CN114062570A - Method for evaluating quality of pinellia ternate and sparrow lawn pinellia ternate based on organic acid - Google Patents
Method for evaluating quality of pinellia ternate and sparrow lawn pinellia ternate based on organic acid Download PDFInfo
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Abstract
The invention discloses a method for evaluating the quality of pinellia ternate and sparrow lawn pinellia ternate based on organic acid, and belongs to the field of chemical component analysis of traditional Chinese medicines. The method utilizes 75% ethanol to extract the total organic acid components of the tubers of the pinellia ternata and the sparrow lawn pinellia ternata through heating and refluxing, and uses ethyl acetate to extract repeatedly to remove impurities, so as to obtain an organic acid extracting solution. Detecting the extracting solution by using UPLC-MS/MS, qualitatively analyzing the organic acid components by using a standard substance database to identify 109 organic acid components in total, quantitatively detecting by using a multi-reaction detection mode MRM of triple quadrupole mass spectrometry, and screening 91 organic acid components with significant difference in content by combining a difference multiple of more than 2 times or less than 0.5 time. The invention provides an excellent technical means for evaluating the quality of the pinellia ternate and the sparrow lawn pinellia ternate by utilizing the organic acid, and has important application value in the quality control and the type identification of the pinellia ternate drugs.
Description
Technical Field
The invention belongs to the field of chemical component analysis of traditional Chinese medicines, and particularly relates to a method for evaluating the quality of pinellia ternate and rays of lawn pinellia ternate based on organic acid.
Background
Pinellia ternate (Pinellia ternate) is a perennial herb of Pinellia ternate (Pinellia) of Araceae, and is mainly distributed in Hubei, Henan, Anhui, Shandong, Sichuan and the like; the tuber is used as a medicine, has the effects of relieving cough, eliminating phlegm, stopping vomiting, calming, hypnosis, resisting tumor and the like, and is a large amount of medicinal materials commonly used in China. The sparrow lawn pinellia ternate (Pinelliayaoluopinensis) is a special species of the national natural protection area of the Bian lawn, has similar efficacy with the pinellia ternate, but has faster efficacy than the pinellia ternate, and is possibly related to chemical components of the ban.
Research shows that organic acid is an important chemical component of pinellia ternata, mainly comprises succinic acid, oxalic acid, malic acid, aconitic acid, formic acid, acetic acid and the like, and has correlation with cough relieving and phlegm eliminating effects. 2015 edition of Chinese pharmacopoeia records that the content determination of organic acid in pinellia ternata adopts potentiometric titration method, and the quality is controlled by calculating succinic acid content; however, the method only can roughly reflect the content of organic acid components of the pinellia ternata, and the types of the organic acid components cannot be analyzed. In the prior art, Zhaixing and the like perform species analysis on chemical components of a semi-summer by using an ultra performance liquid chromatography-time of flight mass spectrometry (UPLC-Q-TOF-MS/MS), but do not perform extraction, separation and detection on organic acid components of pinellia ternata, so that the identified organic acid species are few. At present, the research on the organic acid component of the stinging lawn pinellia is rarely reported.
Therefore, the method for extracting and measuring the organic acid components of the pinellia ternata and the rays of the lawn pinellia ternata needs to be optimized, and the types and the content differences of the organic acid components of the pinellia ternata and the rays of the lawn pinellia ternata are deeply compared, so that references are provided for the quality control and the type identification of the pinellia ternata.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for evaluating the quality of pinellia ternate and rays of lawn pinellia ternate based on organic acid, and particularly adopts UPLC-MS (ultra Performance Liquid Chromatography Mass Spectrometry) to detect the organic acid components and the content of the pinellia ternate and rays of lawn pinellia ternate, so as to evaluate and compare the quality of the pinellia ternate and rays of lawn pinellia ternate.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for evaluating the quality of pinellia ternate and sparrow lawn pinellia ternate based on organic acid comprises the following steps:
(1) deactivating enzymes of a sample to be detected, baking the sample to be detected to constant weight, grinding and sieving the sample, and collecting powder, wherein the sample to be detected is tuber of pinellia ternata or snipe turfgrass tuber of pinellia ternata;
(2) mixing the powder obtained in the step (1) with an ethanol solution, carrying out hot reflux extraction, and carrying out reduced pressure concentration to obtain an organic acid crude extract;
(3) adjusting the pH value of the organic acid crude extract obtained in the step (2) to 10-12 by using an anhydrous sodium carbonate aqueous solution, repeatedly extracting by using ethyl acetate until the extract is colorless, and combining the extract;
(4) acidifying the extract obtained in the step (3) with hydrochloric acid until the pH value is 2-3, repeatedly extracting with ethyl acetate, and combining the extract;
(5) evaporating the extract liquid obtained in the step (4) to dryness under reduced pressure, and redissolving the extract liquid with an ethanol solution to obtain a sample to be detected of total free organic acid;
(6) detecting the total free organic acid sample to be detected (including a quality control sample QC) by using an ultra performance liquid chromatography-tandem mass spectrometry, and performing qualitative and quantitative analysis on the components of the total free organic acid sample to be detected by using a standard substance database and a multi-Reaction detection mode MRM (multiple Reaction monitoring) of a triple quadrupole mass spectrometry;
(7) based on the results of the qualitative and quantitative analyses in step (6), the specific components of the total free organic acids and their contents difference in the pinellia ternata and the rays of lawn pinellia ternata were obtained.
Preferably, in the step (1), the water-removing temperature is 100-110 ℃, and the water-removing time is 10-20 min; the baking temperature is 50-60 ℃, and the baking time is 24-72 hours; the sieving mesh number of the sample powder is 50-70 meshes.
Preferably, in the step (2), the ratio of the mass of the powder to the volume of the ethanol solution is 300-500 mg: 3-5 mL; the hot reflux extraction temperature is 60-80 ℃, the extraction time is 1-2 h, and the extraction times are 2-3; the concentration of the ethanol solution is 70-80%.
Preferably, in the step (3), the concentration of the anhydrous sodium carbonate aqueous solution is 3% -5%, and the extraction times of ethyl acetate are 3-5 times; in the step (4), the extraction times of ethyl acetate are 3-5 times.
Preferably, the chromatographic detection conditions in the step (6) are as follows: the column was an Agilent SB-C181.8 μm.times.2.1 mm.times.100 mm; the mobile phase A is formic acid water solution with volume concentration of 0.1%, and the mobile phase B is formic acid acetonitrile solution with volume concentration of 0.1%.
Preferably, the mobile phase flow rate: 0.35 mL/min; the column temperature of the chromatographic column is 40 ℃; the sample injection amount is specifically 4 mu L; elution gradient: the proportion of the B phase is 5% at 0.00min, the B phase is linearly increased to 95% within 9.00min and is maintained at 95% for 1min and 10.00-11.10 min, the B phase is decreased to 5% and is balanced to 14min by 5%.
Preferably, the mass spectrum detection condition in the step (6): linear Ion TRAP (LIT) and triple quadrupole (QQQ) scans were obtained on a triple quadrupole linear ion TRAP mass spectrometer (Q TRAP), AB 4500Q TRAP plc/MS system equipped with ESI Turbo ion spray interface, operating both positive and negative ion modes controlled by analyst1.6.3 software (AB Sciex).
Preferably, the electrospray ion source (ESI) operating parameters are: an ion source, turbo spray; the source temperature is 550 ℃; ion spray voltage (IS)5500V (positive ion mode)/-4500V (negative ion mode); ion source gas i (gsi), gas ii (gsii) and curtain gas (CUR) were set at 50, 60 and 25psi, respectively, and the impact induced ionization parameter was set high.
Preferably, instrument tuning and mass calibration is performed with 10. mu. mol/L and 100. mu. mol/L polypropylene glycol solutions in QQQ and LIT modes, respectively; the QQQ scan uses MRM mode and sets collision gas (nitrogen) to medium; completing DP and CE of each MRM ion pair by optimizing the declustering voltage (DP) and the collision voltage (CE); a specific set of MRM ion pairs is monitored at each time period based on the metabolites eluted during each time period.
Preferably, the standard substance database is specifically MWDB.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method is characterized by extracting organic acids as core medicinal components of the pinellia ternata, removing impurities from the obtained crude extract of the total organic acids to obtain a relatively pure total organic acid extract of the pinellia ternata, detecting by using UPLC-MS/MS, analyzing by combining a standard substance database, identifying 109 organic acid components (104 organic acids are not shown or are not reported), and screening to obtain 91 organic acid components with obvious content difference in the pinellia ternata and the sparrow lawn pinellia ternata, wherein the sparrow lawn pinellia ternata is higher than the pinellia ternata;
(2) the method provided by the invention can be used for analyzing organic acid components of common pinellia ternate and Anhui rays lawn country-level natural protection area specific rays, and can also be used for comparative analysis research of the common pinellia ternate and Anhui rays lawn pinellia ternate, and the method has important application value and prospect in judging the potential and difference of medicinal effects of the common pinellia ternate and the Anhui rays lawn pinellia ternate, for example, can be used for further clarifying the reason that the medicinal effect of the rays and lawn pinellia ternate is faster than that of the common pinellia ternate. The invention provides an excellent technical means for quality control of pinellia, and also provides a technical support for development and utilization of the rays of the Pink pinellia in the later period.
Drawings
FIG. 1 is a total ion flow diagram of pinellia ternate and rays of lawn pinellia ternate organic acid component in positive ion mode;
FIG. 2 is a total ion flow diagram of pinellia ternate and rays of lawn pinellia ternate in an anion mode;
FIG. 3 is a thermal map of the differential organic acid composition of pinellia and stinging lawn of pinellia, the names of the organic acids on the right side of the thermal map being in order from top to bottom: tridecanedioic acid, 2-methylsuccinic acid, glutaric acid, 2-aminoisobutyric acid, suberic acid, 3-hydroxycinnamic acid, vanillic acid, L-malic acid, 6-aminocaproic acid, hexadecyl diacid, isoferulic acid, ferulic acid, citric acid, succinic acid, isocitric acid, methylmalonic acid, 4-acetylaminobutyric acid, azelaic acid, quinic acid, 4-guanidinobutyric acid, 3-dehydro-L-threonic acid, 3-amino-2-naphthoic acid, 4-pentenoic acid, monomethylglutaric acid, 3- (3-hydroxyphenyl) -3-hydroxypropionic acid, 3-methacrylic acid, methylbutenoic acid, 2-methylglutaric acid, 2-propylsuccinic acid, gamma-aminobutyric acid, p-coumaric acid, fumaric acid, 2-hydroxyisocaproic acid, Protocatechuic acid, 2- (formylamino) benzoic acid, tetradecanedioic acid, malonic acid, caffeic acid, sinapic acid, citraconic acid, 1-methylpiperidine-2-carboxylic acid, 3-methylmalic acid, 2-furancarboxylic acid, phenylpyruvic acid, beta-hydroxyisovaleric acid, mandelic acid, aminomalonic acid, gentisic acid, 5-acetylaminovaleric acid, adipic acid, pimelic acid, 2-propylmalic acid, 2-isopropylmalic acid, 3-O-feruloylquinic acid, cinnamic acid, p-hydroxyphenylacetic acid, 3-methylsalicylic acid, pyrrole-2-carboxylic acid, sebacic acid, 3, 4-dihydroxybenzeneacetic acid, cis-p-coumaroyltartaric acid, 5-methoxysalicylic acid, D-galacturonic acid, 2-methylmalic acid, ethylmalonic acid, Tranexamic acid, 10-hydroxydecanoic acid, acetoxyacetic acid, dodecanedioic acid, 3-hydroxymandelic acid, 3-methoxybenzoic acid, trans-5-O-p-coumaroylshikimic acid, glucono-syringic acid, feruloyl syringic acid, 3-hydroxyglutaric acid, DL-3-phenyllactic acid, gentisic acid, 2-hydroxy-3-phenylpropionic acid, 2-hydroxyethylphosphonic acid, 6-hydroxyhexanoic acid, D-xylonic acid, hydroxyphenyllactic acid, dimethylmalonic acid, 2-propylglutaric acid, 9-oxononanoic acid, alpha-ketoglutaric acid, 2-hydroxy-2-methyl-3-oxobutanoic acid, 3, 4-dihydroxybenzeneacetic acid, 3-hydroxy-3-methyl-2-oxopentanoic acid, 2-hydroxy-4-methylvaleric acid, 2-acetyl-2-hydroxybutyric acid.
Detailed Description
The following examples are given by way of illustration and not by way of limitation.
Example 1: extraction and detection of organic acid components of pinellia ternata and sparrow lawn pinellia ternata
1. Instrument and reagent
(1) The instrument comprises the following steps: ultra high performance liquid chromatograph UPLC (SHIMADZU Nexera X2) and tandem mass spectrometer MS/MS (Applied Biosystems 4500QTRAP), high speed universal pulverizer.
(2) Reagent testing: pinellia ternate and sparrow lawn pinellia ternate tuber materials are provided by the bioscience institute of the symposium fertilizer academy of sciences, ethanol, acetonitrile, formic acid and ethyl acetate are in chromatographic grade, and other reagents are analytically pure.
2. Pretreatment of materials
Cleaning the freshly collected tubers of the pinellia ternata and the sparrow lawn pinellia ternata with clear water, slicing, deactivating enzymes in a 105 ℃ oven for 15min, and drying at 60 ℃ to constant weight (48 h). Then, the mixture is ground into powder by a high-speed universal grinder and then sieved by a 60-mesh sieve.
3. Extraction of total free organic acids
(1) Weighing 300-500 mg of dried pinellia ternate and stinging lawn pinellia ternate powder into a centrifuge tube, adding 3-5 mL of 75-80% ethanol, heating and refluxing at 60-80 ℃ for 2-3 times, extracting for 1-2 h each time, combining the extracting solutions, and evaporating to dryness under reduced pressure to concentrate to a small volume;
(2) adding 3-5% anhydrous sodium carbonate solution, adjusting the pH value to 11, repeatedly extracting for 3-5 times by using ethyl acetate, and combining the extract liquor;
(3) acidifying the extract obtained in the step (2) with hydrochloric acid until the pH value reaches 2, repeatedly extracting with ethyl acetate for 3-5 times, and combining the extract;
(4) and (4) evaporating the extract obtained in the step (3) to dryness under reduced pressure, re-dissolving the extract with 1-2 mL of 75% ethanol, and filtering the re-dissolved extract through a 0.22-micrometer microporous filter membrane to obtain a sample.
4. Detection analysis of samples
(1) Chromatographic conditions
The chromatographic column is Agilent SB-C181.8 μm × 2.1mm × 100 mm; mobile phase: phase A is ultrapure water (with 0.1% formic acid added), phase B is acetonitrile (with 0.1% formic acid added); flow rate: 0.35 mL/min; the column temperature is 40 ℃; the sample volume is 4 mu L; elution gradient: the proportion of the B phase is 5% at 0.00min, the B phase is linearly increased to 95% within 9.00min and is maintained at 95% for 1min and 10.00-11.10 min, the B phase is decreased to 5% and is balanced to 14min by 5%.
(2) Conditions of Mass Spectrometry
Linear Ion TRAP (LIT) and triple quadrupole (QQQ) scans were obtained on a triple quadrupole linear ion TRAP mass spectrometer (Q TRAP), AB 4500Q TRAP UPLC/MS system equipped with an ESI Turbo ion spray interface, operating in both positive and negative ion modes controlled by Analyst1.6.3 software (AB Sciex). ESI source operating parameters: an ion source, turbo spray; the source temperature is 550 ℃; ion spray voltage (IS)5500V (positive ion mode)/-4500V (negative ion mode); ion source gas i (gsi), gas ii (gsii) and curtain gas (CUR) were set at 50, 60 and 25psi, respectively, and the impact induced ionization parameter was set high.
Instrument tuning and mass calibration were performed in QQQ and LIT modes with 10 μmol/L and 100 μmol/L polypropylene glycol solutions, respectively. The QQQ scan uses the MRM mode and sets the collision gas (nitrogen) to medium. Through further DP and CE optimization, the DP and CE of each MRM ion pair is completed. A specific set of MRM ion pairs is monitored at each time period based on the metabolites eluted during each time period.
In the quality control sample QC, a to-be-detected sample of the total free organic acid of the pinellia ternata and a to-be-detected sample of the total free organic acid of the stingray lawn are mixed in equal volume and are used for analyzing the repeatability of the sample under the same treatment method. The self-built database MWDB is a standard substance database built by Wuhan Miteville Biotechnology Limited and contains 5000 kinds of plants and metabolites in Chinese medicinal materials.
5. Qualitative analysis of organic acid composition
Based on the self-built database MWDB, the material is characterized according to the second-level spectrum information, isotope signals are removed during analysis, and the K content+、Na+、NH4 +And the fragment ions which are themselves other higher molecular weight species. From pinellia ternate and spartina rays lawn pinellia ternate, 109 organic acid components are identified, wherein oxalic acid, malic acid, citric acid, succinic acid and trans-aconitic acid are reported in the pinellia ternate, and the rest 104 organic acids are not or rarely reported. Specific results are shown in table 1.
TABLE 1 separation and identification of organic acid components from pinellia and stinging lawn pinellia
Example 2: screening of pinellia ternate and sparrow lawn pinellia ternate differential organic acid components
1. Quantitative analysis of organic acid content
And (3) processing mass spectrum data by using software analysis 1.6.3 to obtain a total ion flow diagram (TIC) of the metabolites of the pinellia ternata and the stinging lawn pinellia ternata. And (4) screening out characteristic ions of each substance through a triple quadrupole, and performing integration and correction of chromatographic peaks by using MultiaQuant software to complete quantitative analysis of organic acid components.
2. Screening for differential organic acid composition
Comparing the chromatographic peak integrals (peak areas) of different organic acid components of the pinellia ternate and the sparrow lawn pinellia ternate, wherein the difference multiples are more than 2 times or less than 0.5 time, namely the screened different organic acid components.
As can be seen from the graphs in FIGS. 1 and 2, the total ion flow chart (TIC) peaks of the pinellia ternate and the rays lawn pinellia ternate in the positive and negative ion modes are different, which indicates that the organic acid contents of the two pinellites are different. Further, the organic acid components having significant differences in content were screened using the peak area difference multiple (greater than 2 times or less than 0.5 times) of the substances, and the results are shown in fig. 3. Among the 109 organic acids, 91 organic acids have significant difference between the two pinellia ternate types, and the content of 5 organic acids which are all the stinging lawn pinellia ternate is higher than that of the pinellia ternate, particularly 4-pentenoic acid, 3-methacrylic acid, methyl butenoic acid, monomethyl glutaric acid and 3- (3-hydroxyphenyl) -3-hydroxypropionic acid, and the difference multiples are 13578 times, 6204 times, 7149 times, 22281 times and 2914 times respectively, which indicates that the stinging lawn pinellia ternate has better quality than the pinellia ternate.
The present invention is described in additional detail with reference to the specific embodiments, which are provided for further illustration only, and do not represent the scope of the present invention, and other insubstantial modifications and adaptations of the invention based on the teachings of the present invention will still fall within the scope of the present invention.
Claims (10)
1. A method for evaluating the quality of pinellia ternate and sparrow lawn pinellia ternate based on organic acid is characterized by comprising the following steps of:
(1) deactivating enzymes of a sample to be detected, baking the sample to be detected to constant weight, grinding and sieving the sample, and collecting powder, wherein the sample to be detected is tuber of pinellia ternata or snipe turfgrass tuber of pinellia ternata;
(2) mixing the powder obtained in the step (1) with an ethanol solution, carrying out hot reflux extraction, and carrying out reduced pressure concentration to obtain an organic acid crude extract;
(3) adjusting the pH value of the organic acid crude extract obtained in the step (2) to 10-12 by using an anhydrous sodium carbonate aqueous solution, repeatedly extracting by using ethyl acetate until the extract is colorless, and combining the extract;
(4) acidifying the extract obtained in the step (3) with hydrochloric acid until the pH value is 2-3, repeatedly extracting with ethyl acetate, and combining the extract;
(5) evaporating the extract liquid obtained in the step (4) to dryness under reduced pressure, and redissolving the extract liquid with an ethanol solution to obtain a sample to be detected of total free organic acid;
(6) detecting the total free organic acid sample to be detected by using ultra performance liquid chromatography-tandem mass spectrometry, and performing qualitative and quantitative analysis on the components of the total free organic acid sample to be detected by using a standard substance database and a multi-reaction detection mode MRM of triple quadrupole mass spectrometry;
(7) based on the results of the qualitative and quantitative analyses in step (6), the specific components of the total free organic acids and their contents difference in the pinellia ternata and the rays of lawn pinellia ternata were obtained.
2. The method for evaluating the quality of pinellia ternate and sparrow lawn pinellia ternate based on organic acid as claimed in claim 1, wherein in the step (1), the green removing temperature is 100-110 ℃, and the green removing time is 10-20 min; the baking temperature is 50-60 ℃, and the baking time is 24-72 hours; the sieving mesh number of the sample powder is 50-70 meshes.
3. The method for evaluating the quality of pinellia ternate and sparrow lawn pinellia ternate based on organic acid as claimed in claim 1, wherein in the step (2), the ratio of the mass of the powder to the volume of the ethanol solution is 300-500 mg: 3-5 mL; the hot reflux extraction temperature is 60-80 ℃, the extraction time is 1-2 h, and the extraction times are 2-3; the concentration of the ethanol solution is 70-80%.
4. The method for evaluating the quality of pinellia ternate and sparrow lawn pinellia ternate based on organic acid as claimed in claim 1, wherein in the step (3), the concentration of the anhydrous sodium carbonate aqueous solution is 3% -5%, and the extraction time of ethyl acetate is 3-5 times; in the step (4), the extraction times of ethyl acetate are 3-5 times.
5. The method for evaluating the quality of pinellia ternate and rays lawn pinellia ternate based on organic acids as claimed in claim 1, wherein the chromatographic detection conditions in the step (6) are as follows:
a chromatographic column: agilent SB-C181.8 μm 2.1mm 100 mm;
mobile phase: the A phase is formic acid water solution with volume concentration of 0.1%, and the B phase is formic acid acetonitrile solution with volume concentration of 0.1%.
6. The method for evaluating the quality of pinellia and sparrow lawn pinellia based on organic acid as claimed in claim 5, wherein:
flow rate of mobile phase: 0.35 mL/min; the column temperature of the chromatographic column is 40 ℃; the sample volume is 4 mu L;
elution gradient: the proportion of the B phase is 5% at 0.00min, the B phase is linearly increased to 95% within 9.00min and is maintained at 95% for 1min and 10.00-11.10 min, the B phase is decreased to 5% and is balanced to 14min by 5%.
7. The method for evaluating the quality of pinellia ternate and sparrow lawn pinellia ternate based on organic acid as claimed in claim 1, wherein the mass spectrum detection condition in the step (6):
the linear ion trap and the triple quadrupole scanning are obtained on a triple quadrupole linear ion trap mass spectrometer, AB4500 QTRAP UPLC/MS/MS system, the system is provided with an ESI Turbo ion spray interface, and the operation of positive and negative ion modes is controlled by analysis 1.6.3 software.
8. The method for evaluating the quality of pinellia and sparrow lawn pinellia based on organic acids as claimed in claim 7, wherein the electrospray ion source operating parameters are: an ion source, turbo spray; the source temperature is 550 ℃; ion spray voltage 5500V/-4500V; ion source gas I, gas II and curtain gas were set at 50, 60 and 25psi, respectively, and the impact induced ionization parameter was set high.
9. The method for evaluating the quality of pinellia and sparrow lawn pinellia based on organic acids as claimed in claim 7, wherein the instrument tuning and quality calibration are performed with polypropylene glycol solutions of 10 μmol/L and 100 μmol/L in QQQ and LIT modes, respectively; the QQQ scan uses MRM mode and sets the collision gas nitrogen to medium; the DP and CE of each MRM ion pair are completed by optimizing the cluster removing voltage and the collision voltage; a specific set of MRM ion pairs is monitored at each time period based on the metabolites eluted during each time period.
10. The method for evaluating the quality of pinellia ternate and stinging lawn pinellia ternate based on organic acids as claimed in claim 1, wherein in the step (6), the standard substance database is specifically MWDB.
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| CN117451903A (en) * | 2023-12-25 | 2024-01-26 | 南京市食品药品监督检验院 | Method for simultaneously detecting 14 organic acids in fruit wine |
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| CN117451903A (en) * | 2023-12-25 | 2024-01-26 | 南京市食品药品监督检验院 | Method for simultaneously detecting 14 organic acids in fruit wine |
| CN117451903B (en) * | 2023-12-25 | 2024-02-23 | 南京市食品药品监督检验院 | Method for simultaneously detecting 14 organic acids in fruit wine |
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