CN106970168A - The method that DART MS methods quickly determine the amino acid in black garlic - Google Patents
The method that DART MS methods quickly determine the amino acid in black garlic Download PDFInfo
- Publication number
- CN106970168A CN106970168A CN201710302702.9A CN201710302702A CN106970168A CN 106970168 A CN106970168 A CN 106970168A CN 201710302702 A CN201710302702 A CN 201710302702A CN 106970168 A CN106970168 A CN 106970168A
- Authority
- CN
- China
- Prior art keywords
- sample
- black garlic
- amino acid
- dart
- quickly determine
- 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
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses a kind of method that DART MS methods quickly determine the amino acid in black garlic, comprise the following steps：（1）Sample pre-treatments；（2）Sample introduction is analyzed；（3）Qualitative and quantitative analysis.Beneficial effects of the present invention：In the present invention, sample-pretreating method simple and fast；Sample introduction analyze speed is fast, and the measure of 4 samples can be achieved in 5min；The rapid screening of amino acid classes and sxemiquantitative in black garlic sample can be achieved.
Description
Technical field
The present invention relates to a kind of method that DART-MS methods quickly determine the amino acid in black garlic, belong to chromatography of ions detection
Field.
Background technology
Black garlic also known as black garlic, fermenting black garlic, are that with fresh raw garlic, belt leather is placed in hot and humid fermenting case natural
The food of fermentation, it makes anti-oxidant, the anti-acid work(of uncooked garlic on the basis of the original composition of uncooked garlic, function is retained
Effect improves decades of times, and the protein of uncooked garlic in itself is largely transformed into human body necessary amino acid daily, and then
Absorbed rapidly by human body, to enhancing body immunity, recover human-body fatigue, keep health to play huge positive role, be
The health food of quick-acting.Main nutrient composition amino acid in black garlic is larger because of the different difference of the place of production and zymotechnique.Mesh
Before, the method that predominantly detects of amino acid is amino acid determining instrument method, and operating procedure is relatively complicated, costly.In recent years, it is various
The black garlic product of various kinds enters the market, so a kind of method of amino acid in quick detection black garlic is set up, to maintaining black garlic market good
Development and guarantee human health are significant.
The content of the invention
The technical problems to be solved by the invention are：A kind of DART-MS methods are provided and quickly determine amino acid in black garlic
Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
The method that DART-MS methods quickly determine the amino acid in black garlic, it is characterised in that comprise the following steps：
(1) sample pre-treatments；(2) sample introduction is analyzed；(3) qualitative and quantitative analysis.
The step of sample pre-treatments, is as follows：Black garlic is shelled, and fragment is cut into scissors, is placed in Yan Portland and is ground to form pureed；It is accurate
5.00g really is weighed in centrifuge tube, 50ml is added water to, 30min is vibrated, then ultrasound 20min, finally centrifuges 5min (5000r/
Min), it is to be measured.
The step of sample introduction is analyzed is as follows：
1. DART sources (Ion Sense)；400 DEG C of temperature；Point-to-point speed 0.2mm/s；Working gas：Helium (5-
5.5psi)；Positive ion mode；
②4000Q trap MS/MS(AB)；CUR 10psi；Scanning range 100-300Da；Sweep time：0.5s；
3. the μ L of testing sample 5 are taken with liquid-transfering gun (0-10 μ L ranges), uniform point is at the tip of glass rod, and position is put in holding
The uniformity put, direct injection analysis.
Beneficial effects of the present invention：
In the present invention, sample-pretreating method simple and fast；Sample introduction analyze speed is fast, achievable 4 samples in 5min
Determine；The rapid screening of amino acid classes and sxemiquantitative in black garlic sample can be achieved.
Brief description of the drawings
The embodiment to the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is black garlic sample total ion chromatogram.
Fig. 2 is black garlic sample A amino acid detection mass spectrogram.
Fig. 3 is black garlic sample B amino acid detection mass spectrogram.
Fig. 4 is black garlic sample C amino acid detection mass spectrogram.
Fig. 5 is black garlic sample D amino acid detection mass spectrogram.
Embodiment
Embodiment 1
The method that the DART-MS methods that the present embodiment is provided quickly determine the amino acid in black garlic, it is characterised in that including under
Row step：
(1) sample pre-treatments；(2) sample introduction is analyzed；(3) qualitative and quantitative analysis.
The step of sample pre-treatments, is as follows：Black garlic is shelled, and fragment is cut into scissors, is placed in Yan Portland and is ground to form pureed；It is accurate
5.00g really is weighed in centrifuge tube, 50ml is added water to, 30min is vibrated, then ultrasound 20min, finally centrifuges 5min (5000r/
Min), it is to be measured.
The step of sample introduction is analyzed is as follows：
1. DART sources (Ion Sense)；400 DEG C of temperature；Point-to-point speed 0.2mm/s；Working gas：Helium (5-
5.5psi)；Positive ion mode；
②4000Q trap MS/MS(AB)；CUR 10psi；Scanning range 100-300Da；Sweep time：0.5s；
3. the μ L of testing sample 5 are taken with liquid-transfering gun (0-10 μ L ranges), uniform point is at the tip of glass rod, and position is put in holding
The uniformity put, direct injection analysis.
The actual sample of embodiment 2 is detected
Different black garlic samples are taken, labeled as sample A, B, C, D, is detected, found after measured as described in Example 1,
Variety classes amino acid response modes on mass spectrum are different, can be summarized as two classes：[M (parent ion)+H]+pattern and [M+Na]+mould
Formula, partial amino-acid (example：Leucine) both of which has response.Different aminoacids response modes are shown in Table 1 in black garlic sample.
Different aminoacids DART-MS methods response modes are distributed in the black garlic of table 1
Note * N (no response)
Fig. 1 is black garlic sample total ion chromatogram (4 pins difference sample).Fig. 2-5 is black garlic sample A, B, C, D respectively
Amino acid detects mass spectrogram.
Analyze after testing, find black garlic sample in mainly contain leucine, lysine, glutamic acid, valine, alanine,
The amino acid such as tyrosine, tryptophan, cystine, phenylalanine, proline, content and species because sample is different and it is different.It is contained
The content of amino acid can be according to the elevation measurement of appearance.
The above described is only a preferred embodiment of the present invention, being not the limitation for making other forms to the present invention, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
Imitate embodiment.But it is every without departing from technical solution of the present invention content, the technical spirit according to the present invention is to above example institute
Any simple modification, equivalent variations and the remodeling made, still fall within the protection domain of technical solution of the present invention.
Claims (3)
1. the method that DART-MS methods quickly determine the amino acid in black garlic, it is characterised in that comprise the following steps：
（1）Sample pre-treatments；（2）Sample introduction is analyzed；（3）Qualitative and quantitative analysis.
2. according to the method described in claim 1, it is characterised in that as follows the step of sample pre-treatments：Black garlic is shelled, and uses scissors
Fragment is cut into, is placed in Yan Portland and grinds to form pureed；5.00g accurately is weighed in centrifuge tube, 50ml is added water to, and vibrates 30min, so
Ultrasound 20min, finally centrifuges 5min afterwards（5000r/min）, it is to be measured.
3. according to the method described in claim 1, it is characterised in that the step of sample introduction is analyzed is as follows：
1. DART sources（Ion Sense）；400 DEG C of temperature；Point-to-point speed 0.2mm/s；Working gas：Helium（5-5.5 psi）；
Positive ion mode；
② 4000 Q trap MS/MS(AB)；CUR 10 psi；Scanning range 100-300Da；Sweep time：0.5s；
3. liquid-transfering gun is used（0-10 μ L ranges）The μ L of testing sample 5 are taken, uniform point is at the tip of glass rod, and position is put in holding
Uniformity, direct injection analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710302702.9A CN106970168A (en) | 2017-05-03 | 2017-05-03 | The method that DART MS methods quickly determine the amino acid in black garlic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710302702.9A CN106970168A (en) | 2017-05-03 | 2017-05-03 | The method that DART MS methods quickly determine the amino acid in black garlic |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106970168A true CN106970168A (en) | 2017-07-21 |
Family
ID=59330201
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710302702.9A Pending CN106970168A (en) | 2017-05-03 | 2017-05-03 | The method that DART MS methods quickly determine the amino acid in black garlic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106970168A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104597106A (en) * | 2014-12-24 | 2015-05-06 | 江苏科技大学 | Method for measuring activity of glutamic-pyruvic transaminase based on DART-MS/MS |
| CN105158391A (en) * | 2015-09-06 | 2015-12-16 | 天津师范大学 | Establishment method of inducing callus cultured Allium sativum L. allinase inactivation extract HPLC fingerprint |
| JP6101385B2 (en) * | 2015-04-24 | 2017-03-22 | 株式会社 資生堂 | Analysis method |
-
2017
- 2017-05-03 CN CN201710302702.9A patent/CN106970168A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104597106A (en) * | 2014-12-24 | 2015-05-06 | 江苏科技大学 | Method for measuring activity of glutamic-pyruvic transaminase based on DART-MS/MS |
| JP6101385B2 (en) * | 2015-04-24 | 2017-03-22 | 株式会社 資生堂 | Analysis method |
| CN105158391A (en) * | 2015-09-06 | 2015-12-16 | 天津师范大学 | Establishment method of inducing callus cultured Allium sativum L. allinase inactivation extract HPLC fingerprint |
Non-Patent Citations (3)
| Title |
|---|
| JUNGMIN LEE 等: "Free amino acid and cysteine sulfoxide composition of 11 garlic (Allium sativum L.) cultivars by gas chromatography with flame ionization and mass selective detection", 《J.AGRIC.FOOD CHEM.》 * |
| KANAKO SEKIMOTO 等: "Ionization characteristics of amino acids in direct analysis in real time mass spectrometry", 《ANALYST》 * |
| 赵岩 等: "非发酵黑蒜的制备及其质量评价", 《食品科技》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103713078B (en) | Amino acid whose assay method in a kind of honey | |
| Tylingo et al. | Isolation and characterization of acid soluble collagen from the skin of african catfish (Clarias gariepinus), salmon (Salmo salar) and baltic cod (Gadus morhua) | |
| CN103543218A (en) | Method for measuring tetracycline antibiotic residue in protein-rich sample | |
| CN106442840B (en) | The assay method of biogenic amine in a kind of cigarette mainstream flue gas | |
| CN110850000A (en) | Method for quantifying honey MRJP2 by liquid chromatography-tandem mass spectrometry | |
| CN110850001A (en) | Method for quantifying honey MRJP3 by liquid chromatography-tandem mass spectrometry | |
| CN107014957B (en) | Method for rapidly judging donkey skin quality by using odor components | |
| Sánchez-Machado et al. | High-performance liquid chromatographic analysis of amino acids in edible seaweeds after derivatization with phenyl isothiocyanate | |
| CN116087401A (en) | Detection method of rice target fragrant substances | |
| CN102241730A (en) | Extraction and dielectrophoresis analytical method for total protein of cattail cauloid | |
| CN106970168A (en) | The method that DART MS methods quickly determine the amino acid in black garlic | |
| CN113804806A (en) | Ultra-high performance liquid chromatography-tandem mass spectrometry determination method for amino acids in bird's nest | |
| CN106841473B (en) | Method for rapidly analyzing content of free amino acid in fresh vegetable sample | |
| CN114894934B (en) | Construction method and application of scorpion medicinal material and formula particle UPLC characteristic spectrum thereof | |
| Jing et al. | Determination of free amino acids in burley tobacco by high performance liquid chromatography | |
| CN106093264A (en) | A kind of assay method of Fructus Fragariae Ananssae Xanthophyll Cycle Components | |
| CN102768282B (en) | Preparation and detection methods of kit for detecting chub vitellogenin (VTG) | |
| CN113429474B (en) | Method for identifying adulteration of vegetable protein meat sample based on characteristic peptide fragment label | |
| CN108709946A (en) | A kind of method of 17 kinds of amino acid in detection food | |
| CN111983061B (en) | Method for detecting aging mode of dried orange peel | |
| Suriyanont et al. | Making process and factors associating to properties of fermented fish (Plara) in some parts of upper northeast area of Thailand | |
| CN113740475A (en) | Construction method of green pepper GC-MC fingerprint | |
| CN109293741B (en) | Polypeptide for identifying donkey-hide gelatin and horse hide derived components in donkey-hide gelatin product | |
| Vidyalakshmi et al. | Simultaneous determination of 17 amino acids in microbial pigments from Monascus spp by UHPLC amino acid analyser using pre-column derivatization | |
| CN116087399A (en) | Application of chicken's gizzard-membrane specific polypeptide in identifying chicken's gizzard-membrane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170721 |