CN108645947B - Method for detecting tyramine content in soy sauce - Google Patents
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Abstract
The invention provides a method for detecting the tyramine content in soy sauce, and belongs to the technical field of food analysis. The method is pre-column derivatization-ultra high performance liquid chromatography, and a Waters Acquity I class ultra high performance liquid chromatograph and a C18 column are used. The method has the advantages of less sample consumption, short time, good method linearity, simple operation, good reproducibility and high accuracy.
Description
The technical field is as follows:
the invention relates to a food detection method, in particular to an ultra-high performance liquid chromatography detection method for tyramine content in soy sauce.
Background art:
tyramine (Tyramine), also known as p-hydroxyphenylethylamine, is a class of nitrogen-containing low-molecular biogenic amines. Biogenic amines, as a class of physiologically active substances, participate in metabolic activities in the body. Biogenic amines are widely found in a wide variety of food products, relatively more in food products rich in proteins and amino acids, especially fish and products thereof, cheese, meat products and fermented food products. Tyramine in food is mainly produced by removing tyrosine carboxyl under catalysis of decarboxylase produced by related microorganisms, or aldehyde and ketone are produced by amination and transamination. Thus, biogenic amines in food products are derived from two sources, namely, raw material carry-over and decarboxylation by microorganisms. The problem of biogenic amines in naturally fermented foods is receiving increasing attention because the traditional fermentation process is difficult to control and mechanism is not clear. Excessive intake of biogenic amine may cause various toxic symptoms such as headache, dizziness, nausea, respiratory distress, palpitation, etc. Of all biogenic amines, histamine and tyramine are the most significant for human health. Tyramine has an effect of increasing blood pressure, and excessive ingestion of tyramine causes a serious side effect by consuming monoamine oxidase inhibitors in the body, which is why tyramine is also called casetoxin. Tyramine also has effects in promoting peripheral vasoconstriction, stimulating cardiac rhythm acceleration, increasing blood glucose concentration, and eliminating norepinephrine in nervous system, thereby causing migraine. More than 100mg of tyramine orally taken by human body can cause migraine, more than 1080mg can cause toxic swelling, and the content of tyramine in the food regulated by European Union must not exceed 100-800 mg/kg.
Soy sauce is a food with a long history, is used for table and seasoning, and is widely manufactured and eaten due to unique flavor, delicious taste and rich nutrition. However, the soy sauce is generally prepared by a natural fermentation method, and fermentation strains are complex, so that the potential safety hazard of microbial biogenic amine is high. In consideration of food safety, people should reduce the intake of biogenic amine as much as possible, and it is urgent to detect and monitor the content of biogenic amine in food. Since tyrosine produces tyramine during fermentation, the analysis of tyramine in soy sauce can not only ensure food safety, but also obtain useful information related to food production and fermentation processes.
The detection methods of the biogenic amine comprise a gas chromatography-tandem mass spectrometry method, an ion chromatography method, a high performance liquid chromatography, a thin layer chromatography, a high performance liquid chromatography-tandem mass spectrometry method and the like, and the methods have the defects of more complicated processing steps, long analysis time, difficult operation and the like. The detection method for detecting tyramine by Ultra Performance Liquid Chromatography (UPLC) can obtain better separation effect and shorter analysis time by using the chromatographic column with small-particle-size filler, and simultaneously simplifies the processing steps. Therefore, the method has the advantages of less sample consumption, short time, good method linearity, simple operation, good reproducibility, high accuracy and the like.
The invention content is as follows:
the invention aims to simplify the sample pretreatment step, shorten the sample detection time, and rapidly and accurately determine the tyramine content in the soy sauce by using a UPLC detection method in research and design.
The technical problem to be solved by the invention is realized by the following technical scheme:
(1) preparation of standard solution: accurately weighing tyramine, and preparing into 1 mg/mL solution with 0.1M hydrochloric acid-1Filtering the solution with a microporous filter membrane of 0.22 mu m, and storing the solution at 4 ℃ for later use. The gradient standard working solution used was diluted to the desired concentration with 0.1M hydrochloric acid. Accurately weighing internal standard, and preparing with deionized water to obtain the product with concentration of 50 μ g/mL-1Filtering the solution with a microporous filter membrane of 0.22 mu m, and storing the solution at 4 ℃ for later use.
(2) Preparation of sample solution: diluting the soy sauce sample by 5-20 times with deionized water, and filtering with microporous membrane of 0.22 μm; adding 50 mu g/mL-1And performing derivatization reaction by using 100 mu L of internal standard solution.
(3) And (3) derivatization reaction: taking 100 μ L of standard solution or sample, adding 100 μ L of saturated sodium bicarbonate with pH of 10 and 5-10 mg/mL-1Dansyl chloride (200 μ L) in acetone is reacted at 50-60 deg.C in the dark for 10-20 min. After finishing addingThe reaction was stopped with 100. mu.L of ammonia for 20-30 min. Acetonitrile was added to make a volume of 1 mL. Filtering with a microporous membrane of 0.22 μm. And (5) detecting the filtrate on a column.
(4) And (3) detection: adopting a Waters Acquity I-Class ultra performance liquid chromatograph, a C18 chromatographic column with the flow rate of 0.3 mL/min and the flow rate of 2.1 multiplied by 50mm and 1.7 mu m, wherein the mobile phase is deionized water and acetonitrile-1Ultraviolet detection wavelength 254nm, sample amount 10 μ L, column temperature 55 deg.C, mobile phase A is acetonitrile, mobile phase B is deionized water, detector: a PDA detector. And (3) quantitatively calculating the content of tyramine in the sample by adopting an internal standard method according to the ratio of the peak area of the target analyte to the peak area of the internal standard.
The specific process for preparing the mixed gradient standard working solution in the step (1) is that the concentration is 1 mg.mL-1The tyramine standard solution is prepared by 0.1M hydrochloric acid with concentration gradient of 50, 100, 200, 300, 400 and 500 mu g/mL-1The concentration of the internal standard benzylamine of each concentration of the mixed standard working solution is 50. mu.g.mL-1。
The elution procedure for UPLC was: the mobile phase A is acetonitrile, the mobile phase B is deionized water, and gradient elution is adopted for 0-20min, wherein the content of A is 50-85%, the content of B is 50-15%, the content of A is 20-21min, the content of A is 85-50%, the content of B is 15-50%, the content of A is 21-25min, the content of A is 50% and the content of B is 50%.
Compared with the literature, the separation method has the advantages of simple treatment process, short analysis time and simple and reliable establishment method, and can be applied to detection of the tyramine content in the soy sauce; the method has the advantages of simple and convenient sample analysis, low detection limit, high sensitivity, good repeatability and good recovery rate.
Drawings
FIG. 1 is a UPLC chromatogram peak of a standard solution with an internal standard;
FIG. 2 is a UPLC chromatogram peak of a soy sauce sample with an internal standard;
FIG. 3 is a UPLC chromatogram peak of a soy sauce sample with an internal standard and a standard solution added;
FIG. 4 is a standard curve for tyramine.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer.
The present invention is described in further detail below with reference to specific examples.
Example 1
(a) Pretreatment of the sample solution: diluting 5mL of soy sauce sample to be detected by 10 times with deionized water, filtering with a microporous membrane of 0.22 μm, and storing the filtrate at 4 deg.C for use.
(b) Derivatization reaction of the sample: a100. mu.L sample was taken from the filtrate, and 50. mu.g/mL of the sample was added-1100 μ L of internal standard solution, 100 μ L of saturated sodium bicarbonate with pH adjusted to 10 with sodium hydroxide, and 8 mg/mL prepared with acetone-1The derivatization reaction is carried out on 200 mu L dansyl chloride at 55 ℃ in the dark for 15 min. After the reaction, 100. mu.L of ammonia water was added to terminate the reaction for 25 min. Acetonitrile was added to make a volume of 1 mL. Filtering with a microporous membrane of 0.22 μm, and detecting the filtrate on a column.
(c) Detection conditions of UPLC: adopting a Waters Acquity I-Class ultra performance liquid chromatograph, a C18 chromatographic column with the flow rate of 0.3 mL/min and the flow rate of 2.1 multiplied by 50mm and 1.7 mu m, wherein the mobile phase is deionized water and acetonitrile-1Ultraviolet detection wavelength 254nm, sample amount 10 μ L, column temperature 55 deg.C, mobile phase A is acetonitrile, mobile phase B is deionized water, detector: a PDA detector. The elution procedure for UPLC was: the mobile phase A is acetonitrile, the mobile phase B is deionized water, and gradient elution is adopted for 0-20min, wherein the content of A is 50-85%, the content of B is 50-15%, the content of A is 20-21min, the content of A is 85-50%, the content of B15-50%, the content of A is 21-25min, the content of A is 50% and the content of B is 50%.
(d) And (c) substituting the measured value in the step (c) into a linear regression equation of a tyramine standard substance to calculate to obtain the content of tyramine in the soy sauce sample.
The linear regression equation of tyramine standard comprises precisely weighing 100mg of tyramine, placing in a 100mL brown volumetric flask, and diluting to constant volume with 0.1M hydrochloric acid to obtain a solution with a concentration of 1 mg/mL-1Filtering the tyramine standard solution with a microporous filter membrane of 0.22 mu m, and storing at 4 ℃ for later use; precisely weighing 100mg of internal standard benzylamine, placing the weighed internal standard benzylamine into a 100mL volumetric flask, and preparing the weighed internal standard benzylamine into the volumetric flask with the deionized water to obtain the internal standard benzylamine with the concentration of 1 mg/mL-1The solution (a) of (b) is,then continuously diluting the mixture with deionized water to the concentration of 50 mu g/mL-1Filtering the solution with a microporous filter membrane of 0.22 mu m, and storing the solution at 4 ℃ for later use.
The concentration is 1 mg/mL-1The tyramine standard solution is prepared by 0.1M hydrochloric acid with concentration gradient of 50, 100, 200, 300, 400 and 500 mu g/mL-1The concentration of the internal standard benzylamine of each concentration of the standard working solution is 50. mu.g.mL-1. Performing derivatization reaction according to the step (b), filtering by a 0.22 mu m filter membrane, and detecting by using UPLC with the same conditions as the step (c); and taking the peak area ratio-concentration as linear regression to obtain a linear regression equation of the tyramine standard substance.
Example 2
(a) Pretreatment of the sample solution: diluting 2mL of soy sauce sample to be detected by 20 times with deionized water, filtering with a microporous membrane of 0.22 μm, and storing the filtrate at 4 ℃ for later use.
(b) Derivatization reaction of the sample: a100. mu.L sample was taken from the filtrate, and 50. mu.g/mL of the sample was added-1100 μ L of internal standard solution, 100 μ L of saturated sodium bicarbonate adjusted to pH10 with sodium hydroxide, and 5 mg/mL prepared with acetone-1The derivatization reaction is carried out on 200 mu L dansyl chloride at 50 ℃ in the dark for 20 min. After the reaction is finished, 100 mu L of ammonia water is added to terminate the reaction for 30 min. Acetonitrile was added to make a volume of 1 mL. Filtering with a microporous membrane of 0.22 μm, and detecting the filtrate on a column.
(c) Detection conditions of UPLC: adopting a Waters Acquity I-Class ultra performance liquid chromatograph, a C18 chromatographic column with the flow rate of 0.3 mL/min and the flow rate of 2.1 multiplied by 50mm and 1.7 mu m, wherein the mobile phase is deionized water and acetonitrile-1Ultraviolet detection wavelength 254nm, sample amount 10 μ L, column temperature 55 deg.C, mobile phase A is acetonitrile, mobile phase B is deionized water, detector: a PDA detector. The elution procedure for UPLC was: the mobile phase A is acetonitrile, the mobile phase B is deionized water, and gradient elution is adopted for 0-20min, wherein the content of A is 50-85%, the content of B is 50-15%, the content of A is 20-21min, the content of A is 85-50%, the content of B15-50%, the content of A is 21-25min, the content of A is 50% and the content of B is 50%.
(d) And (c) substituting the measured value in the step (c) into a linear regression equation of a tyramine standard substance to calculate to obtain the content of tyramine in the soy sauce sample.
Tyramine labelThe standard linear regression equation comprises precisely weighing tyramine 100mg, placing in a 100mL brown volumetric flask, and diluting to constant volume with 0.1M hydrochloric acid to obtain a solution with a concentration of 1 mg/mL-1Filtering the tyramine standard solution with a microporous filter membrane of 0.22 mu m, and storing at 4 ℃ for later use; precisely weighing 100mg of internal standard benzylamine, placing the weighed internal standard benzylamine into a 100mL volumetric flask, and preparing the weighed internal standard benzylamine into the volumetric flask with the deionized water to obtain the internal standard benzylamine with the concentration of 1 mg/mL-1The solution of (1) was further diluted with deionized water to a concentration of 50. mu.g.mL-1Filtering the solution with a microporous filter membrane of 0.22 mu m, and storing the solution at 4 ℃ for later use.
The concentration is 1 mg/mL-1The tyramine standard solution is prepared by 0.1M hydrochloric acid with concentration gradient of 50, 100, 200, 300, 400 and 500 mu g/mL-1The concentration of the internal standard benzylamine of each concentration of the standard working solution is 50. mu.g.mL-1. Performing derivatization reaction according to the step (b), filtering by a 0.45 mu m filter membrane, and detecting by using UPLC (ultra performance liquid chromatography) with the same conditions as the step (c); and taking the peak area ratio-concentration as linear regression to obtain a linear regression equation of the tyramine standard substance.
Example 3
(a) Pretreatment of the sample solution: diluting 10mL of soy sauce sample to be detected by 5 times with deionized water, filtering with a microporous membrane of 0.22 μm, and storing the filtrate at 4 ℃ for later use.
(b) Derivatization reaction of the sample: a100. mu.L sample was taken from the filtrate, and 50. mu.g/mL of the sample was added-1100 μ L of internal standard solution, 100 μ L of saturated sodium bicarbonate adjusted to pH10 with sodium hydroxide, and 10 mg/mL prepared with acetone-1The derivatization reaction is carried out on 200 mu L dansyl chloride at 60 ℃ in the dark for 10 min. After the reaction, 100. mu.L of ammonia water was added to terminate the reaction for 20 min. Acetonitrile was added to make a volume of 1 mL. Filtering with a microporous membrane of 0.22 μm, and detecting the filtrate on a column.
(c) UPLC detection conditions: adopting a Waters Acquity I-Class ultra performance liquid chromatograph, a C18 chromatographic column with the flow rate of 0.3 mL/min and the flow rate of 2.1 multiplied by 50mm and 1.7 mu m, wherein the mobile phase is deionized water and acetonitrile-1Ultraviolet detection wavelength 254nm, sample amount 10 μ L, column temperature 55 deg.C, mobile phase A is acetonitrile, mobile phase B is deionized water, detector: a PDA detector. The elution procedure for UPLC was: mobile phase AAcetonitrile, deionized water as mobile phase B, and gradient elution for 0-20min, A50-85%, B50-15%, 20-21min, A85-50%, B15-50%, 21-25min, A50%, and B50%.
(d) And (c) substituting the measured value in the step (c) into a linear regression equation of a tyramine standard substance to calculate to obtain the content of tyramine in the soy sauce sample.
The linear regression equation of tyramine standard comprises precisely weighing 100mg of tyramine, placing in a 100mL brown volumetric flask, and diluting to constant volume with 0.1M hydrochloric acid to obtain a solution with a concentration of 1 mg/mL-1Filtering the tyramine standard solution with a microporous filter membrane of 0.22 mu m, and storing at 4 ℃ for later use; precisely weighing 100mg of internal standard benzylamine, placing the weighed internal standard benzylamine into a 100mL volumetric flask, and preparing the weighed internal standard benzylamine into the volumetric flask with the deionized water to obtain the internal standard benzylamine with the concentration of 1 mg/mL-1The solution of (1) was further diluted with deionized water to a concentration of 50. mu.g.mL-1Filtering the solution with a microporous filter membrane of 0.22 mu m, and storing the solution at 4 ℃ for later use.
The concentration is 1 mg/mL-1The tyramine standard solution is prepared by 0.1M hydrochloric acid with concentration gradient of 50, 100, 200, 300, 400 and 500 mu g/mL-1The concentration of the internal standard benzylamine of each concentration of the standard working solution is 50. mu.g.mL-1. Performing derivatization reaction according to the step (b), filtering by a 0.22 mu m filter membrane, and detecting by using UPLC with the same conditions as the step (c); each concentration was done in 3 replicates and detected by separate injection. Taking one of the samples as an example, the obtained chromatogram peak image is shown in FIG. 3. Taking the average value of the peak area ratios as the abscissa and the corresponding concentration as the ordinate, linear regression was performed to obtain a regression curve as shown in FIG. 4.
Analytical parameters of the UPLC detection method are shown in tables 1-3.
TABLE 1 Linear regression equation and related parameters for tyramine standards
Note that x: tyramine concentration (. mu.g.mL)-1) (ii) a y: peak area ratio; detection limit: the signal-to-noise ratio (S/N) is 3; limit of quantitation: the signal to noise ratio (S/N) was 10.
As can be seen from Table 1 and FIG. 4, R of the resulting linear regression equation2Is 0.9997, has stable linearity and small error. As is clear from Table 1, the lowest detection concentration was 250 ng/mL-1The detection limit is 50 ng/mL-1The method is low in detection limit and meets the requirement of trace measurement. The relative standard deviation of the measurement results of the same sample after being continuously injected for 8 times is calculated to be 0.06 percent, which indicates that the precision of the instrument is good. The relative standard deviation of the same sample was measured to be 0.20% in 3 consecutive days, indicating that the stability of the method was good.
TABLE 2 repeatability and reproducibility experiments
The standard solution and the soy sauce sample are continuously measured for 6 times in the same day, and the relative standard deviation is 2.12 percent and 3.62 percent respectively; the standard solution and soy sauce samples were measured 1 time per day for 3 consecutive days with relative standard deviations of 3.13 and 3.09%. The results show that the method has good repeatability and reproducibility.
TABLE 3 spiking recovery test
As can be seen from table 3, the average recovery of this test method was 87.3% with a relative standard deviation of 6.63%.
The tyramine content was calculated by a linear regression equation for 5 commercially available soy sauce samples tested according to the method of the present invention, and the results are shown in Table 4.
TABLE 45 tyramine content (Mean + -SD) in soy sauce samples (n ═ 3)
As can be seen from Table 4, the tyramine content of the five purchased soy sauces was in the range of 166-792 mg/L, and did not exceed the standards set by the European Union.
The UPLC method for determining the tyramine content in the soy sauce provided by the invention has the advantages of small sample consumption, quick and accurate determination result, quick analysis time, small solvent loading capacity, and stable determination result, and has good specificity, precision and recovery rate. Has the characteristics of trace, simplicity, convenience, quickness, sensitivity and the like, and can meet the requirement of trace measurement.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.
Claims (1)
1. A method for detecting the content of tyramine in soy sauce is characterized by comprising the following steps:
(a) pretreatment of the sample solution: diluting 5mL of a soy sauce sample to be detected by 10 times with deionized water, filtering with a microporous filter membrane of 0.22 mu m, and storing the filtrate at 4 ℃ for later use;
(b) derivatization reaction of the sample: a100. mu.L sample was taken from the filtrate, and 50. mu.g/mL of the sample was added-1100 μ L of internal standard solution, 100 μ L of saturated sodium bicarbonate with pH adjusted to 10 with sodium hydroxide, and 8 mg/mL prepared with acetone-1200 mu L of dansyl chloride, and carrying out derivatization reaction at 55 ℃ in a dark place for 15 min; after the reaction is finished, 100 mu L of ammonia water is added to terminate the reaction for 25min, acetonitrile is added to the reaction solution to reach the constant volume of 1mL, a millipore filter membrane is used for filtering the solution with the diameter of 0.22 mu m, and the filtrate is put on a column for detection;
(c) detection conditions of UPLC: adopting a Waters Acquity I-Class ultra performance liquid chromatograph, a C18 chromatographic column with the flow rate of 0.3 mL/min and the flow rate of 2.1 multiplied by 50mm and 1.7 mu m, wherein the mobile phase is deionized water and acetonitrile-1Ultraviolet detection wavelength 254nm, sample amount 10 μ L, column temperature 55 deg.C, mobile phase A is acetonitrile, mobile phase B is deionized water, detector: a PDA detector;
the elution procedure for UPLC was: the mobile phase A is acetonitrile, the mobile phase B is deionized water, and gradient elution is adopted for 0-20min, wherein the elution is carried out for 0-20min, A50-85%, B50-15%, 20-21min, A85-50%, B15-50%, 21-25min, A50% and B50%;
(d) substituting the measured value in the step (c) into a linear regression equation of a tyramine standard substance to calculate to obtain the content of tyramine in the soy sauce sample;
the linear regression equation of tyramine standard comprises precisely weighing 100mg of tyramine, placing in a 100mL brown volumetric flask, and diluting to constant volume with 0.1M hydrochloric acid to obtain a solution with a concentration of 1 mg/mL-1Filtering the tyramine standard solution with a microporous filter membrane of 0.22 mu m, and storing at 4 ℃ for later use; precisely weighing 100mg of internal standard benzylamine, placing the weighed internal standard benzylamine into a 100mL volumetric flask, and preparing the weighed internal standard benzylamine into the volumetric flask with the deionized water to obtain the internal standard benzylamine with the concentration of 1 mg/mL-1The solution of (1) was further diluted with deionized water to a concentration of 50. mu.g.mL-1Filtering the solution with a microporous filter membrane of 0.22 mu m, and storing the solution at 4 ℃ for later use;
the concentration is 1 mg/mL-1The tyramine standard solution is prepared by 0.1M hydrochloric acid with concentration gradient of 50, 100, 200, 300, 400 and 500 mu g/mL-1The concentration of the internal standard benzylamine of each concentration of the standard working solution is 50. mu.g.mL-1(ii) a Performing derivatization reaction according to the step (b), filtering by a 0.22 mu m filter membrane, and detecting by using UPLC with the same conditions as the step (c); and taking the peak area ratio-concentration as linear regression to obtain a linear regression equation of the tyramine standard substance.
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| CN101793642A (en) * | 2009-12-17 | 2010-08-04 | 东北农业大学 | Separation and liquid chromatography column pre-column derivatization method of biogenic amine in soybean paste |
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| JPH0452554A (en) * | 1990-06-20 | 1992-02-20 | Ichiro Yoshihara | Easy and quick gas chromatographic analyzing method of cyclic amino acid amine, serotonin and cholesterol in serum |
| CN101793642A (en) * | 2009-12-17 | 2010-08-04 | 东北农业大学 | Separation and liquid chromatography column pre-column derivatization method of biogenic amine in soybean paste |
| CN101793881A (en) * | 2009-12-17 | 2010-08-04 | 东北农业大学 | Method for detecting biogenic amine in food |
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