CN114280204A - Liquid chromatography tandem mass spectrometry screening method for identifying animal-derived articles - Google Patents
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Abstract
The application provides a liquid chromatography tandem mass spectrometry screening method for identifying animal-derived goods, which is used for detecting the content of hydroxyproline in a consumer product by sampling; pretreating and detecting the content of hydroxyproline in the pretreated sample solution; wherein the pretreatment step comprises: mixing a sample with a digesting agent with specified mass, and carrying out reflux digestion treatment for a specified time at a first specified temperature; and adding a diluent with a specified volume ratio for dilution treatment to obtain a pretreated sample solution. The method has the advantages of high analysis speed and strong map characteristic, can clearly identify the interference of other amino acids (such as leucine and isoleucine), has high reproducibility, and can achieve 80-120% of hydroxyproline recovery rate.
Description
Technical Field
The application relates to the field of detection, in particular to a liquid chromatography tandem mass spectrometry screening method for identifying animal-derived goods.
Background
trans-4-hydroxy-L-proline (chemical accession No. 51-35-4) is one of imino acids, a non-essential amino acid, one of the main components of collagen tissue, and is a specific amino acid in collagen, accounting for about 13% of the total amount of collagen amino acids. Collagen is the most abundant protein in the living body, and accounts for about 1/3 total body protein.
Due to the improvement of environmental awareness at home and abroad and the prevalence of simple vegetarian meanings, more and more strict vegetarians have stricter requirements on daily consumer goods used or required by the vegetarians, and whether the daily consumer goods contain animal-derived material components becomes the focus of attention of the group.
The foreign detection standard for the measurement of the hydroxyproline, ISO 3496:1994, uses a colorimetric method to measure the content of the hydroxyproline in meat or meat products, the detection range is only meat or meat products, the analysis method is the colorimetric method, but due to the defects of complex sample matrix, interference of the background color of the sample and the like, the quantitative result is easily influenced, and the reproducibility of the result is greatly reduced.
Disclosure of Invention
In view of the problems, the present application is directed to providing a liquid chromatography tandem mass spectrometry screening method of identifying an item of animal origin that overcomes or at least partially solves the problems, comprising:
a liquid chromatography tandem mass spectrometry screening method for identifying animal-derived goods is used for detecting the content of hydroxyproline in a consumable product and comprises the following steps: sampling; pretreating and detecting the content of hydroxyproline in the pretreated sample solution;
wherein the pretreatment step comprises:
mixing a sample with a digesting agent with specified mass, and carrying out reflux digestion treatment for a specified time at a first specified temperature;
and adding a diluent with a specified volume ratio for dilution treatment to obtain a pretreated sample solution.
Further, the step of mixing the sample with a digesting agent of a specified mass and performing a reflux digestion process at a first specified temperature for a specified time comprises:
mixing the sample with a digesting agent of a specified mass in a closed container;
the closed vessel was subjected to reflux digestion at a first specified temperature for a specified time.
Further, the step of adding a diluent in a specified volume ratio for dilution treatment to obtain a pretreated sample solution includes:
cooling the sample liquid to a second specified temperature;
and adding a diluent with a specified volume ratio to dilute the sample solution to a specified multiple, and filtering to obtain a pretreated sample solution.
Further, the step of detecting the content of hydroxyproline in the pretreated sample solution comprises:
and detecting the content of hydroxyproline in the pretreated sample solution by using a liquid chromatography tandem mass spectrometer.
Further, the step of detecting the content of hydroxyproline in the pretreated sample solution by using a liquid chromatography tandem mass spectrometer comprises the following steps:
the first mobile phase is an aqueous solution containing 0.1% formic acid;
the second mobile phase was methanol containing 0.1% formic acid;
the flow rate is: 0.3 mL/min;
gradient: at the beginning, the current mobile phase consists of 90% of the first mobile phase and 10% of the second mobile phase;
when the time reaches 4.5min, the current mobile phase is adjusted to be composed of 90% of the first mobile phase and 10% of the second mobile phase;
when 5min is reached, the current mobile phase is adjusted to be composed of 50% of first mobile phase and 50% of second mobile phase;
when 5.5min is reached, the current mobile phase remains composed of 100% of the second mobile phase;
when 7.5min is reached, the current mobile phase remains composed of 100% of the second mobile phase;
when 8min is reached, the current mobile phase is adjusted to be composed of 90% of the first mobile phase and 10% of the second mobile phase;
at 10min, the current mobile phase was adjusted to consist of 90% of the first mobile phase and 10% of the second mobile phase.
Further, the step of sampling comprises:
shearing the object to be detected into fragments with the area less than 5mm multiplied by 5 mm;
0.5g of sample was weighed.
Further, the volume ratio of the sample to the digesting agent is 0.5 g: 10-15 mL.
Further, the specified volume ratio of the diluent is 1:1 in aqueous methanol.
Further, the first specified temperature is 105 ℃.
Further, the specified time is 16 h.
The application has the following advantages:
in the embodiments of the present application, the sampling is performed; pretreating and detecting the content of hydroxyproline in the pretreated sample solution; wherein the pretreatment step comprises: mixing a sample with a digesting agent with specified mass, and carrying out reflux digestion treatment for a specified time at a first specified temperature; and adding a diluent with a specified volume ratio for dilution treatment to obtain a pretreated sample solution. The method has the advantages of high analysis speed and strong map characteristic, can clearly identify the interference of other amino acids (such as leucine and isoleucine), has high reproducibility, and can achieve 80-120% of hydroxyproline recovery rate.
Drawings
In order to more clearly illustrate the technical solutions of the present application, the drawings needed to be used in the description of the present application will be briefly introduced below, and it is apparent that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive labor.
FIG. 1 is a schematic flow chart diagram of a liquid chromatography tandem mass spectrometry screening method for identifying an animal-derived item according to an embodiment of the present disclosure;
FIG. 2 is a schematic flow chart diagram of a liquid chromatography tandem mass spectrometry screening method for identifying an animal-derived item according to an embodiment of the present disclosure;
FIG. 3 is a schematic flow chart diagram of a liquid chromatography tandem mass spectrometry screening method for identifying an animal-derived item according to an embodiment of the present application;
FIG. 4 is a schematic liquid chromatography-tandem mass spectrometry screening method for identifying an animal-derived item according to an embodiment of the present application;
fig. 5 is a schematic liquid chromatography diagram of a liquid chromatography tandem mass spectrometry screening method for identifying an animal-derived item according to an embodiment of the present application.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the descriptions related to "first", "second", etc. in the present invention are for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, the technical solutions of the respective embodiments may be combined with each other, but must be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
Referring to fig. 1, a liquid chromatography tandem mass spectrometry screening method for identifying an animal-derived product, provided by an embodiment of the present application, is shown for detecting the content of hydroxyproline in a consumable product;
the method comprises the following steps: s1 sampling; s2 pretreatment and S3 detection of the content of hydroxyproline in the pretreated sample solution;
wherein the pretreatment step comprises:
s21, mixing the sample with a digesting agent with a specified mass, and carrying out reflux digestion treatment for a specified time at a first specified temperature;
and S22, adding a diluent with a specified volume ratio for dilution treatment to obtain a pretreated sample solution.
In the embodiments of the present application, the sampling is performed; pretreating and detecting the content of hydroxyproline in the pretreated sample solution; wherein the pretreatment step comprises: mixing a sample with a digesting agent with specified mass, and carrying out reflux digestion treatment for a specified time at a first specified temperature; and adding a diluent with a specified volume ratio for dilution treatment to obtain a pretreated sample solution. The method has the advantages of high analysis speed and strong map characteristic, can clearly identify the interference of other amino acids (such as leucine and isoleucine), has high reproducibility, and can achieve 80-120% of hydroxyproline recovery rate.
Hereinafter, a liquid chromatography tandem mass spectrometry screening method for identifying an article of animal origin in the present exemplary embodiment will be further described.
In an embodiment of the present invention, the specific process of "sampling" in step S1 can be further described with reference to the following description.
As described in the above step S1, sampling is generally one of the important steps for extracting a small amount of target substance from a target substance for detection, and has one of the effective ways to obtain various data from the target substance for testing without affecting the main properties of the target substance, the extraction amount of the target substance is sufficient for 3-5 times of testing, the sampling process requires randomness for the selection process of the sampling area of the target substance, and subjective selection cannot be mixed in the selection process, in the embodiment of the present invention, the sampling weight is generally 0.1g-1g, preferably 0.50g, and the weighed sample is placed in a headspace bottle for standby.
As described in the above step S2, the pretreatment is generally a step for the purpose of impurity removal and purification before performing an effective process on the target object, and in some special experiments, the pretreatment step also includes the purpose of changing the material property, and in the embodiment of the present invention, the pretreatment step is preferably the above steps S21-S22.
As described in the step S3, the step of detecting the content of hydroxyproline in the pretreated sample solution is generally a step of performing a specified experiment or detection on the target substance after the steps S1-S2, and generally obtains direct data or indirect data, where the direct data is data of the target substance directly as a detection target value or result; the indirect data is data of a target value or result obtained only after corresponding calculation, replacement or comparison, the detection result generally has a deviation value according to the deviation of detection equipment, environment, preprocessing steps and auxiliary products, and after the difference between the preprocessing step and the auxiliary products is used for formulating a detection standard, the error amplitude caused by the preprocessing step and the auxiliary products can be correspondingly and effectively avoided.
Mixing a sample with a digesting agent of a predetermined mass at a first predetermined temperature for a predetermined time period as in the above step S21, and mixing the sample with the digesting agent of the predetermined mass in a headspace bottle in the course of carrying out the above step S22 to such an extent that the sample and the digesting agent are in the same reactor and in contact with each other; wherein the specified mass is generally 5-15mL, preferably 10 mL; wherein, the concentration of the digesting agent is generally 1-5mol/L, preferably 3 mol/L; and (3) after the sample is mixed with the digesting agent, performing reflux digestion on the mixed solution, wherein the reflux digestion process is generally performed by using an oven, wherein in the reflux digestion process, the temperature in the reaction device is required to be kept within the first specified temperature, the first specified temperature is generally 90-120 ℃, in the embodiment of the invention, 105 ℃ is preferred, the power of the oven is generally 500-3000W, the preferred ultrasonic power is 1000-2000W, and the duration of the ultrasonic extraction process is generally 10-25h, preferably 16 h.
Adding a diluent with a specified volume ratio to perform dilution treatment to obtain a pretreated sample solution as described in the step S22, wherein the temperature of the sample after the reflux digestion treatment is usually higher in the process of performing the step S22, and the temperature of the sample solution is reduced to a specified temperature to prevent the reaction from excessively proceeding to influence the test result; the sample and the diluent in a predetermined volume ratio may be mixed to such an extent that the sample and the diluent in a predetermined volume ratio are in contact with each other in the same reactor or more, wherein the second predetermined temperature is generally 10 to 35 ℃, preferably 20 to 30 ℃ in the methanol aqueous solution of 1:1 in the diluent in a predetermined volume ratio.
Referring to fig. 2, in the method for screening animal-derived goods by liquid chromatography-tandem mass spectrometry, the step of mixing the sample with a digestion agent with a specified mass and performing reflux digestion treatment at a first specified temperature for a specified time includes:
s211, mixing the sample with a digesting agent with a specified mass in a closed container;
and S212, carrying out reflux digestion treatment on the closed container for a specified time at a first specified temperature.
As described in step S211, since the sample and the digesting agent of a predetermined mass are mixed in the closed vessel, which is a headspace bottle, and the mixing degree of the sample and the digesting agent of a predetermined mass in the headspace bottle needs to be sufficiently mixed with each other, the sample and the digesting agent of a predetermined mass are mixed and then shaken up and shaken. Wherein the digesting agent is sulfuric acid with the concentration of 3 mol/L; wherein, the digestion agent with the specified mass is generally 5-15mL, and preferably 10 mL.
As described in step S212 above, the closed vessel is subjected to the reflux digestion process at the first prescribed temperature for a prescribed time, and in order to accelerate some chemical reactions, which are slow or difficult to perform, it is often necessary to keep the reactants boiling for a long time, and therefore, the closed vessel is subjected to the reflux digestion process at the first prescribed temperature for a prescribed time. Wherein, in the reflux digestion, the temperature in the reaction device is required to be kept within the first designated temperature, wherein the first designated temperature is generally 90 ℃ to 120 ℃, in the embodiment of the invention, 105 ℃ is preferred, wherein, in the reflux digestion process, the power of the oven is generally 500W to 3000W, the preferred ultrasonic power is 1000W to 2000W, and the duration of the ultrasonic extraction process is generally 10 h to 25h, preferably 16 h.
Referring to fig. 2, in this embodiment, the step of adding the diluent at the specified volume ratio to perform the dilution treatment to obtain the pre-treated sample solution includes:
s221, cooling the sample liquid to a second specified temperature;
and S222, adding a diluent with a specified volume ratio to dilute the sample solution to a specified multiple, and filtering to obtain a pretreated sample solution.
Cooling the sample liquid to a second designated temperature, wherein the second designated temperature is generally 10-35 ℃, preferably 20-30 ℃, and reducing the sample liquid in the headspace bottle to the designated temperature drop to prevent the excessive reaction from affecting the test result during the step S221; in the embodiment of the invention, the headspace bottle is taken out, and the quartz test tube is placed in a test tube rack and cooled to 20-30 ℃ at normal temperature.
Adding a diluent with a specified volume ratio to dilute the sample solution to a specified multiple, and filtering to obtain a pretreated sample solution, wherein the sample and the diluent with the specified volume ratio are mixed to a degree that the sample and the diluent with the specified volume ratio are in contact with each other in the same reactor, wherein the second specified temperature is generally 10-35 ℃, and preferably 20-30 ℃; wherein the specified multiple is 1000 times. In the process of implementing the steps, the diluted sample liquid is filtered by a filter membrane with the pore diameter of 0.45 micrometer, and the obtained filtrate is the standard liquid to be detected.
In this embodiment, in the method for screening animal-derived articles by liquid chromatography-tandem mass spectrometry, the step of detecting the content of hydroxyproline in the pretreated sample solution includes;
and S31, detecting the content of hydroxyproline in the pretreated sample solution by using a liquid chromatography tandem mass spectrometer.
As described in the above step S31, the content of hydroxyproline in the pretreated sample solution is detected by using a liquid chromatography tandem mass spectrometer, wherein the using condition of the liquid chromatography tandem mass spectrometer in the detection process is preferably a parameter in the embodiment of the present invention.
Watch 1
Referring to fig. 3, in the present embodiment, the liquid chromatography tandem mass spectrometry screening method for identifying an animal-derived product includes:
s11, shearing the object to be measured into fragments with the area less than 5mm multiplied by 5 mm;
s12, weighing 0.5g of sample.
In this embodiment, in the above method for screening animal-derived articles by liquid chromatography-tandem mass spectrometry, the volume ratio of the sample to the digesting agent is 0.5 g: 10-15 mL.
In this embodiment, in the above method for screening animal-derived products by liquid chromatography-tandem mass spectrometry, the diluent at the specified volume ratio is 1:1 in aqueous methanol.
In the present embodiment, the first prescribed temperature is 105 ℃.
In the present embodiment, the above-mentioned specified time is 16 h.
In one implementation, to verify that the test results of the method are valid, some high-risk materials in consumer goods are subjected to a benchmarking recovery test.
1. Description of the samples: 1) brown leather; 2) white cotton with glue; 3) ivory white cotton with glue; 4) camel rubber with glue; 5) brown rubber with glue.
2. And (3) a labeling process: and performing a comparison test on each material, taking two same materials with the same mass, testing one part according to a specified pretreatment method, adding a certain amount of hydroxyproline standard solution into the other part, then completely treating according to the pretreatment method, filtering, and testing on a machine. And calculating the standard adding recovery rate by combining the results of two samples of the same material with the theoretical standard adding concentration, thereby verifying whether the method is effective.
3. The analysis conditions of the instrument are as follows:
instrument type: liquid chromatography tandem mass spectrometry (Agilent 1260-Eibocaisi 4000);
a chromatographic column: a carbon 18 reverse phase chromatography column, particle size 2.7 microns, size 4.6 mm by 100 mm;
flow rate: 0.3ml per minute;
column oven: 40 ℃;
sample introduction amount: 20 microliter;
mobile phase: 0.1% formic acid in water (A) 0.1% formic acid in methanol (B);
temperature gradient:
| Time | proportion of the Mobile phase (A) | Proportion of mobile phase (B) |
| 0 minute | 90％ | 10％ |
| 4.5 minutes | 90％ | 10％ |
| 5 minutes | 50％ | 50％ |
| 5.5 |
0％ | 100％ |
| 7.5 |
0％ | 100％ |
| 8 minutes | 90％ | 10％ |
| 10 minutes | 90％ | 10％ |
A target object: trans-4-hydroxy-L-proline (chemical accession number 51-35-4);
parent ion: ion 132: 86,68,58, 132;
ion source temperature: 500 degrees celsius.
4. Standard recovery (%):
| material numbering | Concentration of the sample without adding a standard | Concentration of spiked sample | Theoretical normalized concentration | Recovery rate of added standard |
| 1 | 0.05ng/mL | 10.59ng/mL | 10ng/mL | 105.4％ |
| 2 | 1.72ng/mL | 10.26ng/mL | 10ng/mL | 85.4％ |
| 3 | 1.91ng/mL | 11.62ng/mL | 10ng/mL | 97.1％ |
| 4 | 0.48ng/mL | 23.93ng/mL | 20ng/mL | 117.2％ |
| 5 | 0.36ng/mL | 10.38ng/mL | 10ng/mL | 100.2％ |
Watch two
5. The obtained liquid chromatogram of the labeled analyte is shown in fig. 4-5, wherein fig. 4 is a liquid chromatogram with a parent ion of 132 and a daughter ion of 68, and fig. 5 is a liquid chromatogram with a parent ion of 132 and a daughter ion of 86.
The standard addition recovery experiment proves that the hydroxyproline recovery rate can reach 80-120% by using the method provided by the invention, and the requirement of conventional detection is met.
In addition, to verify the reproducibility of the test results, some positive samples were taken in the laboratory and compared among laboratories, which were: 1) yellow-earth leather; 2) light brown split pigskin; 3) black leather; 4) brown leather; 5) white imitation leather fabric.
The comparison results are shown in the third table:
| material numbering | Laboratory A results | Laboratory B results | Deviation of results |
| 1 | 61651mg/kg | 59936mg/kg | 1.41％ |
| 2 | 51405mg/kg | 54479mg/kg | 2.90％ |
| 3 | 58114mg/kg | 58835mg/kg | 0.62％ |
| 4 | 57835mg/kg | 57317mg/kg | 0.45％ |
| 5 | 44041mg/kg | 41600mg/kg | 2.85％ |
Watch III
The comparison result confirmation method has higher reproducibility and can meet the technical requirements of conventional detection.
While preferred embodiments of the present application have been described, additional variations and modifications of these embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including the preferred embodiment and all such alterations and modifications as fall within the true scope of the embodiments of the application.
Finally, it should also be noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, or article that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or terminal device. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, or article that comprises the element.
The liquid chromatography tandem mass spectrometry screening method for identifying animal-derived articles provided by the application is described in detail above, and specific examples are applied in the text to explain the principle and the implementation of the application, and the description of the above examples is only used to help understand the method and the core ideas of the application; meanwhile, for a person skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.
Claims (10)
1. A liquid chromatography tandem mass spectrometry screening method for identifying animal-derived goods is used for detecting the content of hydroxyproline in a consumable product, and is characterized by comprising the following steps: sampling; pretreating and detecting the content of hydroxyproline in the pretreated sample solution;
wherein the pretreatment step comprises:
mixing a sample with a digesting agent with specified mass, and carrying out reflux digestion treatment for a specified time at a first specified temperature;
and adding a diluent with a specified volume ratio for dilution treatment to obtain a pretreated sample solution.
2. The method for screening by liquid chromatography-tandem mass spectrometry for identifying an animal-derived product according to claim 1, wherein the step of mixing the sample with a digesting agent of a specified mass and performing a refluxing digestion process at a first specified temperature for a specified time comprises:
mixing the sample with a digesting agent of a specified mass in a closed container;
the closed vessel was subjected to reflux digestion at a first specified temperature for a specified time.
3. The method for screening animal-derived products according to claim 2, wherein the step of adding a specified volume ratio of diluent to dilute the sample solution to obtain a pre-treated sample solution comprises:
cooling the sample liquid to a second specified temperature;
and adding a diluent with a specified volume ratio to dilute the sample solution to a specified multiple, and filtering to obtain a pretreated sample solution.
4. The method for screening by liquid chromatography-tandem mass spectrometry for identifying an animal-derived product according to claim 3, wherein the step of detecting the content of hydroxyproline in the pretreated sample solution comprises:
and detecting the content of hydroxyproline in the pretreated sample solution by using a liquid chromatography tandem mass spectrometer.
5. The method for screening by LC-MS/MS of claim 4, wherein the step of detecting the content of hydroxyproline in the pretreated sample solution by LC-MS comprises:
the first mobile phase is an aqueous solution containing 0.1% formic acid;
the second mobile phase was methanol containing 0.1% formic acid;
the flow rate is: 0.3 mL/min;
gradient: at the beginning, the current mobile phase consists of 90% of the first mobile phase and 10% of the second mobile phase;
when the time reaches 4.5min, the current mobile phase is adjusted to be composed of 90% of the first mobile phase and 10% of the second mobile phase;
when 5min is reached, the current mobile phase is adjusted to be composed of 50% of first mobile phase and 50% of second mobile phase;
when 5.5min is reached, the current mobile phase remains composed of 100% of the second mobile phase;
when 7.5min is reached, the current mobile phase remains composed of 100% of the second mobile phase;
when 8min is reached, the current mobile phase is adjusted to be composed of 90% of the first mobile phase and 10% of the second mobile phase;
at 10min, the current mobile phase was adjusted to consist of 90% of the first mobile phase and 10% of the second mobile phase.
6. The method of claim 1, wherein the step of sampling comprises:
shearing the object to be detected into fragments with the area less than 5mm multiplied by 5 mm;
0.5g of sample was weighed.
7. The method for screening by liquid chromatography-tandem mass spectrometry for identifying an animal-derived product according to claim 1, wherein the volume ratio of the sample to the digesting agent is 0.5 g: 10-15 mL.
8. The method for screening by liquid chromatography-tandem mass spectrometry for identifying an animal-derived product according to claim 1, wherein the specified volume ratio of the diluent is 1:1 in aqueous methanol.
9. The method of liquid chromatography-tandem mass spectrometry screening of identifying an animal-derived item as claimed in claim 1, wherein the first specified temperature is 105 ℃.
10. The method for liquid chromatography-tandem mass spectrometry screening of an animal-derived item for identification as claimed in claim 1, wherein the specified time is 16 h.
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| CN109085278A (en) * | 2018-08-06 | 2018-12-25 | 杭州佰勤医疗器械有限公司 | Liquid chromatography tandem mass spectrometry detects kit and its application of a variety of amino acid simultaneously |
| CN110470766A (en) * | 2019-08-30 | 2019-11-19 | 天津云检医学检验所有限公司 | A kind of semi-quantitative analysis method of amino acid, fatty acyl carnitine and fatty acid |
| CN111189939A (en) * | 2020-01-14 | 2020-05-22 | 上海市农业科学院 | Method for detecting endogenous free amino acids of plants by using ultra-high performance liquid chromatography-tandem mass spectrometry |
| CN111289671A (en) * | 2020-02-15 | 2020-06-16 | 安徽农业大学 | Enrichment detection method of free D-type amino acid |
| CN112730723A (en) * | 2020-12-30 | 2021-04-30 | 申友基因组研究院(南京)有限公司 | Method for detecting 22 free amino acids in plasma by ultra-high performance liquid chromatography-tandem mass spectrometry |
| CN113804806A (en) * | 2021-10-20 | 2021-12-17 | 厦门市燕之屋丝浓食品有限公司 | Ultra-high performance liquid chromatography-tandem mass spectrometry determination method for amino acids in bird's nest |
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