CN106066367A - The method of nine kinds of Amadori compound concentrations in detection pastry food simultaneously - Google Patents
The method of nine kinds of Amadori compound concentrations in detection pastry food simultaneously Download PDFInfo
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Abstract
nullThe method of nine kinds of Amadori compound concentrations in detection pastry food simultaneously，The present invention is to prepare glycine and glucose Amadori compound、Alanine and glucose Amadori compound、α aminobutyric acid and glucose Amadori compound、Proline and glucose Amadori compound、Aspartic acid and glucose Amadori compound、Isoleucine and glucose Amadori compound、Glutamic acid and glucose Amadori compound、Phenylalanine and glucose Amadori compound、Nine kinds of Amadori compound mixing mother solutions of tryptophan and glucose Amadori compound and sample solution，Prepare standard working solution，Use liquid chromatogram-triple tandem quadrupole mass spectrometer，Analyze detection and obtain nine kinds of Amadori compound concentrations in pastry food sample solution.The inventive method accurately and reliably, highly sensitive, be especially suitable for the analysis of nine kinds of Amadori compounds in complex matrices pastry food.
Description
Technical field
The invention belongs to chemical composition analysis determination techniques field in pastry food, be specifically related to a kind of employing liquid phase color
The method of nine kinds of Amadori compound concentrations in spectrum-tandem mass spectrometry detection pastry food.
Background technology
Amadori compound is reducing sugar (with glucose as representative) and amino-compound (based on aminoacid) generation
The class key that Maillard (non-enzymatic brown) reaction generates asks product 1-amino-1-deoxidation-2-ketose, is that N-replaces
Glucose is reset through Amadori.Amadori rearrangement product can occur under different temperatures and pH value condition further
The reaction that row are complicated, generates and multiple have the micromolecular compound of aromatic odor and have the macromolecular compound of dark brown color
Melanoid, thus affect fragrance and the color of cake food.Amadori is Studies of The Aromatic Substances before an important class, its kind and content
Substantial connection is had with local flavor and the color and luster of food.Or a kind of excellent antioxidant, it is possible to except reactive oxygen free radical, therefore,
Amadori compound in qualitative and quantitative analysis pastry food has important finger to its inherent quality of evaluation and raising fragrance
Lead meaning.
Amadori compound polarity is strong, kind is many, structure is similar, the difficulty of this compounds in qualitative and quantitative analysis food
Spend bigger.At present, analysis for Amadori compound both at home and abroad mainly uses gas chromatography (GC), high performance liquid chromatography
Method (HPLC), LC/MS (LC/MS), liquid chromatography-tandem triple level Four bar mass spectrum (LC-MS/MS) etc., wherein,
LC/MS method and LC-MS/MS method are current maximally effective method for qualitative analysis.For pastry food, its complicated component, if miscellaneous
Matter residual then affects the accuracy of result of the test too much, and therefore, in detection pastry food, Amadori compound needs to carry out greatly
Amount and the bigger pre-treatment work of difficulty, the most not yet have and measure the relevant report of Amadori compound in pastry food.
Summary of the invention
The present invention removes based on liquid chromatography-tandem triple level Four bar mass spectrograph (LC-MS/MS) has common high-efficient liquid phase color
The separation function of spectrometer, has again the high selective advantage of mass ions, it is possible to play the most accurate function when qualitative, quantitative
On the premise of, it is provided that use LC-MS/MS to measure 9 kinds of Amadori compound concentrations in pastry food simultaneously, and accurately and reliably,
Highly sensitive method.
The purpose of the present invention is achieved through the following technical solutions:
The method of nine kinds of Amadori compound concentrations in detection pastry food simultaneously, method step is as follows:
(1) prepare nine kinds of Amadori compound mixing mother solutions: weigh respectively glycine and glucose Amadori compound,
Alanine and glucose Amadori compound, butyrine and glucose Amadori compound, proline and glucose
Amadori compound, aspartic acid and glucose Amadori compound, isoleucine and glucose Amadori compound, paddy
Propylhomoserin and glucose Amadori compound, phenylalanine and glucose Amadori compound, tryptophan and glucose Amadori
Compound standard product 10mg is in 10mL volumetric flask, and each methanol-water using mass concentration 70% dissolves and determines molten, the most each point
Do not pipette the above-mentioned nine kinds of solution of 5mL in 100mL volumetric flask, use that the methanol-water of mass concentration 70% is fixed the most molten obtains nine kinds
Amadori compound mixing mother solution；
(2) standard working solution is prepared: pipette 0.02mL, 0.10mL, 0.20mL, 0.50mL, 1.0mL nine kinds respectively
Amadori compound mixing mother solution, in 10mL volumetric flask, uses the aqueous formic acid constant volume of mass concentration 0.5%, is marked
Quasi-working solution series；In standard working solution series, the concentration of nine kinds of Amadori compounds be respectively 0.10 μ g/mL, 0.50
μg/mL、1.00μg/mL、2.50μg/mL、1.00μg/mL；
(3) sample solution is prepared: carry out the dissolving of Amadori compound in pastry food, extract and purify, specifically walk
Suddenly be to weigh 1.0g pastry food in 50mL centrifuge tube, add 10mL methanol, supersound extraction 10min, 10000r/min from
Heart 5min, supernatant is poured in another centrifuge tube, adds 10mL normal hexane, and vortex 1min, 10000r/min are centrifuged 2min, discard
Upper strata normal hexane layer, adds 10mL normal hexane, and vortex 1min, 10000r/min are centrifuged 2min, discard upper strata normal hexane equally
Layer, lower layer methanol nitrogen under the conditions of 35 DEG C dries up, after adding the aqueous formic acid dissolving of 2mL mass concentration 0.5%, through 0.22
Sample solution is obtained after μm filter membrane；
(4) liquid chromatography-tandem triple level Four bar mass spectral analysis is carried out: use liquid chromatography-tandem triple level Four bar matter
Spectrometer, the liquid chromatograph of analysis detection, Mass Spectrometry Conditions are as follows:
Chromatographic column is WatersAcquity BEH C18 (1.7 μm, 2.1mm × 100mm), column temperature: 25 DEG C；Mobile phase A is
0.5% first aqueous acid, Mobile phase B is methanol solution；Gradient elution, condition is 0～10min:95%A～0%A, 10.1
～14min:0%A, 14.1～18min:95%A；Flow velocity: 0.2mL/min, sampling volume 2 μ L；
Ion source: use electron spray ionisation source, scan mode is cation scanning, and detection mode is multiple-reaction monitoring MRM,
Electron spray voltage 500V, is dried temperature 325 DEG C, dry gas stream amount 6L/min, sheath temperature 380 DEG C, sheath throughput 10L/
Min, capillary voltage 4000V；
(5) standard curve and result of calculation are drawn: the variable concentrations standard working solution that respectively prepared by aspiration step (2) enters
Row LC-MS/MS analyzes, under the instrument parameter that step (4) determines, with nine kinds of Amadori compound quota ion peak areas pair
Its corresponding mass concentration carries out linear regression, obtains the standard working curve of each target compound；Distinguish aspiration step again
(3) sample solution prepared carries out LC-MS/MS analysis, under the instrument parameter that step (4) determines, obtains nine kinds of Amadoriization
Compound quota ion peak area, substitutes into regression equation, is calculated nine kinds of Amadori compound concentrations in sample solution.
Pastry food of the present invention refers to, with flour or rice flour, sugar, oils and fats, egg, milk as primary raw material, be equipped with
Various adjuvants, stuffing material and flavouring agent, just make type, then through steaming, bake, explode, frying the food that either type is processed into.Described dry
Gas and sheath gas are the nitrogen of purity >=99.99%.
The inventive method has the advantage that
(1) present invention establishes a kind of liquid chromatograph-triple quadrupole bar tandem mass spectrometer and detects in pastry food simultaneously
The method of nine kinds of Amadori compounds, it is possible to it is qualitative, fixed to carry out in pastry food nine kinds of Amadori compounds exactly
Amount；
(2) present invention uses methanol as extraction solution, has simultaneously worked as the effect of precipitating proteins, uses normal hexane to go
Except lipoid material disturbs, it is possible to the interference to detection signal of the effective removal pastry food complex matrices；
(3) present invention uses the selection of BEH C18 chromatographic column and 0.5% aqueous formic acid+methanol as mobile phase, to nine kinds
The separation of Amadori compound has reached excellent separating effect, can realize the qualitative of nine kinds of Amadori compounds in 6min
Analyze and quantitative determination；
(4) detection limit of the present invention is between 0.13 μ g/g～0.70 μ g/g, withinday precision RSD (n=6) 2.44%～
5.79%, day to day precision RSD (n=3) 3.02%～5.97%, good stability, the response rate 80.3%～112.4% it
Between, accuracy is high；Liquid chromatography-tandem triple level Four bar mass spectrograph is simple and quick, accurately and reliably, reproducible.
The inventive method accurately and reliably, highly sensitive, be especially suitable for nine kinds of Amadoriization in complex matrices pastry food
The analysis of compound.
Accompanying drawing explanation
Fig. 1 is total ion current (TIC) figure of nine kinds of Amadori compounds；
Fig. 2 is the MRM figure of glycine and glucose Amadori compound (Fru-Gly) quota ion；
Fig. 3 is the MRM figure of alanine and glucose Amadori compound (Fru-Ala) quota ion；
Fig. 4 is the MRM figure of butyrine and glucose Amadori compound (Fru-Amb) quota ion；
Fig. 5 is the MRM figure of proline and glucose Amadori compound (Fru-Pro) quota ion；
Fig. 6 is the MRM figure of aspartic acid and glucose Amadori compound (Fru-Asn) quota ion；
Fig. 7 is the MRM figure of isoleucine and glucose Amadori compound (Fru-Ile) quota ion；
Fig. 8 is the MRM figure of glutamic acid and glucose Amadori compound (Fru-Glu) quota ion；
Fig. 9 is the MRM figure of phenylalanine and glucose Amadori compound (Fru-Phe) quota ion；
Figure 10 is the MRM figure of tryptophan and glucose Amadori compound (Fru-Trp) quota ion；
Figure 11 is total ion current (TIC) figure of certain cookies；
Figure 12 is the MRM figure of certain cookies isoleucine and glucose Amadori compound (Fru-Ile) quota ion；
Figure 13 is the MRM figure of certain cookies phenylalanine and glucose Amadori compound (Fru-Phe) quota ion；
Figure 14 is the MRM figure of certain cookies tryptophan and glucose Amadori compound (Fru-Trp) quota ion.
Detailed description of the invention
Below by embodiment, the present invention is further described.
A kind of employing liquid chromatography-tandem triple level Four bar mass spectrography detects nine kinds of Amadori in pastry food simultaneously
The method of compound concentration, first prepares following determining instrument and material:
Liquid chromatography-tandem triple level Four bar mass spectrograph (Agilent 1290-6460, the U.S.)；Analytical balance (prunus mume (sieb.) sieb.et zucc. Teller
AB204-S, Switzerland)；Volumetric flask, 10mL, 100mL；Centrifuge tube, 50mL；Deionized water (reaches one-level water in GB/T 6682
Require)；Formic acid (analytical pure, Xilong Chemical Co., Ltd)；Methanol (chromatographically pure, Dikma company)；Normal hexane (chromatographically pure,
Dikma company)；Strata-X-AW solid-phase extraction column (Phenomenex SPE pillar, 60mg/3mL)；High pure nitrogen (purity >=
99.999%, Kunming Mei Saier gas products company limited).
Detection method step is as follows:
(1) nine kinds of Amadori compound mixing mother solutions are prepared: weigh glycine and glucose Amadori compound respectively
(Fru-Gly), alanine and glucose Amadori compound (Fru-Ala), butyrine and glucose Amadori chemical combination
Thing (Fru-Amb), proline and glucose Amadori compound (Fru-Pro), aspartic acid and glucose Amadori chemical combination
Thing (Fru-Asn), isoleucine and glucose Amadori compound (Fru-Ile), glutamic acid and glucose Amadori chemical combination
Thing (Fru-Glu), phenylalanine and glucose Amadori compound (Fru-Phe), tryptophan and glucose Amadori chemical combination
Thing (Fru-Trp) standard substance 10mg is in 10mL volumetric flask, and each methanol-water using mass concentration 70% dissolves and determines molten, then
Each above-mentioned nine kinds of solution of 5mL that pipette respectively are in 100mL volumetric flask, and the methanol-water of employing mass concentration 70% is the most molten obtains nine kinds
Amadori compound mixing mother solution；
(2) standard working solution is prepared: pipette 0.02mL, 0.10mL, 0.20mL, 0.50mL, 1.0mL nine kinds respectively
Amadori compound mixing mother solution, in 10mL volumetric flask, uses the aqueous formic acid constant volume of mass concentration 0.5%, is marked
Quasi-working solution series；In standard working solution series, the concentration of nine kinds of Amadori compounds be respectively 0.10 μ g/mL, 0.50
μg/mL、1.00μg/mL、2.50μg/mL、1.00μg/mL；
(3) sample solution is prepared: carry out the dissolving of Amadori compound in pastry food, extract and purify, specifically walk
Suddenly be to weigh 1.0g pastry food in 50mL centrifuge tube, add 10mL methanol, supersound extraction 10min, 10000r/min from
Heart 5min, supernatant is poured in another centrifuge tube, adds 10mL normal hexane, and vortex 1min, 10000r/min are centrifuged 2min, discard
Upper strata normal hexane layer, adds 10mL normal hexane, and vortex 1min, 10000r/min are centrifuged 2min, discard upper strata normal hexane equally
Layer, lower layer methanol nitrogen under the conditions of 35 DEG C dries up, after adding the aqueous formic acid dissolving of 2mL mass concentration 0.5%, through 0.22
Sample solution is obtained after μm filter membrane；Described pastry food can be based on flour or rice flour, sugar, oils and fats, egg, milk etc.
Want raw material, be equipped with various adjuvant, stuffing material and flavouring agent, just make type, then through steaming, bake, explode, frying the food that either type is processed into
Product；
(4) carry out liquid chromatography-tandem triple level Four bar mass spectrum (LC-MS/MS) to analyze: use liquid chromatography-tandem three
Weight level Four bar mass spectrometer, the liquid chromatograph of analysis detection, Mass Spectrometry Conditions are as follows:
Chromatographic column is WatersAcquity BEH C18 (1.7 μm, 2.1mm × 100mm), column temperature 25 DEG C；Mobile phase A is
The aqueous formic acid of mass concentration 0.5%, Mobile phase B is methanol solution；Gradient elution, condition be 0～10min:95%A～
0%A, 10.1～14min:0%A, 14.1～18min:95%A；Flow velocity: 0.2mL/min, sampling volume 2 μ L；Can be in 6min
Realize qualitative analysis and the quantitative determination of nine kinds of Amadori compounds；
Tandem mass spectrum condition is positive ion mode ionization, and ion source uses electron spray ionisation source (ESI), and scan mode is just
Ion scan, detection mode is multiple-reaction monitoring pattern (MRM), electron spray voltage 500V, is dried temperature 325 DEG C, is dried gas
Flow 6L/min, sheath temperature 380 DEG C, sheath throughput 10L/min, capillary voltage, 4000V.Described dry gas and sheath gas are equal
Nitrogen for purity >=99.99%.
The quasi-molecular ion peak ([M+H] of nine kinds of Amadori compounds+Quasi-molecular ions), taper hole voltage, quota ion, qualitative
Ion, collision energy (CE) see table 1, and nine kinds of Amadori compound standard product total ion current figures and each quota ion MRM figure are shown in
Fig. 1 to Figure 10.
[the M+H]+quasi-molecular ions of each compound of table 1, taper hole voltage, quota ion, qualitative ion, collision energy
(5) standard curve and result of calculation are drawn: the variable concentrations standard working solution that respectively prepared by aspiration step (2) enters
Row LC-MS/MS analyzes, under the instrument parameter that step (4) determines, with nine kinds of Amadori compound quota ion peak areas pair
Its corresponding mass concentration carries out linear regression, obtains the standard working curve of each target compound；Distinguish aspiration step again
(3) sample solution prepared carries out LC-MS/MS analysis, under the instrument parameter that step (4) determines, obtains nine kinds of Amadoriization
Compound quota ion peak area, substitutes into regression equation, is calculated nine kinds of Amadori compound concentrations in sample solution.
The inventive method is done following Method validation: calculate the detection limit of the method respectively with 3 times and 10 times of levels of noise
And quantitative limit.The related data of gained is shown in Table 2.
The linear equation of 2 nine kinds of Amadori compounds of table, correlation coefficient, detection limit, quantitative limit
Selecting a certain cookies sample, after pre-treatment, testing result is for determining containing Fru-Ile, Fru-Phe and Fru-Trp
Three kinds of materials, add high, medium and low three contents levels (0.50 μ g/g, 1.50 μ g/g, 5.00 μ g/g) the most respectively nine kinds
Amadori compound hybrid standard mother solution carries out recovery testu, calculates the response rate；Carry out the in a few days accurate of the method simultaneously
Degree and day to day precision measure, and represent by the relative standard deviation (RSD) of measurement result, are shown in Table 3.
The withinday precision of 3 nine kinds of Amadori compounds of table, day to day precision, the response rate
| Compound | Withinday precision (RSD, n=6) | Day to day precision (RSD, n=3) | The response rate |
| Fru-Gly | 4.23% | 5.76% | 80.3%～112.4% |
| Fru-Ala | 4.38% | 5.93% | 88.1%～99.4% |
| Fru-Amb | 4.31% | 4.48% | 91.0%～106.6% |
| Fru-Pro | 5.31% | 5.97% | 82.1%～98.9% |
| Fru-Asn | 2.86% | 3.03% | 92.5%～102.3% |
| Fru-Ile | 3.92% | 3.69% | 91.1%～99.5% |
| Fru-Glu | 5.79% | 5.12% | 84.5%～108.4% |
| Fru-Phe | 3.46% | 3.02% | 92.0%～95.1% |
| Fru-Trp | 2.44% | 3.49% | 94.1%～104.6% |
Sample determination: a certain cookies sample, schemes (Figure 12, Tu13He from total ion current figure (Figure 11) and the MRM of testing sample
It can be seen that sample has a chromatographic peak and Fru-Ile, Fru-Phe at 2.949min, 3.561min and 4.276min in Figure 14)
Close with the retention time of Fru-Trp, sample characteristic molecular quasi-molecular ions at M/Z=276.1, divides with the feature of Fru-Ile
Daughter ion peak is identical；Sample characteristic molecular quasi-molecular ions at M/Z=310.1, with the characteristic molecular quasi-molecular ions phase of Fru-Phe
With；Sample characteristic molecular quasi-molecular ions at M/Z=349.2 is identical with the characteristic molecular quasi-molecular ions of Fru-Trp；Can determine that sample
Containing Fru-Ile, Fru-Phe and Fru-Trp in product.
In the peak area of Fru-Ile, Fru-Phe and Fru-Trp substitutes into equation of linear regression in sample, i.e. can get sample
In product the concentration of Fru-Ile, Fru-Phe and Fru-Trp be 1.126 μ g/mL, 0.818 μ g/mL and 2.462 μ g/mL, then be multiplied by
Constant volume 2mL, divided by weighing, obtains: this cookies contains Fru-Ile 2.230 μ g/g, Fru-Phe 1.620 μ g/g,
Fru-Trp4.876μg/g。
Claims (3)
- The method of nine kinds of Amadori compound concentrations in detection pastry food the most simultaneously, it is characterised in that method step is such as Under:(1) nine kinds of Amadori compound mixing mother solutions are prepared: weigh glycine and glucose Amadori compound (Fru-respectively Gly), alanine and glucose Amadori compound (Fru-Ala), butyrine and glucose Amadori compound (Fru-Amb), proline and glucose Amadori compound (Fru-Pro), aspartic acid and glucose Amadori compound (Fru-Asn), isoleucine and glucose Amadori compound (Fru-Ile), glutamic acid and glucose Amadori compound (Fru-Glu), phenylalanine and glucose Amadori compound (Fru-Phe), tryptophan and glucose Amadori compound (Fru-Trp) standard substance 10mg is in 10mL volumetric flask, and each methanol-water using mass concentration 70% dissolves and determines molten, respectively Pipette the above-mentioned nine kinds of solution of 5mL respectively in 100mL volumetric flask, use that the methanol-water of mass concentration 70% is fixed the most molten obtains nine kinds Amadori compound mixing mother solution；(2) standard working solution is prepared: pipette nine kinds of Amadori of 0.02mL, 0.10mL, 0.20mL, 0.50mL, 1.0mL respectively Compound mixing mother solution, in 10mL volumetric flask, uses the aqueous formic acid constant volume of mass concentration 0.5%, obtains standard work molten Liquid series；In standard working solution series, the concentration of nine kinds of Amadori compounds be respectively 0.10 μ g/mL, 0.50 μ g/mL, 1.00μg/mL、2.50μg/mL、1.00μg/mL；(3) sample solution is prepared: carry out the dissolving of Amadori compound in pastry food, extract and purify, comprise the concrete steps that Weighing 1.0g pastry food in 50mL centrifuge tube, add 10mL methanol, supersound extraction 10min, 10000r/min is centrifuged 5min, supernatant is poured in another centrifuge tube, adds 10mL normal hexane, and vortex 1min, 10000r/min are centrifuged 2min, discard Layer normal hexane layer, adds 10mL normal hexane, and vortex 1min, 10000r/min are centrifuged 2min, discard upper strata normal hexane layer equally, Lower layer methanol nitrogen under the conditions of 35 DEG C dries up, after adding the aqueous formic acid dissolving of 2mL mass concentration 0.5%, through 0.22 μm Sample solution is obtained after filter membrane；(4) liquid chromatography-tandem triple level Four bar mass spectral analysis is carried out: use liquid chromatography-tandem triple level Four bar mass spectrum to divide Analyzer, the liquid chromatograph of analysis detection, Mass Spectrometry Conditions are as follows:Chromatographic column is WatersAcquity BEH C18 (1.7 μm, 2.1mm × 100mm), column temperature: 25 DEG C；Mobile phase A is 0.5% first aqueous acid, Mobile phase B is methanol solution；Gradient elution, condition is 0～10min:95%A～0%A, 10.1 ～14min:0%A, 14.1～18min:95%A；Flow velocity: 0.2mL/min, sampling volume 2 μ L；Ion source: use electron spray ionisation source, scan mode is cation scanning, and detection mode is multiple-reaction monitoring MRM, EFI Mist voltage 500V, is dried temperature 325 DEG C, dry gas stream amount 6L/min, sheath temperature 380 DEG C, sheath throughput 10L/min, hair Tubule voltage 4000V；(5) standard curve and result of calculation are drawn: the variable concentrations standard working solution that respectively prepared by aspiration step (2) is carried out LC-MS/MS analyzes, under the instrument parameter that step (4) determines, with nine kinds of Amadori compound quota ion peak areas to it Corresponding mass concentration carries out linear regression, obtains the standard working curve of each target compound；Distinguish aspiration step (3) again The sample solution of preparation carries out LC-MS/MS analysis, under the instrument parameter that step (4) determines, obtains nine kinds of Amadori chemical combination Thing quota ion peak area, substitutes into regression equation, is calculated nine kinds of Amadori compound concentrations in sample solution.
- The method of nine kinds of Amadori compound concentrations in the pastry food of detection simultaneously the most according to claim 1, it is special Levying and be, described pastry food refers to, with flour or rice flour, sugar, oils and fats, egg, milk as primary raw material, be equipped with various auxiliary Material, stuffing material and flavouring agent, just make type, then through steaming, bake, explode, frying the food that either type is processed into.
- The method of nine kinds of Amadori compound concentrations in the pastry food of detection simultaneously the most according to claim 1, it is special Levying and be, described dry gas and sheath gas are the nitrogen of purity >=99.99%.
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| CN108614053A (en) * | 2016-12-09 | 2018-10-02 | 内蒙古蒙牛乳业（集团）股份有限公司 | The quick detection of preservative and sweetener in butter or cream |
| CN114609302A (en) * | 2022-04-12 | 2022-06-10 | 河南中烟工业有限责任公司 | Method for monitoring internal quality of fenugreek extract based on HPLC-MS and application |
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