CN108680690A - It is a kind of fermentation sauce class in tyramine content detection method - Google Patents
It is a kind of fermentation sauce class in tyramine content detection method Download PDFInfo
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Abstract
The present invention provides a kind of detection methods of tyramine content in fermentation sauce class, belong to food analysis technical field.The method is UPLC methods, uses I class Ultra Performance Liquid Chromatography instruments of Waters Acquity, C18 columns.The method of the present invention amount of samples is few, and the time is short, and method is linearly good, easy to operate, favorable reproducibility, and accuracy is high.
Description
Technical field：
The present invention relates to a kind of food detection methods, and in particular to it is a kind of fermentation sauce class in tyramine content ultra high efficiency liquid phase
Chromatographic detection method.
Background technology：
Biogenic amine is mainly by aliphatic (putrescine, cadaverine, spermidine, spermine), aromatic series (tyrasamine, β-phenyl ethylamine) and heterocycle
Race's (tryptamines, histamine) is constituted.Biogenic amine participates in the metabolic activity in organism as a kind of physiological activator.Biogenic amine is wide
It is general to be present in varieties of food items.It is each may to cause headache, dizziness, nausea, respiratory distress, palpitaition etc. for Excess free enthalpy biogenic amine
Kind poisoning symptom.In all biogenic amines, maximum to Human health effects is histamine and tyrasamine.Tyrasamine also known as Uteramin
(Tyramine), it is a kind of nitrogenous low molecular biogenic amine, the tyrasamine in food is mainly the decarboxylation generated by related microorganisms
Enzymatic is sloughed the carboxyl of tyrosine and is generated or aldehyde and ketone pass through amination and transamination generates.Therefore in food
Biogenic amine there are two types of source：One kind coming from raw material, and one is the generations of the decarboxylic reaction of microorganism.In fermented food
The content of biogenic amine is inseparable with microbial action.Because traditional fermentation process is difficult to control, mechanism is not apparent, natural to send out
Biogenic amine problem in ferment food is more paid close attention to by people.Tyrasamine has the function of increasing blood pressure, and the excessive tyrasamine that absorbs can be
Consumption monoamine oxidase inhibitors in vivo, so as to cause serious side effect, the reason of being also known as tyrotoxin here it is tyrasamine.Junket
Amine, which is also manifested by the harm of human body, promotes peripheral vessel to shrink, and irritates heart rate, increases blood sugar concentration, eliminates nervous system
In norepinephrine, to cause migraines.Human oral's tyrasamine, which is more than 100mg, can cause migraine, more than 1080mg
It can cause Poisoning swelling, tyrasamine must not exceed 100-800mg/kg in European Union's regulation food.
The detection method of biogenic amine has gas chromatography tandem mass spectrometry method, the chromatography of ions, high performance liquid chromatography, thin layer
Chromatography, high performance liquid chromatography-tandem mass method, the pre-treatment step of these methods is all relatively complicated, not easy to operate.The present invention
Tyrasamine is measured by ultra-performance liquid chromatography (ultra-performance liquid chromatography, UPLC)
Detection method can obtain better separating effect and shorter analysis time, together by using the chromatographic column of small particle size filler
When simplify pre-treatment step.Therefore the method for the present invention has amount of samples few, and the time is short, and method is linearly good, easy to operate, weight
The advantages that existing property is good, and accuracy is high.
Ferment sauce class be a kind of food with a long history, for going with rice or bread and seasoning, because its unique flavor, delicious flavour,
It is full of nutrition and made and eaten extensively.But the method that the making for sauce class of fermenting generally uses spontaneous fermentation, fermenting microbe are multiple
It is miscellaneous, therefore there are the security risks of higher microbial origin biogenic amine.For food-safe consideration, people should be as far as possible
The intake of biogenic amine is reduced, and it is then an essential ring to detect and monitor the content of biogenic amine in food.Due to junket ammonia
Acid generates tyrasamine during the fermentation, therefore can not only ensure food safety to the analysis of tyrasamine in fermentation sauce class, can be with
It obtains and food production and the relevant useful information of fermentation technology process.
Invention content：
The technical problem to be solved in the present invention is simplified sample pretreatment step, shortens sample detection time, and research is set
Meter rapidly and accurately measures tyramine content in fermentation sauce class using UPLC detection methods.
The purpose of the present invention is achieved through the following technical solutions:
(1) preparation of standard solution：Precision weighs tyrasamine and is made into a concentration of 1.0mgmL with 0.1M hydrochloric acid-1Solution, it is micro-
Filter membrane 0.22 μm of 4 DEG C of filtering in hole saves backup.The gradient standard working solution 0.1M hydrochloric acids used are to required concentration.Essence
The close internal standard that weighs is configured to a concentration of 10 μ gmL with deionized water-1Solution, 4 DEG C of preservations are standby after the filtering of 0.22 μm of miillpore filter
With.
(2) preparation of sample solution：After fermentation sauce class adds trichloroacetic acid refiner to be homogenized 2.0min, on centrifuge
4000rpm centrifuges 10.0min, precipitates 2 times plus trichloroacetic acid is homogenized after centrifuging, merge supernatant trichloroacetic acid constant volume, extract
It is saved backup for 4 DEG C after the 0.22 μm of filtering of liquid miillpore filter.
(3) derivative reaction：100 μ l of standard solution or sample are taken, 10 μ gmL are added-1100 μ l of inner mark solution respectively plus are used
Sodium hydroxide adjusts the 100 μ l of saturated sodium bicarbonate that pH value is 10 and the 2.0-5.0mgmL prepared with acetone-1Dansyl Cl
200 μ l, 10.0-20.0min is protected from light at 50-60 DEG C.After plus 100 μ l of ammonium hydroxide terminate reaction 20.0-30.0min.
Add acetonitrile constant volume to 1.0mL.Upper post detection after 0.22 μm of filtering of miillpore filter.
(4) it detects：Using I class Ultra Performance Liquid Chromatography instruments of Waters Acquity, C18,2.1 × 50mm, 1.7 μm
Chromatographic column, mobile phase are deionized water and acetonitrile, flow velocity 0.3mLmin-1, ultraviolet detection wavelength 254nm, 10 μ L of sample size, column
55 DEG C of temperature, mobile phase A is acetonitrile, and Mobile phase B is water, detector：PDA detectors.Use internal standard method with target analytes peak face
The ratio of product and internal standard peak area carries out the quantitative content for calculating tyrasamine in sample.
The detailed process that the step (1) prepares mixing gradient standard working solution is as follows:By a concentration of 1.0mgmL-1
Tyrasamine standard solution with 0.1M hydrochloric acid compound concentration gradients be 0.5,1.0,5.0,10.0,20.0,40.0,60.0,80.0 μ
g·mL-1Standard working solution, a concentration of 10 μ gmL of internal standard benzene methanamine in the hybrid standard working solution of each concentration-1。
The mass concentration of trichloroacetic acid is 5% in the step (2).
The elution program of UPLC is in the step (4)：Mobile phase A is acetonitrile, and Mobile phase B is deionized water, using ladder
Degree elution, in 0-20min, A 50-85%, B 50-15%, 20-21min, A85-50%, B 15-50%, 21-25min,
A50%, B 50%.
Compared with the literature, separation method processing procedure is simple by the present invention, establishes one kind and is suitable for measuring in fermentation sauce class
The method of the method for tyramine content, foundation is simple and reliable, can be applied to the detection of tyramine content in fermentation sauce class；This method pair
Sample analysis is simple and convenient, and detection limit is low, high sensitivity, and repeatability and the rate of recovery are good.
Description of the drawings
Fig. 1 is the UPLC chromatography peak figures added with interior target standard solution；
Fig. 2 is the UPLC chromatography peak figures added with interior target fermentation sauce class sample；
Fig. 3 is the UPLC chromatography peak figures of the fermentation sauce class sample added with internal standard and tyrasamine standard solution；
Fig. 4 is the standard curve of tyrasamine.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.
The present invention is described in further detail below by specific examples of the implementation.
Embodiment 1
(a) pretreatment of sample solution：Take oyster sauce 2.0g that 5% trichloroacetic acid 15.0mL is added to be homogenized 2.0min with refiner
Afterwards, 4000rpm centrifuges 10.0min on centrifuge, and precipitation is again plus 5% trichloroacetic acid 10.0mL is homogenized after centrifuging 2 times, in merging
Clear liquid 5% trichloroacetic acid constant volume to 50mL, extracting solution 0.22 μm of filtering of miillpore filter.
(b) derivative reaction of sample：100 μ l samples are taken from filtrate, and 10 μ gmL are added-1100 μ l of inner mark solution, then
The 100 μ l of saturated sodium bicarbonate for being 10 with sodium hydroxide adjustment pH value are sequentially added, are the 2.0mg that solvent is prepared with acetone
mL-1200 μ l of dansyl Cl are carried out in the dark derivative reaction at 55 DEG C, react 15.0min.After plus 100 μ l of ammonium hydroxide terminate
React 25.0min.Add acetonitrile constant volume to 1.0mL.Upper post detection after 0.22 μm of filtering of miillpore filter.
(c) testing conditions of UPLC：Using I class Ultra Performance Liquid Chromatography instruments of Waters Acquity, C18,2.1 ×
50mm, 1.7 μm of chromatographic columns, mobile phase are deionized water and acetonitrile, flow velocity 0.3mLmin-1, ultraviolet detection wavelength 254nm, into
10 μ L of sample amount, 55 DEG C of column temperature, mobile phase A are acetonitrile, and Mobile phase B is deionized water, detector：PDA detectors.The elution of UPLC
Program is：Mobile phase A is acetonitrile, and Mobile phase B is deionized water, using gradient elution, in 0-20min, A50-85%, B 50-
15%, 20-21min, A85-50%, B15-50%, 21-25min, A50%, B 50%.
(d) step (c) is measured numerical value to compare with tyrasamine standard items equation of linear regression, obtains junket in fermentation sauce class sample
The content of amine.
Tyrasamine standard items equation of linear regression:Precision weighs tyrasamine 100.0mg and is positioned in 100mL brown volumetric flasks, uses
0.1M hydrochloric acid is settled to scale to get a concentration of 1.0mgmL-1Tyrasamine standard solution, the filtering of 0.22 μm of miillpore filter, 4 DEG C
It saves backup；The quality 100.0mg that precision weighs internal standard benzene methanamine is positioned in 100mL volumetric flasks, is configured to deionized water
A concentration of 1.0mgmL-1Solution, be further continued for being diluted to a concentration of 10 μ gmL with deionized water-1Solution, miillpore filter
0.22 μm of 4 DEG C of filtering saves backup.
By a concentration of 1.0mgmL-1Tyrasamine standard solution with 0.1M hydrochloric acid compound concentration gradients be 0.5,1.0,5.0,
10.0、20.0、40.0、60.0、80.0μg·mL-1Standard working solution, the internal standard benzene of the standard working solution of each concentration
A concentration of 10 μ gmL of methylamine-1.Reaction is performed the derivatization by step (b) respectively, after 0.22 μm of membrane filtration, takes and adopts in right amount
It is detected with UPLC, UPLC methods conditional synchronization is rapid (c)；Using one concentration of ratio of peak area as linear regression, tyrasamine is obtained
The equation of linear regression of standard items.
Embodiment 2
(a) pretreatment of sample solution：Take barbeque sauce 5.0g that 5% trichloroacetic acid 25.0mL is added to be homogenized 2.0min with refiner
Afterwards, 4000rpm centrifuges 10.0min on centrifuge, and precipitation is again plus 5% trichloroacetic acid 15.0mL is homogenized after centrifuging 2 times, in merging
Clear liquid 5% trichloroacetic acid constant volume to 50mL, extracting solution 0.22 μm of filtering of miillpore filter.
(b) derivative reaction of sample：100 μ l samples are taken from filtrate, and 10 μ gmL are added-1100 μ l of inner mark solution, then
Sequentially add the 100 μ l of saturated sodium bicarbonate, the 3.0mgmL prepared with acetone that are 10 with sodium hydroxide adjustment pH value-1Red sulphur
200 μ l of acyl chlorides are carried out in the dark derivative reaction at 50 DEG C, react 20.0min.After plus 100 μ l of ammonium hydroxide terminate reaction
30.0min.Add acetonitrile constant volume to 1.0mL.Upper post detection after 0.22 μm of filtering of miillpore filter.
(c) testing conditions of UPLC：Using I class Ultra Performance Liquid Chromatography instruments of Waters Acquity, C18,2.1 ×
50mm, 1.7 μm of chromatographic columns, mobile phase are deionized water and acetonitrile, flow velocity 0.3mLmin-1, ultraviolet detection wavelength 254nm, into
10 μ L of sample amount, 55 DEG C of column temperature, mobile phase A are acetonitrile, and Mobile phase B is deionized water, detector：PDA detectors.The elution of UPLC
Program is：Mobile phase A is acetonitrile, and Mobile phase B is deionized water, using gradient elution, in 0-20min, A50-85%, B 50-
15%, 20-21min, A85-50%, B15-50%, 21-25min, A50%, B 50%.
(d) step (c) is measured numerical value to compare with tyrasamine standard items equation of linear regression, obtains junket in fermentation sauce class sample
The content of amine.
Tyrasamine standard items equation of linear regression:Precision weighs tyrasamine 100.0mg and is positioned in 100mL brown volumetric flasks, uses
0.1M hydrochloric acid is settled to scale to get a concentration of 1.0mgmL-1Tyrasamine standard solution, the filtering of 0.22 μm of miillpore filter, 4 DEG C
It saves backup；The quality 100mg that precision weighs internal standard benzene methanamine is positioned in 100mL volumetric flasks, is configured to deionized water dense
Degree is 1.0mgmL-1Solution, be further continued for being diluted to a concentration of 10 μ gmL with deionized water-1Solution, miillpore filter
0.22 μm of 4 DEG C of filtering saves backup.
By a concentration of 1.0mgmL-1Tyrasamine standard solution with 0.1M hydrochloric acid compound concentration gradients be 0.5,1.0,5.0,
10.0、20.0、40.0、60.0、80.0μg·mL-1Standard working solution, the internal standard benzene of the standard working solution of each concentration
A concentration of 10 μ gmL of methylamine-1.Reaction is performed the derivatization by step (b) respectively, after 0.22 μm of membrane filtration, takes and adopts in right amount
It is detected with UPLC, UPLC methods conditional synchronization is rapid (c)；Using one concentration of ratio of peak area as linear regression, tyrasamine is obtained
The equation of linear regression of standard items.
Embodiment 3
(a) pretreatment of sample solution：Take fermented bean curd 3.0g that 5% trichloroacetic acid 20.0mL is added to be homogenized 2.0min with refiner
Afterwards, 4000rpm centrifuges 10.0min on centrifuge, and precipitation is again plus 5% trichloroacetic acid 10.0mL is homogenized after centrifuging 2 times, in merging
Clear liquid 5% trichloroacetic acid constant volume to 50mL, extracting solution 0.22 μm of filtering of miillpore filter.
(b) derivative reaction of sample：100 μ l samples are taken from filtrate, and 10 μ gmL are added-1100 μ l of inner mark solution, then
Sequentially add the 100 μ l of saturated sodium bicarbonate, the 5.0mgmL prepared with acetone that are 10 with sodium hydroxide adjustment pH value-1Red sulphur
200 μ l of acyl chlorides are carried out in the dark derivative reaction at 60 DEG C, react 10.0min.After plus 100 μ l of ammonium hydroxide terminate reaction
20.0min.Add acetonitrile constant volume to 1.0mL.Upper post detection after 0.22 μm of filtering of miillpore filter.
(c) testing conditions of UPLC：Using I class Ultra Performance Liquid Chromatography instruments of Waters Acquity, C18,2.1 ×
50mm, 1.7 μm of chromatographic columns, mobile phase are deionized water and acetonitrile, flow velocity 0.3mLmin-1, ultraviolet detection wavelength 254nm, into
10 μ L of sample amount, 55 DEG C of column temperature, mobile phase A are acetonitrile, and Mobile phase B is deionized water, detector：PDA detectors.The elution of UPLC
Program is：Mobile phase A is acetonitrile, and Mobile phase B is deionized water, using gradient elution, in 0-20min, A50-85%, B 50-
15%, 20-21min, A85-50%, B15-50%, 21-25min, A 50%, B 50%.
(d) step (c) is measured numerical value to compare with tyrasamine standard items equation of linear regression, obtains junket in fermentation sauce class sample
The content of amine.
Tyrasamine standard items equation of linear regression:Precision weighs tyrasamine 100.0mg and is positioned in 100mL brown volumetric flasks, uses
0.1M hydrochloric acid is settled to scale to get a concentration of 1.0mgmL-1Tyrasamine standard solution, the filtering of 0.22 μm of miillpore filter, 4 DEG C
It saves backup；The quality 100.0mg that precision weighs internal standard benzene methanamine is positioned in 100mL volumetric flasks, is configured to deionized water
A concentration of 1.0mgmL-1Solution, be further continued for being diluted to a concentration of 10 μ gmL with deionized water-1Solution, miillpore filter
0.22 μm of 4 DEG C of filtering saves backup.
By a concentration of 1.0mgmL-1Tyrasamine standard solution with 0.1M hydrochloric acid compound concentration gradients be 0.5,1.0,5.0,
10.0、20.0、40.0、60.0、80.0μg·mL-1Standard working solution, the internal standard benzene of the standard working solution of each concentration
A concentration of 10 μ gmL of methylamine-1.Reaction is performed the derivatization by step (b) respectively, after 0.22 μm of membrane filtration, takes and adopts in right amount
It is detected with UPLC, UPLC methods conditional synchronization is rapid (c)；Each concentration does 3 parallel, difference sample detections.With wherein once into
For sample, obtained chromatography peak figure is as shown in Figure 3.Using the average value of the ratio of peak area as abscissa, with corresponding a concentration of
Ordinate carries out linear regression, obtains regression curve and see Fig. 4.
The analysis parameter of detection method is shown in Table 1-3.
The equation of linear regression and relevant parameter of 1 tyrasamine standard items of table
Note:x:Tyrasamine concentration (μ gmL-1)；y:Peak area ratio；* detection limit:Signal-to-noise ratio (S/N) is 3；* quantitative limits:
Signal-to-noise ratio (S/N) is 10.
The R for the equation of linear regression that table 1 and Fig. 4 can be seen that2It is 0.9996, linear stable, error is small.From table 1
Understand that concentration limit is 250ngmL-1, detect and be limited to 50ngmL-1, illustrate that the detection limit of this method is low, meet trace
The requirement of measurement.It is 0.06% to 8 relative standard deviations measured of same sample continuous sample introduction, illustrates that the precision of instrument is good
It is good.Same sample is measured respectively in 3 days and finds that relative standard deviation is 0.20%, the stability of illustration method is good.
2 repeatability of table and reproducibility experiment
Standard solution and fermentation sauce class sample are continuously measured 6 times interior on the same day, relative standard deviation is respectively 2.12
With 1.09%；Standard solution and fermentation sauce class sample are measured 1 time daily in 3 days, relative standard deviation is 3.13 Hes
4.84%.As a result illustrate that this method has good repeatability and reproducibility.
3 recovery of standard addition of table is tested
It can be seen that from table 3, the average recovery rate of the detection method is 89.9%, relative standard deviation 4.84%.
The equation of linear regression of tyrasamine obtains tyramine content in fermentation sauce class sample according to standard sample, as shown in table 4.
The content (Mean ± SD) (n=3) of tyrasamine in the fermentation sauce class sample of table 4
As can be seen from Table 4, in three kinds of measuring fermentation sauce classes the content of tyrasamine in 7.54-131.63mg/kg models
In enclosing, required without departing from standard as defined in European Union.
The method that UPLC provided by the invention measures tyramine content in fermentation sauce class, amount of samples is few, and measurement result is quick
Accurately, analysis time is fast, and solvent carrying capacity is few, the experimental results showed that, measurement result is stablized, and has good specificity, precision
And the rate of recovery.Have the characteristics that micro, easy, quick, sensitive, the requirement of determination of trace can be met.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc. should all be included in the protection scope of the present invention.
Claims (4)
1. the detection method of tyramine content in a kind of fermentation sauce class, it is characterised in that this method includes the following steps：
(1) preparation of standard solution：Precision weighs tyrasamine and is made into a concentration of 1.0mgmL with 0.1M hydrochloric acid-1Solution, micropore filter
0.22 μm of 4 DEG C of filtering of film saves backup.The gradient standard working solution 0.1M hydrochloric acids used are to required concentration.Precision claims
Internal standard is taken to be configured to a concentration of 10 μ gmL with deionized water-1Solution, saved backup for 4 DEG C after the filtering of 0.22 μm of miillpore filter.
(2) preparation of sample solution：After fermentation sauce class adds trichloroacetic acid refiner to be homogenized 2.0min, 4000rpm on centrifuge
10.0min is centrifuged, precipitates 2 times plus trichloroacetic acid is homogenized after centrifuging, merge supernatant trichloroacetic acid constant volume, extracting solution micropore
It is saved backup for 4 DEG C after 0.22 μm of filtering of filter membrane.
(3) derivative reaction：100 μ l of standard solution or sample are taken, 10 μ gmL are added-1100 μ l of inner mark solution respectively plus use hydrogen-oxygen
Change sodium adjustment the pH value 100 μ l of saturated sodium bicarbonate for being 10 and the 2.0-5.0mgmL prepared with acetone-1200 μ l of dansyl Cl,
It is protected from light 10.0-20.0min at 50-60 DEG C.After plus 100 μ l of ammonium hydroxide terminate reaction 20.0-30.0min.Add acetonitrile
Constant volume is to 1.0mL.Upper post detection after 0.22 μm of filtering of miillpore filter.
(4) it detects：Using I class Ultra Performance Liquid Chromatography instruments of Waters Acquity, C18,2.1 × 50mm, 1.7 μm of chromatographies
Column, mobile phase are deionized water and acetonitrile, flow velocity 0.3mLmin-1, ultraviolet detection wavelength 254nm, 10 μ L of sample size, column temperature 55
DEG C, mobile phase A is acetonitrile, and Mobile phase B is water, detector：PDA detectors.Use internal standard method with target analytes peak area and
The ratio of internal standard peak area carries out the quantitative content for calculating tyrasamine in sample.
2. the detection method of tyramine content in sauce class of fermenting as described in claim 1, which is characterized in that prepared by the step (1)
The detailed process for mixing gradient standard working solution is as follows:By a concentration of 1.0mgmL-1Tyrasamine standard solution 0.1M hydrochloric acid
Compound concentration gradient is 0.5,1.0,5.0,10.0,20.0,40.0,60.0,80.0 μ gmL-1Standard working solution, each
A concentration of 10 μ gmL of the internal standard benzene methanamine of the hybrid standard working solution of concentration-1。
3. the detection method of tyramine content in sauce class of fermenting as described in claim 1, which is characterized in that three in the step (2)
Chloroacetic mass concentration is 5%.
4. the detection method of tyramine content in sauce class of fermenting as described in claim 1, which is characterized in that in the step (4)
The elution program of UPLC is：Mobile phase A is acetonitrile, and Mobile phase B is deionized water, using gradient elution, in 0-20min, A 50-
85%, B 50-15%, 20-21min, A 85-50%, B 15-50%, 21-25min, A 50%, B 50%.
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| CN109298092A (en) * | 2018-11-01 | 2019-02-01 | 常州合全药业有限公司 | Detect the HPLC method of sulfonyloxy methyl chlorinity in industrial wastes |
| CN111879859A (en) * | 2019-11-27 | 2020-11-03 | 江南大学 | Method for accurately detecting content of butanediamine in fermentation liquor |
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| CN111879859B (en) * | 2019-11-27 | 2021-10-08 | 江南大学 | Method for accurately detecting content of butanediamine in fermentation liquor |
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