CN110455953A - A method of quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously - Google Patents
A method of quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously Download PDFInfo
- Publication number
- CN110455953A CN110455953A CN201910776484.1A CN201910776484A CN110455953A CN 110455953 A CN110455953 A CN 110455953A CN 201910776484 A CN201910776484 A CN 201910776484A CN 110455953 A CN110455953 A CN 110455953A
- Authority
- CN
- China
- Prior art keywords
- acid
- sample
- benzoic acid
- phenyllactic
- sorbic acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/047—Standards external
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a kind of method for quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously, the method is realized in C18It is quickly detected from phenyllactic acid, benzoic acid and sorbic acid simultaneously on column, under the chromatographic condition of optimization, realizes and completes separation detection in 11min, and sample quality concentration has good linear relationship, R within the scope of 0.25-50mg/L2>0.998.The detection limit of this method is between 0.01-0.05mg/L, and for quantitative limit between 0.025-0.25mg/L, the rate of recovery reaches 96.93-118.42%, precision 0.93%-6.21%.The method rate of recovery with higher and preferable precision are fully able to meet the analysis detection of phenyllactic acid, benzoic acid, sorbic acid in daily fermented food.And this method is without complicated sample pre-treatments.
Description
Technical field
The invention belongs to field of food detection, and in particular to a kind of quickly to detect phenyllactic acid, benzoic acid and sorb simultaneously
The method of acid.
Background technique
In food production, for the shelf-life for extending food, it is anti-that some food are often added in process
Rotten agent.Benzoic acid and sorbic acid are most common artificial synthesized food preservatives, but excessively edible benzoic acid and sorbic acid can shadows
Absorption of the human body to vitamin and calcium is rung, human liver's burden is aggravated, and toxication is caused to react or induce cancer.Therefore country's mark
Quasi- para Toluic Acid, the use scope of sorbic acid and limitation have done strict regulations.
In addition to artificial synthesized food preservative, contain antibacterial in certain plants, animal, microorganism itself or its metabolin
Corrosion-resistant substance-natural antiseptic agent.The phenyllactic acid (PLA) being found for the first time for 1998 is a kind of fungicide, natural of wide spectrum
New food preservative can effectively prevent food spoilage, and have very strong antibacterial work to a variety of food-borne pathogens
With.Phenyllactic acid can be generated by lactic acid bacteria by fermenting raw materials of phenylalanine, and phenylalanine is as a kind of common amino acid, extensively
It is general to be formed in the bodies of aminal and plant, therefore be likely to by the food that zymotechnique produces containing phenyllactic acid.There are researcher's discovery, phenyllactic acid
With preservative synergy, the additive amount of artificial preservative in food can be effectively reduced.In the following natural antiseptic agent
Other compound artificial preservatives of phenyllactic acid use the trend that may become a kind of food antiseptic.
Currently, reported benzoic acid, sorbic acid detection method mainly have chromatography and spectroscopic methodology, such as gas chromatography
(GC), capillary electrophoresis (CE), high performance liquid chromatography (HPLC), Liquid Chromatography-Mass Spectrometry (LC-MS), liquid phase color
Spectrum-triple quadrupole bar mass spectrography (LC-MS/MS), time-of-flight mass spectrometry method (LC-TOF/MS) and Surface enhanced Raman spectroscopy method
(SERS) etc..But above detection method detects new food preservative both for the detection of Common Preservatives --- benzene cream
Acid and other food preservatives are not reported also.Therefore it establishes and a kind of quickly while detecting phenyllactic acid, benzoic acid, sorbic acid
Method is necessary.
This research is intended to establish a kind of while detecting natural antiseptic agent phenyllactic acid and artificial preservative in fermented food
The analysis method of the simple, fast high performance liquid chromatography of benzoic acid, sorbic acid, and this method is applied into a variety of fermented foods and is examined
It surveys, establishes the Fundamental database of phenyllactic acid in fermented food.
Summary of the invention
Present invention aims at establish a kind of while detecting in fermented food natural antiseptic agent phenyllactic acid and artificial synthesized prevent
The analysis method of rotten agent benzoic acid, the simple, fast high performance liquid chromatography of sorbic acid.
The present invention the specific technical proposal is:
1, a kind of method for quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously, described method includes following steps:
1) it prepares mixed standard solution: weighing the standard items of phenyllactic acid, benzoic acid, sorbic acid respectively, be configured to have dense
Spend the hybrid standard liquid of gradient；
2) testing sample solution is prepared:
Sample containing protein weighs 2.5g sample in 25mL colorimetric cylinder, is separately added into 0.25mol/L ferrocyanide
Potassium solution and each 1mL of 0.5mol/L acetic acid zinc solution shake 2min with 10% methanol-water solution constant volume, mix, take 10mL molten
Liquid 4000rpm is centrifuged 5min, and taking supernatant liquor to cross 0.22um polyethersulfone membranes, to obtain filtrate spare；
Nonprotein sample: weighing 2.5g sample in 25mL colorimetric cylinder, is settled to 10mL with 10% methanol-water,
Be vortexed concussion 2min, mixes, taking supernatant liquor to cross 0.22um polyethersulfone membranes, to obtain filtrate spare；
3) detecting instrument and testing conditions:
Instrument: high performance liquid chromatograph；Detector: UV detector；Chromatographic column: C18Column, mobile phase: 0.02mol/L acetic acid
80:20 is mixed by volume for ammonium and methanol；Flow velocity: 1mL/min；Sample volume: 20 μ L；Input mode: full ring sample introduction；Detection
Wavelength: 220nm；Chromatogram column temperature: 25 DEG C；
4) standard curve is drawn:
In the serial mixed standard solution injection high performance liquid chromatograph that step 1) is prepared, in the chromatographic condition of step 3)
Under eluted and detected, it is qualitative with retention time, according to the corresponding relationship of the size of the surveyed peak area of each concentration and its concentration
Draw standard curve, and evaluation criteria curve linear degree；
5) sample to be tested detects:
It takes testing sample solution in step 2) to inject in high performance liquid chromatograph, is examined under the chromatographic condition of step 3)
It surveys, measures the peak area of each object in filtrate, it is qualitative with retention time, it is quantitative according to 4) the middle standard curve made, it calculates
Out in sample to be tested phenyllactic acid, benzoic acid, sorbic acid content.
Preferably, retarder thinner used in the step 1) mixed standard solution is distilled water.
Preferably, phenyllactic acid, benzoic acid, sorbic acid concn are in 2mg/L respectively in the step 1) mixed standard solution,
The gradient series of 5mg/L, 10mg/L, 20mg/L, 30mg/L, 40mg/L, 50mg/L.
Preferably, the step 3) C18The specification of chromatographic column is 250mm × 4.6mm internal diameter, and grain diameter is 5 μm.
Preferably, regulating step 3) pH of 0.02mol/L ammonium acetate is 6.44 in the mobile phase, the methanol is content
Chromatographically pure greater than 99.8%.
Preferably, accuracy in detection, precision and the rate of recovery are verified by the following method: mixed standard solution is constantly dilute
It releases to signal-to-noise ratio S/N=3, using this sample introduction concentration as detection limit (LOD), using the corresponding concentration of 10 times of signal-to-noise ratio as lower limit of quantitation
(LOQ).Recovery testu is done with primary vinegar, the accuracy of method is investigated by calculating the rate of recovery, with the opposite mark of the rate of recovery
Quasi- deviation (RSD) investigates the precision of method, and mixed standard solution is added in primary vinegar sample, and mark-on level is respectively 5,
10,20mg/L, each pitch-based sphere is measured in parallel 6 times, and calculates recovery of standard addition with following formula；
Wherein, Csm indicates mark-on detected value；Cm indicates sample detection value；Cs indicates spiked levels.
Preferably, this method benzoic acid range of linearity is 0.01-50mg/L, phenyllactic acid 0.075-50mg/L, sorbic acid
For 0.05-50mg/L, and linear dependence is all larger than 0.998, and 0.01 between 0.05mg/L, quantitative limit exists detection limit
0.025 between 0.25mg/L.
The beneficial effects of the invention are that: detection method disclosed by the invention is realized in C18It is quickly detected from simultaneously on column
Phenyllactic acid, benzoic acid and sorbic acid are realized under the chromatographic condition of optimization and complete separation detection in 11min, and mass concentration
There is good linear relationship, R within the scope of 0.25-50mg/L2>0.998.The detection limit of this method is in 0.01-0.05mg/L
Between, for quantitative limit between 0.025-0.25mg/L, the rate of recovery reaches 96.93-118.42%, precision 0.93%-
6.21%.Show that this method has the higher rate of recovery and preferable precision, is fully able to meet benzene cream in daily fermented food
The analysis detection of acid, benzoic acid, sorbic acid.And this method is without complicated sample pre-treatments.
Figure of description
Fig. 1 is the uv atlas of phenyllactic acid, benzoic acid, sorbic acid under the conditions of different wave length；
Fig. 2 is the chromatography of phenyllactic acid, benzoic acid, sorbic acid in 20mg/L hybrid standard liquid under the conditions of different mobile phases
Elution curve.
Specific embodiment
Technical solution of the present invention is described further below in conjunction with Figure of description and specific embodiment:
Chromatographic column used in following embodiment uses SapphiresilTM C18Column (5 μm of partial sizes, 4.6mm i.d ×
250mm), detector is UV detector.
Prepare mixed standard solution:
The standard items for weighing phenyllactic acid, benzoic acid, sorbic acid respectively are configured to the hybrid standard liquid with concentration gradient；
Phenyllactic acid, benzoic acid, sorbic acid concn are in 2mg/L, 5mg/L, 10mg/L, 20mg/L respectively in the mixed standard solution,
The gradient series of 30mg/L, 40mg/L, 50mg/L are spare.
It enumerates a kind of specific preparation method of mixed solution: taking 100mg/L phenyllactic acid 0.1mL, 100mg/L benzoic acid respectively
0.1mL, 100mg/L sorbic acid acid 0.1mL are added 0.7mL distilled water, are configured to 10mg/L hybrid standard in 2mL centrifuge tube
Solution.
Sample pre-treatments:
1) containing the sample of protein
2.5g sample is accurately weighed in 25mL colorimetric cylinder, is separately added into 0.25M potassium ferrocyanide solution and 0.5M acetic acid
Each 1mL of zinc solution shakes 2min with 10% methanol-water constant volume, mixes, and takes 10mL solution 4000rpm to be centrifuged 5min, takes upper layer
Clear liquid crosses 0.22um polyethersulfone membranes, to upper machine.
2) other samples
2.5g sample is accurately weighed in 25mL colorimetric cylinder, is settled to 10mL with 10% methanol-water, be vortexed concussion 2min,
It mixes, takes supernatant liquor to cross 0.22um polyethersulfone membranes, to upper machine.
The optimization of chromatographic condition
1) Detection wavelength is determined
Use the mixed solution of 0.01g/L benzoic acid, 0.01g/L sorbic acid, 0.8g/L phenyllactic acid in different detections respectively
It is detected under wavelength, Fig. 1 is the UV absorption spectrogram of phenyllactic acid, benzoic acid, sorbic acid.As can be seen from the figure component to be measured
There is UV absorption, and the maximum absorption wavelength of each component is different, but three kinds of preservatives have relatively strong ultraviolet suction at 220nm
It receives, is the detection sensitivity of balanced three kinds of preservatives, therefore select 220nm as Detection wavelength.
2) mobile phase is determined
Using the hybrid standard liquid of 20mg/L as experimental subjects, different mobile phases are investigated to phenyllactic acid, benzoic acid, sorbic acid
The influence of separating effect makees mobile phase with phosphate-methanol, trifluoroacetic acid-methanol, and three kinds of preservative separation are incomplete；With
0.02mol/L ammonium acetate-methanol is as mobile phase, and by optimizing, ammonium acetate pH is 6.44 and the volume proportion of two-phase is 80:20
When, phenyllactic acid, benzoic acid, sorbic acid obtain preferable separating degree and obtain suitable retention time and preferable peak shape,
As shown in Figure 2.
3) flow velocity is determined
The influence that research flow rate of mobile phase separates three kinds of preservatives, it is found that the flow velocity of 1.0mL/min is suitably to separate
Speed.In contrast, the elution rate of compound to be separated can be accelerated by flow velocity being increased to 1.2mL/min, but pressure can connect
Nearly alarming value；And after flow velocity is reduced to 0.5mL/min, better separation parameter can be obtained, but analyze long operational time, no
It is able to achieve quick separating.Therefore the flow velocity of 1.0mL/min is selected to carry out subsequent experimental.
4) chromatography box temperature degree is determined
Investigate 22 DEG C, 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C respectively as chromatograph box temperature to separating effect and retention time
Influence.With the raising of chromatogram column temperature, three kinds of preservative object retention times move forward.But 22 DEG C subtract with 40 DEG C of retention times
When young in 2min, at the same consider energy consumption the problem of, therefore select 25 DEG C as best chromatograph box temperature.
5) filter membrane is determined
Investigate the influence of suction-operated of the different filter membranes to phenyllactic acid, benzoic acid, sorbic acid.With the mixed sample of 10mg/L
As liquid to be filtered, using machine testing upper after different types of membrane filtration, testing result is shown in Table 1.The above results show that using
Poly (ether sulfone) film filtering mixed sample concentration detectable concentration and there is no the original liquid concentration of film more closely, 0.22um nylon filter
Film has humidification to phenyllactic acid, benzoic acid, sorbic acid etc., and reason is that extractant has stripping to nylon leaching film.Therefore
Select filter membrane of the polyethersulfone membranes as sample filtering.
The testing result of the different filter membranes of table 1
Method validation
Under chromatographic condition determined above, using phenyllactic acid, benzoic acid, sorbic acid concentration as horizontal axis (X), peak area is
The longitudinal axis (Y) prepares 2,5,10,20,30,40,50mg/L mixed standard solution and draws standard curve, thus appraisal procedure
The linearity.Mixed standard solution is constantly diluted to signal-to-noise ratio S/N=3, using this sample introduction concentration as detection limit (LOD), with 10 times
The corresponding concentration of signal-to-noise ratio is lower limit of quantitation (LOQ).It is verified by above method, obtains the range of linearity as shown in Table 2, correlation
Coefficient, regression equation, detection limit, quantitative limit:
2 range of linearity of table, related coefficient, regression equation, detection limit, quantitative limit
It is shown by table 2, by the optimization of testing conditions, this method benzoic acid range of linearity is 0.01-50mg/L, phenyllactic acid
For 0.075-50mg/L, sorbic acid 0.05-50mg/L, and linear dependence is all larger than 0.998, detection limit 0.01 to
Between 0.05mg/L, for quantitative limit 0.025 between 0.25mg/L, this method realizes the sensitive inspection for providing and having the wide range of linearity
It surveys.
The test of sample mark-on reclaims
Recovery testu is done with primary vinegar, investigates the accuracy of method, by calculating the rate of recovery with the opposite of the rate of recovery
The precision of standard deviation (RSD) investigation method.Mixed standard solution is added in primary vinegar sample, mark-on level is respectively 5,
10,20mg/L, each pitch-based sphere is measured in parallel 6 times, and calculates recovery of standard addition with following formula.
Wherein, Csm indicates mark-on detected value；Cm indicates sample detection value；Cs indicates spiked levels.
This research is chosen certain primary vinegar and is tested as mark-on reclaims.Respectively into sample be added 5,10,20mg/L difference it is dense
The phenyllactic acid of degree, benzoic acid, sorbic acid mixed sample, mix, its rate of recovery measured after sample pre-treatments.Each addition
Horizontal parallel measures 6 times, and the result is shown in shown in table 3.
3 recovery of standard addition of table (n=6)
Show that this method rate of recovery reaches 96.93-118.42% by table 3, precision reaches 0.93%-6.21%.Show
This method has the higher rate of recovery and preferable precision.
The detection of actual sample
Sample using the method established above to purchase from Yong Hui supermarket and Jingdone district detects, and testing result is shown in Table
4.Most of as can be seen from Table 4, numerous food product is free of any additive there is no as promising to undertake production firm,
All contain different degrees of preservative in such food.According to the GB7718-94 food labelling universal standard, there is inspection in sample
Not the case where not being inconsistent out with sample label (2-3,5,11-17, No. 19), but the relevant criterion for comparing national food additive finds benzene
Formic acid and sorbic acid detection value are less than addition limit (1g/kg)." three are not added " is all write on 11 to No. 16 sample labels, still
11-14 sample has benzoic acid, sorbic acid detection, and 15-16 sample has benzoic acid detection, and 11, examines in 14, No. 15 samples
Concentration of benzoic acid out is higher.And 4,6, No. 18 samples are consistent with label.
The testing result of 4 actual sample of table
ND --- it is not detected
Indicated above, the present invention establishes HPLC-UV and quickly detects phenyllactic acid in food, benzoic acid, sorbic acid, with analysis
Standard items are corresponding with the retention time of sample qualitative.Under the chromatographic condition of optimization, three kinds of preservatives are completed within 11 minutes
Separation detection, detection limit is between 0.01-0.05mg/L, and quantitative limit is between 0.025-0.25mg/L, rate of recovery 96.93-
118.42mg/L precision 0.93%-6.21%.And advantage of the invention is that sample pre-treatments are simple, without complexity
Sample pre-treatments.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to reality
Example is applied to describe the invention in detail, those skilled in the art should understand that, it can be to technical side of the invention
Case is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered in the present invention
Scope of the claims in.
Claims (7)
1. a kind of method for quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously, which is characterized in that the method includes such as
Lower step:
1) it prepares mixed standard solution: weighing the standard items of phenyllactic acid, benzoic acid, sorbic acid respectively, be configured to concentration ladder
The hybrid standard liquid of degree；
2) testing sample solution is prepared:
Sample containing protein weighs 2.5g sample in 25mL colorimetric cylinder, it is molten to be separately added into 0.25mol/L potassium ferrocyanide
Liquid and each 1mL of 0.5mol/L acetic acid zinc solution shake 2min with 10% methanol-water solution constant volume, mix, take 10mL solution
4000rpm is centrifuged 5min, and taking supernatant liquor to cross 0.22um polyethersulfone membranes, to obtain filtrate spare；
Nonprotein sample: weighing 2.5g sample in 25mL colorimetric cylinder, is settled to 10mL with 10% methanol-water, is vortexed
2min is shaken, is mixed, taking supernatant liquor to cross 0.22um polyethersulfone membranes, to obtain filtrate spare；
3) detecting instrument and testing conditions:
Instrument: high performance liquid chromatograph；Detector: UV detector；Chromatographic column: C18 column, mobile phase: 0.02mol/L ammonium acetate and
80:20 is mixed methanol by volume；Flow velocity: 1mL/min；Sample volume: 20 μ L；Detection wavelength: 220nm；Chromatogram column temperature:
25℃；
4) standard curve is drawn:
In the serial mixed standard solution injection high performance liquid chromatograph that step 1) is prepared, under the chromatographic condition of step (3)
It is eluted and is detected, it is qualitative with retention time, it is drawn according to the corresponding relationship of the size and its concentration of the surveyed peak area of each concentration
Standard curve processed, and evaluation criteria curve linear degree；
5) sample to be tested detects:
It takes testing sample solution in step 2) to inject in high performance liquid chromatograph, is detected under the chromatographic condition of step 3),
Measure the peak area of each object in filtrate, it is qualitative with retention time, it is quantitative according to the standard curve made in 4), calculate to
The content of phenyllactic acid, benzoic acid, sorbic acid in sample.
2. a kind of method for quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously, feature exist according to claim 1
In retarder thinner used in the step 1) mixed standard solution is distilled water.
3. a kind of method for quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously, feature exist according to claim 1
In, phenyllactic acid, benzoic acid, sorbic acid concn are in 2mg/L, 5mg/L, 10mg/L respectively in the step 1) mixed standard solution,
The gradient series of 20mg/L, 30mg/L, 40mg/L, 50mg/L.
4. a kind of method for quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously, feature exist according to claim 1
In the step 3) C18The specification of chromatographic column is 250mm × 4.6mm internal diameter, and grain diameter is 5 μm.
5. a kind of method for quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously, feature exist according to claim 1
In regulating step 3) pH of 0.02mol/L ammonium acetate is 6.44 in the mobile phase, the methanol is content greater than 99.8%
Chromatographically pure.
6. a kind of method for quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously, feature exist according to claim 1
In verifying accuracy in detection, precision and the rate of recovery by the following method: mixed standard solution be constantly diluted to signal-to-noise ratio S/
N=3, using this sample introduction concentration as detection limit (LOD), using the corresponding concentration of 10 times of signal-to-noise ratio as lower limit of quantitation (LOQ)；With primary vinegar
Recovery testu is done, the accuracy of method is investigated by calculating the rate of recovery, is investigated with the relative standard deviation (RSD) of the rate of recovery
The precision of method, adds mixed standard solution in primary vinegar sample, and mark-on level is respectively 5,10,20mg/L, Mei Getian
Add horizontal parallel to measure 6 times, and calculates recovery of standard addition with following formula；
Wherein, Csm indicates mark-on detected value；Cm indicates sample detection value；Cs indicates spiked levels.
7. a kind of method for quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously, feature exist according to claim 1
In this method benzoic acid range of linearity is 0.01-50mg/L, phenyllactic acid 0.075-50mg/L, sorbic acid 0.05-50mg/
L, and linear dependence is all larger than 0.998, detection limit is 0.01 between 0.05mg/L, and quantitative limit is 0.025 to 0.25mg/L
Between.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910776484.1A CN110455953A (en) | 2019-08-22 | 2019-08-22 | A method of quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910776484.1A CN110455953A (en) | 2019-08-22 | 2019-08-22 | A method of quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110455953A true CN110455953A (en) | 2019-11-15 |
Family
ID=68488381
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910776484.1A Pending CN110455953A (en) | 2019-08-22 | 2019-08-22 | A method of quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110455953A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112945930A (en) * | 2021-02-03 | 2021-06-11 | 上海安谱实验科技股份有限公司 | Method for simultaneously and rapidly detecting benzoic acid and sorbic acid in skin care product |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831394A (en) * | 2010-02-05 | 2010-09-15 | 山东大学 | Heat-resistant bacillus and application thereof in preparing phenyl lactic acid |
| JP2015110543A (en) * | 2013-10-31 | 2015-06-18 | 東レ・ファインケミカル株式会社 | Benzoic acid production method |
-
2019
- 2019-08-22 CN CN201910776484.1A patent/CN110455953A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831394A (en) * | 2010-02-05 | 2010-09-15 | 山东大学 | Heat-resistant bacillus and application thereof in preparing phenyl lactic acid |
| JP2015110543A (en) * | 2013-10-31 | 2015-06-18 | 東レ・ファインケミカル株式会社 | Benzoic acid production method |
Non-Patent Citations (5)
| Title |
|---|
| 宁亚维 等: "苯乳酸与食品防腐剂联合抑菌效果", 《食品与机械》 * |
| 张世满: "HPLC法测定乳制品中苯甲酸、山梨酸、糖精钠方法研究", 《安徽预防医学杂志》 * |
| 张忠华 等: "乳酸菌发酵液中DL-3-苯乳酸高效液相色谱快速检测方法的建立", 《昆明理工大学学报(自然科学版)》 * |
| 郑梦林 等: "不同保鲜剂对冷鲜鸭肉中肠杆菌抑菌特性研究", 《食品科技》 * |
| 黄国昌 等: "高效液相色谱法检测发酵液中苯乳酸和苯丙氨酸含量的研究", 《江西科学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112945930A (en) * | 2021-02-03 | 2021-06-11 | 上海安谱实验科技股份有限公司 | Method for simultaneously and rapidly detecting benzoic acid and sorbic acid in skin care product |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107247093B (en) | The detection method for metanephrine substance of dissociating in urine | |
| CN102818865A (en) | Method for Analyzing Oligomeric Proanthocyanidin (OPC) | |
| CN113267588B (en) | Method for simultaneously detecting 7 acrylic acid and acrylic ester monomers in plastic product | |
| CN110618206B (en) | Method for simultaneously detecting benzoic acid, sorbic acid, saccharin sodium, phenyllactic acid and phenylalanine in fermented food | |
| CN107167532A (en) | A kind of method of food additives in use high performance liquid chromatography test food | |
| CN103336069A (en) | HPLC (High Performance Liquid Chromatography) determination method of phenolic compounds in peach fruit | |
| Liu et al. | Elimination of matrix effects for headspace solid-phase microextraction of important volatile compounds in red wine using a novel coating | |
| Siříšťová et al. | Changes in quality parameters of vodka filtered through activated charcoal. | |
| CN104535705B (en) | Method for synchronously measuring capsaicin and capsorubin in capsicum oleoresin | |
| CN110455953A (en) | A method of quickly detecting phenyllactic acid, benzoic acid and sorbic acid simultaneously | |
| CN109100456B (en) | Method for simultaneously determining content of 3 fat-soluble vitamins in multivitamin injection | |
| CN102507757A (en) | Method for measuring ascorbic acid content in porphyra yezoensis by high performance liquid chromatography | |
| CN110118836A (en) | The method of genetoxic impurity in high effective liquid chromatography for measuring razaxaban | |
| CN111579675A (en) | Method for detecting fat-soluble vitamins in feed | |
| CN106383181A (en) | Method for detection of valine content in fermentation broth by precolumn derivatization-high performance liquid chromatography | |
| CN110632209A (en) | Method for rapidly detecting phenolic acid compounds in raspberries | |
| Rao et al. | Detection of the adulteration of traditional alcoholic beverages by the separation and determination of alprazolam, chloralhydrate and diazepam using reversed-phase high-performance liquid chromatography | |
| CN110618230A (en) | Method for detecting dodecyl paraben | |
| CN110007012A (en) | The measuring method of DCP purity after a kind of improvement | |
| CN113777197B (en) | Method for simultaneously determining citrinin and 1-hydroxy-2-naphthoic acid | |
| CN111175392B (en) | Quality control method of cough-relieving loquat syrup | |
| CN102735774A (en) | Method for detecting content of oxalic acid in yellow millet wine by reversed-phase high-performance liquid chromatography | |
| CN115327003B (en) | Method for detecting clopidogrel oxide related substances | |
| CN113495109B (en) | Method for rapidly detecting benzoic acid or sodium benzoate in chemical synthesis reaction solution or mother solution | |
| CN113030329B (en) | One-test-multiple-evaluation method for determining content of 6 gingerol components in ginger juice brown sugar |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191115 |
|
| RJ01 | Rejection of invention patent application after publication |