙江大学 Method for analyzing and detecting trace ammonia nitrogen in complicated matrix by combining fast distillation method with ion chromatography technology
CN105891387A (en) * 2016-05-16 2016-08-24 辽宁润生康泰生物医药科技有限公司 Enrichment method for detecting hydrophilic amino acid
CN105891387B (en) * 2016-05-16 2018-01-19 辽宁润生康泰生物医药科技有限公司 A kind of enrichment method for being used to detect hydrophilic amino acid
CN110320287A (en) * 2018-03-31 2019-10-11 天津药业研究院有限公司 A kind of tyrosine content and the analysis method in relation to substance
CN109781923A (en) * 2018-12-13 2019-05-21 中华人民共和国日照海关 A kind of method of a variety of amino acid and sugared Rapid Simultaneous Determination in soy sauce
CN110118832A (en) * 2019-04-29 2019-08-13 山西农业大学 Construction method and the application of the organic acid and aroma volatile finger-print of Shanxi mature vinegar
CN110118832B (en) * 2019-04-29 2022-02-11 山西农业大学 Construction method and application of fingerprint of organic acid and volatile aroma components of Shanxi mature vinegar

Similar Documents

Publication Publication Date Title
CN104678044B (en) Reversed-phase high-performance liquid chromatography is utilized to detect the method for tealeaves Free Amino Acids
CN103197022A (en) Method for detecting amino acid contained in table vinegar
CN107202836B (en) Method for rapidly analyzing theanine content in fresh tea sample
CN104502518B (en) A kind of detection method for the treatment of the Chinese medicine preparation of baby anorexia
CN107167532A (en) A kind of method of food additives in use high performance liquid chromatography test food
CN101650347A (en) Method for simultaneously measuring contents of multiple organic acids in feeder acidulant
CN103616448A (en) Method and system for detecting food additive
CN113777190A (en) Method for separating and measuring sanshool content in pepper extract and pepper extract product and application of sanshool content
Huang et al. Simultaneous determination of eight biogenic amines in the traditional Chinese condiment Pixian Douban using UHPLC–MS/MS
CN105021761A (en) Method for determination of a variety of organic acids in grape juice and authenticity of grape juice
CN104820032B (en) Method for detecting ochratoxin A in vegetables and fruits
CN105929044A (en) Method for rapidly detecting hydroxy proline content of milk and dairy products
CN103852531B (en) Method for detecting malto-oligosaccharide in beer through HPLC-ELSD (High-Performance Liquid Chromatography-Evaporative Light Scattering Detector)
CN106248855A (en) One assay method growing tobacco middle biogenic amine
CN105842377A (en) High performance liquid chromatography detection method for pyrazine compounds in Baijiu
CN105717227A (en) Judgment method for flavor quality of concentrated apple juice and application thereof
CN105588900A (en) Compounded amino acid injection 18AA-II content measurement method
CN103344738B (en) Detection method of nine-component heart-calming particle
CN108008060A (en) The assay method and reagent of hydroxyproline in a kind of feed
CN106596765A (en) Method for detecting addition amount of maltodextrin in food materials
CN103278586A (en) Extracting and detecting method for dicyandiamide component in dairy products
CN103743849A (en) Ion chromatography-high resolution mass spectrum hyphenation method for screening and authenticating multiple organic acids in dairy products synchronously and rapidly
CN106841473B (en) Method for rapidly analyzing content of free amino acid in fresh vegetable sample
Fa et al. Color and alcohol removal for the simultaneous detection of amino acids and sugars in wine by two-dimensional ion chromatography
CN115389666A (en) Method for efficiently and simultaneously detecting ergothioneine and ectoine in cosmetics

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C12 Rejection of a patent application after its publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20130710