CN108195957A - The high performance liquid chromatography tandem mass spectrum detection method of phenolic acid in a kind of wheat being simple and efficient - Google Patents
The high performance liquid chromatography tandem mass spectrum detection method of phenolic acid in a kind of wheat being simple and efficient Download PDFInfo
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Abstract
The present invention discloses a kind of high performance liquid chromatography tandem mass spectrum detection method of phenolic acid in wheat being simple and efficient, it will be completely dissolved in the sodium hydroxide solution of 2mol/L by the wheat samples of 0.425mm hole sizers completely, under the conditions of being protected from light after nitrogen charging hydrolysis, it adopts and is extracted with ethyl acetate, upper organic phase rotation is taken to be evaporated.Residue is molten using 50% methanol weight, and 4 DEG C of preservations are to be measured after crossing 0.22 μm of filter membrane；Sample to be tested is detected using high performance liquid chromatography tandem mass spectrum method, does standard curve with phenolic acid standard items, testing result substitutes into standard curve and is compared, and obtains the content of phenolic acid in wheat samples；The detection method extraction step is simple, takes that short high sensitivity, stability are good, and the content suitable in high volume quantitatively detecting phenolic acid wheat samples can provide accurate analysis method for the assessment of agricultural product trophic function.
Description
Technical field
The present invention relates to agricultural product trophic function detection technique field, phenolic acid in particularly a kind of wheat being simple and efficient
High performance liquid chromatography tandem mass spectrum detection method.
Background technology
Phenolic acid (phenolic acid) refers to a kind of compound for having several phenolic hydroxyl group on same phenyl ring, itself has
Play the role of preferably removing free radical, therefore be a kind of good natural.There is antioxygen there are many containing in wheat
Change property phenolic acid, mainly have gallic acid, protocatechuic acid, 4-HBA, vanillic acid, caffeic acid, syringic acid, coumaric acid,
Ferulic acid, sinapic acid.These phenolic acid with natural anti-oxidation, have caused the common concern of people.
Research of the healthcare function possessed by phenolic acid through multidigit scholar is mainly manifested in:It is (cardiovascular to remove interior free yl
A variety of diseases such as disease formation it is related with the formation of extra free radical), vasodilator, anticancer, antiviral, antibacterial anti-inflammatory,
Antiallergy generates cancer cell blood vessel blocking element, stimulation immuning system generating antibody, inhibits phosphatidase, lipoxidase, ring oxygenation
The activity of the enzymes such as enzyme, xanthine oxidase.
The assessment of agricultural product trophic function is to weigh the important indicator of a national agricultural product quality.It is a variety of in agricultural product at present
There are no standard methods for the detection of phenolic acid, and the analysis method of a small number of phenolic acid is mainly high performance liquid chromatography, existing report document
《Phenolic acid composition and antioxidant potential of insoluble andsoluble
dietary fibre extracts derived from select whole-grain cereals》In, for phenolic acid
Extraction is separately extracted by free phenolic acid and with reference to phenolic acid, and this extracting method is complicated, and extraction needs 4 hours, is detected with efficient
Liquid chromatographic detection, a length of 70min of detection time；Also document《Ultra performance liquid chromatography-tandem mass spectrometry measures 5 simultaneously
23 kinds of phenolic acid compounds in place of production cauliflower and broccoli》In, the extraction for phenolic acid is also by free phenolic acid and combination
Phenolic acid separately extracts, and total extraction time needs 5 hours, is detected at present using ultra performance liquid chromatography-tandem mass spectrum, detection limit
For 500 μ g/kg, the detection of the sample low to content has limitation.
High performance liquid chromatography tandem mass spectrum method be it is a kind of integrate efficiently separate the side qualitative, quantitative with multicomponent
Method, separation to heat-labile compound such as phenolic acid and quantitatively has unique advantage.But due to instrument precision, the spies such as sensitivity height
Point is higher to the purity requirement of sample.Wheat samples protein, content of starch are higher, these ingredients how to be allowed not interfere
The detection of phenolic acid is relatively difficult.
Existing liquid chromatography detecting method extracts complicated and time consumption, and detection time is long, and sensitivity is low, it is impossible to meet high-volume
The quick requirement for weighing detection of sample.Vegetables matrix and wheat matrix are different, phenolic acid type also difference in two kinds of matrix,
Still lack at present can it is quick to phenolic acid a variety of in wheat simultaneously, sensitively weigh determination method.
Invention content
In view of the above-mentioned problems, the present invention provides a kind of high performance liquid chromatography tandem mass spectrum of phenolic acid in wheat being simple and efficient
Detection method, i.e., first extract sample purifying, and refined solution is examined through high performance liquid chromatography tandem mass spectrum technology (LC/MS/MS)
It surveys, the content of phenolic acid in sample is quantitative determined finally by standard curve, without separated extraction free phenolic acid and with reference to phenolic acid, contracting
Short detection time.
The invention is realized in this way：
The high performance liquid chromatography tandem mass spectrum detection method of phenolic acid, is as follows in a kind of wheat being simple and efficient,
(1) sample cleanup
2.00g wheat samples accurately are weighed in 250mL triangular flasks, according to mass volume ratio 20:1 (g/ml) measures 40mL
The NaOH of 2mol/L is added in triangular flask, seals up bottleneck rapidly after being quickly filled with nitrogen, oscillation is protected from light under the conditions of 25 DEG C
(2500rpm) hydrolyzes 2h, and hydrolyzate pH value is adjusted after hydrolysis between 1.5-2.0.
The accurate 50mL ethyl acetate that measures is added in triangular flask, 10min is sufficiently mixed with hydrolyzate, under conditions of 4 DEG C
10000rpm centrifuges 5min, takes upper strata ethyl acetate layer, repeats this operation three times, merges all ethyl acetate layers in 40 DEG C of conditions
Lower rotation is evaporated, and residue is molten using methanol (volume ratio) weight of 10mL 50%, and 4 DEG C of preservations are to be measured after crossing 0.22 μm of filter membrane；
(2) 9 kinds of phenolic acid standard items (gallic acid, protocatechuic acid, 4-HBA, vanillic acid, caffeic acid, cloves are taken
Acid, P- coumaric acids, ferulic acid, sinapic acid) and standard reserving solution is configured to, it is diluted, prepared step by step with 50% (volume ratio) methanol
Be followed successively by 0.2 into concentration, 0.3,6,24,100, the phenolic acid standard solution of 200mg/L, carry out high performance liquid chromatography series connection matter respectively
Spectrum detection, establishes standard curve.
(3) in high performance liquid chromatography tandem mass spectrum detection, testing result generation, are carried out to the sample cleanup liquid that step (1) obtains
Enter the standard curve of step (2) acquisition, quantified by external standard method calculates the concentration of each phenolic acid in sample, then is calculated according to formula (1)
The content of phenolic acid in sample；
In formula：
X --- the content of component to be measured in sample, unit for milligrams per kilogram, mg/kg；
C --- the concentration of component to be measured in liquid is measured, unit is micrograms per millilitre, μ g/mL；
V --- constant volume, unit are milliliter, mL；
M --- sample sample weighting amount, unit for gram, g.
Further, in the wheat of the present invention being simple and efficient phenolic acid high performance liquid chromatography tandem mass spectrum detection method,
The high performance liquid chromatography tandem mass spectrum detection specifically refers to：
1) chromatographic condition：
A) chromatographic column：Agilent XDB-C18-2014-3.5μm-2.1*150mm；
B) sample size：2μL
C) column temperature：40℃
D) flow velocity：0.5mL/min
E) mobile phase and elution time：
Mobile phase A：Aqueous solution containing 1% (volume ratio) formic acid；
Mobile phase B:Acetonitrile containing 1% (volume ratio) formic acid；
Using linear gradient elution
Elution time 0-5min, liquid phase A is from 90% to 60%, and Mobile phase B is from 10% to 40%；
Elution time 5-12min, mobile phase A is from 60% to 10%, and Mobile phase B is from 40% to 90%；
Elution time 12-15min, mobile phase A is from 10% to 90%, and Mobile phase B is from 90% to 10%；
Single sample run time is 15min in total；
(2) Mass Spectrometry Conditions：
Ionization mode is electron spray ionisation negative ion mode (ESI-)；Multiple-reaction monitoring (MRM)；Ion source temperature 500
℃；Residence time 100ms；Atomization air pressure 50psi；Assist gas pressure 50psi；Spray voltage -4500V, collision cell project voltage 6V.
Further, in the herein described wheat being simple and efficient phenolic acid high performance liquid chromatography tandem mass spectrum detection method
In, wheat samples powder used in step (1) referred to the wheat samples powder after 0.425mm hole sizers.
Further, in the herein described wheat being simple and efficient phenolic acid high performance liquid chromatography tandem mass spectrum detection method
In, step (1) the hydrolyzate pH value that adjusts refers between 1.5-2.0：Hydrolyzate pH is adjusted with the hydrochloric acid solution of 1mol/L
Value is between 1.5-2.0.
The high performance liquid chromatography tandem mass spectrum detection method of phenolic acid, can apply in a kind of wheat being simple and efficient of the present invention
The extraction and detection of common 9 kinds of phenolic acid in wheat.It is simple, time-consuming short, sensitive with extraction compared with other detection methods
High, the features such as stability is good, entire detection process takes 15 minutes 2 hours.(hydrolysis 2 hours, instrument detect 15 minutes) can fit
For the quantitative detection of phenolic acid in high-volume wheat samples.The foundation of this method enables the phenolic acid in high-volume wheat accurately to survey
It is fixed, it can be assessed for agricultural product trophic function and fast and accurately analysis method is provided.
Description of the drawings
Fig. 1 is 300 μ g/L protocatechuic acid standard items chromatograms；
Fig. 2 is 300 μ g/L 4-HBA standard items chromatograms；
Fig. 3 is 300 μ g/LP- coumaric acid standard items chromatograms；
Fig. 4 is 300 μ g/L vanillic acid standard items chromatograms；
Fig. 5 is 300 μ g/L gallic acid standard items chromatograms；
Fig. 6 is 300 μ g/L caffeic acid standard items chromatograms；
Fig. 7 is 300 μ g/L ferulic acid standard items chromatograms；
Fig. 8 is 300 μ g/L syringic acid standard items chromatograms；
Fig. 9 is 300 μ g/L sinapic acid standard items chromatograms；
Figure 10 is 1 protocatechuic acid chromatogram of sample；
Figure 11 is 4-HBA chromatogram in sample 1；
Figure 12 is P- coumaric acid chromatograms in sample 1；
Figure 13 is vanillic acid chromatogram in sample 1；
Figure 14 is gallic acid chromatogram in sample 1；
Figure 15 is caffeic acid chromatogram in sample 1；
Figure 16 is ferulic acid chromatogram in sample 1；
Figure 17 is syringic acid chromatogram in sample 1；
Figure 18 is sinapic acid chromatogram in sample 1；
Figure 19 is 2 protocatechuic acid chromatogram of sample；
Figure 20 is 4-HBA chromatogram in sample 2；
Figure 21 is P- coumaric acid chromatograms in sample 2；
Figure 22 is vanillic acid chromatogram in sample 2；
Figure 23 is gallic acid chromatogram in sample 2；
Figure 24 is caffeic acid chromatogram in sample 2；
Figure 25 is ferulic acid chromatogram in sample 2；
Figure 26 is syringic acid chromatogram in sample 2；
Figure 27 is sinapic acid chromatogram in sample 2.
Specific embodiment
High performance liquid chromatography tandem mass spectrum used in embodiment is beautiful for Japan's Shimadzu 20ADXR liquid chromatographic systems series connection
State's AB6500 mass spectrums.
Phenolic acid in embodiment is bought from sigma companies.
Embodiment 1 establishes standard curve
The preparation of phenolic acid standard reserving solution：Weigh gallic acid, protocatechuic acid, 4-HBA, vanillic acid, coffee
Acid, syringic acid, coumaric acid, ferulic acid, each 5mg of sinapic acid standard items, respectively with the mixed liquor of methanol and water (volume ratio 1:1) it is molten
It solves and in constant volume to 10mL volumetric flasks, the concentration of 9 kinds of phenolic acid is 0.5mg/mL.Then respectively with 50% methanol (volume ratio)
Be configured to 0.2,0.3,6,24,100, the phenolic acid standard solution of 200mg/L.Carry out high performance liquid chromatography tandem mass spectrum inspection respectively again
It surveys.
Specifically high performance liquid chromatography tandem mass spectrum detection method is：
Chromatographic column is Agilent XDB-C18-2014-3.5 μm -2.1*150mm；2 μ L of sample size；Column temperature：40℃；Flowing
Phase A：Water containing 1% (volume ratio) formic acid；Mobile phase B:Acetonitrile containing 1% (volume ratio) formic acid；Elution time 0-5min, initially
Mobile phase A is from 90% to 60%, and Mobile phase B is from 10% to 40%；Elution time 5-12min, mobile phase A from 60% to 10%,
Mobile phase B is from 40% to 90%；Elution time 12-15min, mobile phase A is from 10% to 90%, and Mobile phase B is from 90% to 10%；
Single sample run time is 15min in total；
Tandem mass spectrum testing conditions are：
Ionization mode is electron spray ionisation negative ion mode (ESI-)；Multiple-reaction monitoring (MRM)；Ion source temperature 500
℃；Residence time 100ms；Atomization air pressure 50psi；Assist gas pressure 50psi；Spray voltage -4500V, collision cell project voltage 6V,
Phenolic acid Mass Spectrometry Conditions parameter such as table 1.
The Mass Spectrometry Conditions parameter of 1. phenolic acid of table
Note：* quota ion
The standard curve, detection limit and quantitative limit for detecting gained are as shown in table 2, and the chromatogram of various phenolic acid standard items is as schemed
1- Fig. 9 (protocatechuic acid, 4-HBA, P- coumaric acids, vanillic acid, gallic acid, caffeic acid, ferulic acid, syringic acid, mustard
The chromatogram of sub- acid is successively such as Fig. 1-Fig. 9) shown in：
Linear equation, detection limit and the quantitative limit of 2 phenolic acid of table
Standard curve is established, in the corresponding range of linearity, 9 kinds of phenolic acid are linear good in wheat matrix, phase relation
Number R2≥0.99。
Sensitivity：By standard solution 50% methanol (volume ratio) gradient dilution, the sensitivity of assay method, method is determined
It measures as 0.2 μ g/mL, detection is limited to 0.1 μ g/mL.(quantitative limit：Signal-to-noise ratio corresponds to target concentration when being equal to 10；Detection limit：Letter
Target concentration is corresponded to when making an uproar than being equal to 3).
Precision：A sample cleanup liquid is taken, continuous sample introduction 6 times in 1 day, the withinday precision mark of 9 kinds of phenolic acid of calculating
Quasi- deviation (RSD), continuously does 3 days, and the day to day precision standard deviation (RSD) for calculating 9 kinds of phenolic acid is shown in Table 3
Stability：A sample cleanup liquid is taken, per testing at regular intervals sample, calculates 9 kinds of phenol in sample
The content of acid calculates RSD, is shown in Table 3.
Repeatability：It repeats to prepare same batch sample 6 times by identical method, calculates the content of 9 kinds of phenolic acid in sample, calculate
Go out RSD, be shown in Table 3.
The rate of recovery：The rate of recovery of method is investigated using matrix mark-on method, high, medium and low three concentration (0.2,0.4,
2 μ g/mL) 3 parallel additions, phenolic content is measured, the rate of recovery and RSD is calculated, is shown in Table 3.
Precision, repeatability, stability and the rate of recovery of 3 phenolic acid of table
2 sample detection of embodiment
1st, wheat samples are taken, carry out analysis detection by following operating process respectively.
(1) take wheat samples, pulverizer be crushed to can be completely by 0.425mm sieve pores until, be placed in -20 DEG C of refrigerators and protect
It deposits for use.
(2) sample is taken out and restored to room temperature, accurately weigh 2.00g sample powders in 250mL triangular flasks, added in
The NaOH of 40mL2mol/L seals up rapidly bottleneck after being quickly filled with nitrogen, and oscillation (2500rpm) hydrolysis is protected from light under the conditions of 25 DEG C
2h adjusts hydrolyzate pH value between 1.5-2.0 after hydrolysis using 1mol/L hydrochloric acid.The step for purpose be to allow sample
Middle reference state phenolic acid is hydrolyzed into free state, is discharged into hydrolyzate, and hydrolyzate is tuned into acidity with hydrochloric acid, is had in acid condition
Conducive to the extraction of phenolic acid.
(3) it accurately measures 50mL ethyl acetate and is sufficiently mixed 10min with hydrolyzate, then in 10000rpm, 4 DEG C of condition
Lower centrifugation 5min, takes upper strata ethyl acetate layer；The step for purpose be that phenolic acid is allowed adequately to be dissolved in ethyl acetate, (phenol
Distribution coefficient of the acid in ethyl acetate is more than distribution coefficient in sodium hydroxide) a large amount of impurity in removal sample.
(4) it repeats (3) operation and three times, merges all ethyl acetate layers rotary evaporated to dryness under the conditions of 40 DEG C,
(5) rotation is evaporated rear residue 10mL50% methanol (volume ratio 1:1) aqueous solution weight is molten, after crossing 0.22 μm of filter membrane
4 DEG C of preservations are to be measured；
2nd, liquid chromatography mass the Series detectors, (chromatogram of sample 1 are carried out to the sample cleanup liquid obtained in the present embodiment
Such as Figure 10-Figure 18 (protocatechuic acid, 4-HBA, P- coumaric acids, vanillic acid, gallic acid, caffeic acid, ferulic acid, cloves
Sour, sinapic acid chromatogram is respectively such as Figure 10-Figure 18) shown in, chromatogram such as Figure 19-Figure 27 (protocatechuic acid, the 4- hydroxyls of sample 2
Yl benzoic acid, P- coumaric acids, vanillic acid, gallic acid, caffeic acid, ferulic acid, syringic acid, sinapic acid chromatogram respectively as scheme
19- Figure 27) shown in, then the standard curve that obtains of testing result substitution embodiment 1 is compared, sample is calculated with quantified by external standard method
The concentration of phenolic acid in product calculates the content of phenolic acid in sample according to formula (1).
In formula：
X --- the content of component to be measured in sample, unit for milligrams per kilogram, mg/kg；
C --- the concentration of component to be measured in liquid is measured, unit is micrograms per millilitre, μ g/mL；
V --- constant volume, unit are milliliter, mL；
M --- sample sample weighting amount, unit for gram, g.
The testing result of phenolic acid is shown in Table 4 in different samples.
Phenolic acid testing result in the different samples of table 4
The entire detection process of the present embodiment takes 15 minutes 2 hours, and including hydrolysis 2 hours, instrument detected 15 minutes.
At present, there are no the bioassay standard of phenolic acid a variety of in wheat, NY/T2012-2011 defines fruit and product middle reaches
Liquid chromatogram measuring method from phenolic content, the assay method time is long, and efficiency is low, and propolis is defined in GB/T23196-2008
Liquid chromatogram-uv detection method of middle ferulaic acid content.Equally, the assay method time is long, and efficiency is low.This method can be surveyed simultaneously
Determine 9 kinds of phenolic acid in wheat, extracting method is quick and easy, takes short, high sensitivity, is applicable to the quantitative inspection of batch samples
It surveys.The foundation of this method enables the accurate quick measure of the phenolic acid in wheat, can assess and is provided accurately for agricultural product trophic function
Analysis method.
Protection scope of the present invention is not limited to the description made in embodiment, without departing from the modification at the present invention program center
Belong to protection scope of the present invention.
Claims (4)
1. the high performance liquid chromatography tandem mass spectrum detection method of phenolic acid in a kind of wheat being simple and efficient, which is characterized in that specific
Step is as follows：
(1) sample extraction：It accurately weighs wheat samples powder to be dissolved in the NaOH solution of 2mol/L, be sealed after being filled with nitrogen, 25
Oscillation hydrolysis 2h is protected from light under the conditions of DEG C, then adjusts hydrolyzate pH value between 1.5-2.0, it is spare as sample to be tested；
Wherein, wheat samples powder and the mass volume ratio of NaOH solution are 20:1；
(2) to take concentration be respectively 0.2,0.3,6,24,100, the gallic acid of 200mg/L, protocatechuic acid, 4-HBA,
Vanillic acid, caffeic acid, syringic acid, P- coumaric acids, ferulic acid, sinapic acid standard solution, respectively carry out high performance liquid chromatography string
Join Mass Spectrometer Method, establish phenolic acid standard curve；
(3) high performance liquid chromatography tandem mass spectrum detection is carried out to the sample to be tested that step (1) obtains, testing result substitutes into step
(2) standard curve obtained is compared, and the concentration of each phenolic acid in sample is calculated with quantified by external standard method, then count according to formula (1)
Calculate the content of phenolic acid in sample；
In formula：
X --- the content of component to be measured in sample, unit for milligrams per kilogram, mg/kg；
C --- the concentration of component to be measured in liquid is measured, unit is micrograms per millilitre, μ g/mL；
V --- constant volume, unit are milliliter, mL；
M --- sample sample weighting amount, unit for gram, g.
2. the high performance liquid chromatography tandem mass spectrum detection method of phenolic acid in the wheat being simple and efficient according to claim 1,
It is characterized in that step (2) and step (3) the high performance liquid chromatography tandem mass spectrum detection refer to：
1) chromatographic condition：
A) chromatographic column：Agilent XDB-C18-2014-3.5μm-2.1*150mm；
B) sample size：2μL
C) column temperature：40℃
D) flow velocity：0.5mL/min
E) mobile phase and elution time：
Mobile phase A：Aqueous solution containing 1% formic acid；
Mobile phase B:Acetonitrile containing 1% formic acid；
Using linear gradient elution：
0-5min, mobile phase A are reduced to 60% by 90%；Mobile phase B is from 10% to 40%；
5-12min, mobile phase A are reduced to 10% from 60%；Mobile phase B is from 40% to 90%；
12-15min, mobile phase A rise to 90% from 10%；Mobile phase B is from 90% to 10%；
Single sample run time is 15min altogether；
2) Mass Spectrometry Conditions：
Ionization mode is electron spray ionisation negative ion mode；Multiple-reaction monitoring；500 DEG C of ion source temperature；Residence time
100ms；Atomization air pressure 50psi；Assist gas pressure 50psi；Spray voltage -4500V, collision cell project voltage 6V.
3. the high performance liquid chromatography tandem mass spectrum detection method of phenolic acid in the wheat being simple and efficient according to claim 2,
It is characterized in that, step (1) the wheat samples powder referred to the wheat samples powder after 0.425mm hole sizers.
4. the high performance liquid chromatography tandem mass spectrum detection method of phenolic acid in the wheat being simple and efficient according to claim 3,
It is characterized in that, step (1) the hydrolyzate pH value that adjusts refers between 1.5-2.0：Water is adjusted with the hydrochloric acid solution of 1mol/L
Liquid pH value is solved between 1.5-2.0.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108982703A (en) * | 2018-08-23 | 2018-12-11 | 中国检验检疫科学研究院 | A kind of LC-MS detection method of polyphenols |
| CN109459507A (en) * | 2018-10-24 | 2019-03-12 | 重庆第二师范学院 | The measuring method of phenolic acid compound in one vegetable oil |
| CN113075347A (en) * | 2021-04-01 | 2021-07-06 | 广东省农业科学院农业生物基因研究中心 | High performance liquid chromatography-triple quadrupole mass spectrometry combined method for rapidly detecting polyphenol |
| CN115128205A (en) * | 2022-08-31 | 2022-09-30 | 中国农业科学院农产品加工研究所 | Method for detecting content of phenolic substances in highland barley |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458948A (en) * | 2014-12-05 | 2015-03-25 | 江苏省农业科学院 | Detection method of straw phenolic acid compound |
| CN106153800A (en) * | 2016-06-22 | 2016-11-23 | 中国农业科学院生物技术研究所 | The HPLC MS/MS detection method of transgenic corns secondary metabolites |
| CN107132291A (en) * | 2017-05-22 | 2017-09-05 | 河北中医学院 | A kind of ultra high efficiency liquid chromatography mass spectrometric combination determines the quantitative approach of 10 kinds of compositions in evodia rutaecarpa granule |
-
2017
- 2017-12-19 CN CN201711375184.XA patent/CN108195957A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458948A (en) * | 2014-12-05 | 2015-03-25 | 江苏省农业科学院 | Detection method of straw phenolic acid compound |
| CN106153800A (en) * | 2016-06-22 | 2016-11-23 | 中国农业科学院生物技术研究所 | The HPLC MS/MS detection method of transgenic corns secondary metabolites |
| CN107132291A (en) * | 2017-05-22 | 2017-09-05 | 河北中医学院 | A kind of ultra high efficiency liquid chromatography mass spectrometric combination determines the quantitative approach of 10 kinds of compositions in evodia rutaecarpa granule |
Non-Patent Citations (6)
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108982703A (en) * | 2018-08-23 | 2018-12-11 | 中国检验检疫科学研究院 | A kind of LC-MS detection method of polyphenols |
| CN108982703B (en) * | 2018-08-23 | 2021-05-14 | 中国检验检疫科学研究院 | Liquid chromatography-mass spectrometry detection method for polyphenol substances |
| CN109459507A (en) * | 2018-10-24 | 2019-03-12 | 重庆第二师范学院 | The measuring method of phenolic acid compound in one vegetable oil |
| CN113075347A (en) * | 2021-04-01 | 2021-07-06 | 广东省农业科学院农业生物基因研究中心 | High performance liquid chromatography-triple quadrupole mass spectrometry combined method for rapidly detecting polyphenol |
| CN115128205A (en) * | 2022-08-31 | 2022-09-30 | 中国农业科学院农产品加工研究所 | Method for detecting content of phenolic substances in highland barley |
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