CN110470759A - A kind of method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables - Google Patents
A kind of method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables Download PDFInfo
- Publication number
- CN110470759A CN110470759A CN201910756484.5A CN201910756484A CN110470759A CN 110470759 A CN110470759 A CN 110470759A CN 201910756484 A CN201910756484 A CN 201910756484A CN 110470759 A CN110470759 A CN 110470759A
- Authority
- CN
- China
- Prior art keywords
- ethephon
- chloroethyl
- cepha
- phosphonic acid
- residual quantity
- 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
Abstract
The invention discloses a kind of methods of ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables, comprising the following steps: step S1, is soaked in the sample to be tested being homogenized in ml headspace bottle by distilled water and potassium hydroxide solution；Step S2, ml headspace bottle is placed in constant temperature in automatic incubator, make to decomposite the ethylene come in water with reach balance in air；Step S3, it with nitrogen as carrier gas, is detected using the gas chromatograph with flame ionization ditector, determines the residual quantity of ethephon (CEPHA),2-(chloroethyl) phosphonic acid in fruits and vegetables.The advantages that method of the invention has sampling amount few, and detection time is short, easy to operate safe, reaction is mild, avoid using it is inflammable and explosive, there is the good irritating reagent of toxicity；Testing result of the invention is accurate, and ethephon (CEPHA),2-(chloroethyl) phosphonic acid detection is limited to 0.05mg/kg, can satisfy the requirement of water fruits and vegetables ethephon (CEPHA),2-(chloroethyl) phosphonic acid drug residue quantitative detection.
Description
Technical field
The present invention relates to a kind of sides of ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in the Detection Technologies of Pesticide Residues field more particularly to measurement fruits and vegetables
Method.
Background technique
As the China of developing country, agricultural is always the foundation leg that we depend on for existence, and pesticide is as farming
The solid guarantee of amount of substance, yield plays an important role.As China begins to use pesticide from generation 30 or 40 years in last century,
Residue problem after the applications of pesticide is also following.Although now pesticide be substantially low toxicity, easily decompose, low-residual dosage form and at
Point, but pesticide can play after use or to natural environment certain pollution, more especially because it is fresh-keeping, accelerate the ripening and other effects
Pesticide can directly contact on crops, due to improper use, the health of the mankind and livestock and poultry can be jeopardized, cause a series of companies
Continuous adverse consequences.
It is counted according to world's agrochemical net, newly-increased agriculture chemical registration 4515 in 2018 compared to 2017, increases by a year-on-year basis
15.38%.End on June 14th, 2019, China's formal registration product is 66 total, wherein sulfone pyrrole grass azoles, nitrile pyrrole mite ester, leaf bacterium
The ingredients such as azoles are domestic first official approval registration.Although China has the phases such as GB 2763-2016, GB 2763.1-2018
To complete food persticide residue standard, but due to the appearance that new product, novel form and frontier use, various pesticides are residual
The exceeded report of allowance, China still need the sanitary index for constantly improving oneself, further strengthen pesticide residue level
It detects very urgent.
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid (Ethrel) also known as ethephon, 2- chloroethyl phosphoric acid, molecular formula: C2H6ClO3P is a kind of high-quality and efficient
Plant growth regulator has and promotes Female flower differentiation, promotes fruit maturation, promotes dwarfing plants, breaks plant dormancy, adjustment portion
Divide the effects such as plant Dot Blots Sex.
The standard of existing country's detection ethephon (CEPHA),2-(chloroethyl) phosphonic acid is " GB 23200.16-2016 national food safety standard fruits and vegetables
The measurement of middle ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity ", " in GB 23200.82-2016 national food safety standard meat and meat products ethephon (CEPHA),2-(chloroethyl) phosphonic acid remain
The detection method of amount ".It is provided according in GB 2763-2012 Pesticide maximum residue limit, ethephon (CEPHA),2-(chloroethyl) phosphonic acid is maximum in fruit and vegetable
Residual quantity is 2mg/kg.Pre-treating method is complicated in national standard, and the pre-treatment reagent and consumptive material needed is more, and derivative examination
Agent diazomethane has the characteristics that penetrating odor, explosive, should not store, experimentation has very big security risk.
Due to the use age of ethephon (CEPHA),2-(chloroethyl) phosphonic acid and the specificity of application method, and it is to skin, the irritating effect of eyes, to viscous
Film has acid corrosion action, can pollute to environment and water body.Therefore, in order to determine ethephon (CEPHA),2-(chloroethyl) phosphonic acid pesticide residue in fruits and vegetables
Amount, there is an urgent need to explore a kind of feasible, easy chemical pesticide detection method.
Summary of the invention
The object of the present invention is to provide a kind of methods of ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables, without using derivative reagent,
Security performance is improved, it is simple to operate.
To achieve the goals above, technical solution provided by the invention is as follows:
A kind of method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables, comprising the following steps:
Step S1, the sample to be tested being homogenized is soaked in ml headspace bottle by distilled water and potassium hydroxide solution；
Step S2, ml headspace bottle is placed in constant temperature in automatic incubator, make to decomposite the ethylene come in water with reached in air
To balance；
Step S3, it with nitrogen as carrier gas, is detected using the gas chromatograph with flame ionization ditector,
Determine the residual quantity of ethephon (CEPHA),2-(chloroethyl) phosphonic acid in fruits and vegetables.
Preferably, the volume ratio of distilled water and potassium hydroxide solution is 1~3:1~6 in step S1, and potassium hydroxide solution is dense
Degree is 1-3g/mL.
It is highly preferred that the volume ratio of distilled water and potassium hydroxide solution is 3:5 in step S1, potassium hydroxide solution concentration is
1g/mL。
Preferably, distilled water is secondary distillation water in step S1.
Preferably, the temperature of constant temperature is 60-90 DEG C in step S2, time 30-60min.
It is highly preferred that the temperature of constant temperature is 80 DEG C in step S2, time 30min.
Preferably, GC conditions are as follows in step S3:
Chromatographic column: 1701 quartz capillary column of DB: 30m × 0.32mm × 0.25 μm；
Chromatogram column temperature:, keeping 4min by 60 DEG C, is warming up to 250 DEG C with 30 DEG C/min, keeps 2min；
Injector temperature: 250 DEG C；
Sample volume: 1 μ L；
Input mode: split sampling, split ratio 5:1；
Column flow rate: 1.0mL/min；
Detector temperature: 280 DEG C.
Specifically, the above-mentioned method for measuring ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in fruits and vegetables, comprising the following steps:
Step S1, by the sample to be tested 2.0g being homogenized in headspace sample bottle, 3mL distilled water and 5mL hydroxide is added
Potassium solution, distilled water are secondary distillation water, and potassium hydroxide solution concentration is 1g/mL；
Step S2, ml headspace bottle is placed in 80 DEG C of constant temperature 30min in automatic incubator, make to decomposite the ethylene come in water and
Reach balance in air；
Step S3, the preparation of standard items:
The standard substance ethephon (CEPHA),2-(chloroethyl) phosphonic acid 25.0mg for weighing purity >=98.5%, being placed in equipped with 2-3mL concentration is 0.081mol/L
In the 25mL brown volumetric flask of hydrochloric acid solution, dissolution is mixed, with 0.081mol/L hydrochloric acid solution constant volume, being configured to concentration is 1000
μ g/mL, 2-8 DEG C of preservation；Then 0.2,1.0,2.0,4.0 and 10.0 μ g/mL gradually are configured to 0.081mol/L hydrochloric acid solution
Standard working solution；
Step S4, each concentration standard working solution 1mL is drawn respectively in 20mL ml headspace bottle, adds distilled water 3mL and 1g/mL
Potassium hydroxide solution 5mL, seals, and with sample to be tested with machine in condition, constant temperature headspace sampling under conditions of 80 DEG C is utilized
Gas chromatograph with flame ionization ditector is detected, and GC conditions are as follows:
Chromatographic column: 1701 quartz capillary column of DB: 30m × 0.32mm × 0.25 μm；
Chromatogram column temperature:, keeping 4min by 60 DEG C, is warming up to 250 DEG C with 30 DEG C/min, keeps 2min；
Injector temperature: 250 DEG C；
Sample volume: 1 μ L；
Input mode: split sampling, split ratio 5:1；
Column flow rate: 1.0mL/min；
Detector temperature: 280 DEG C；
Carrier gas: nitrogen；
Head-space equipment condition: equilibrium temperature: 80 DEG C, equilibration time: 30min, needle temperature: 85 DEG C；
Step S5, standard curve is prepared, brings the peak area of sample to be tested into standard curve, checks in corresponding concentration, is counted
Calculate the content of ethephon (CEPHA),2-(chloroethyl) phosphonic acid in determinand.
Wherein, the fruit is selected from Kiwi berry, mango or banana.The vegetables are selected from cucumber, cucurbita pepo or tomato.
Compared with prior art, technical effect of the invention:
The method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity, first sample to be tested are urged through potassium hydroxide solution in measurement fruits and vegetables provided by the invention
Change to decompose and obtains ethylene gas；Then ethylene is heated by incubator, is reached in ml headspace bottle and to be balanced in liquids and gases
State；It finally with nitrogen as carrier gas, is detected using gas chromatography, external standard method determines ethephon (CEPHA),2-(chloroethyl) phosphonic acid in fruits and vegetables
Residual quantity.Method of the invention has sampling compared with the method for detecting fruits and vegetables ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in the prior art
The advantages that amount is few, and detection time is short, easy to operate safe, reaction is mild, avoid using it is inflammable and explosive, there is the good irritation of toxicity
Reagent；Testing result of the invention is accurate, and ethephon (CEPHA),2-(chloroethyl) phosphonic acid detection is limited to 0.05mg/kg, can satisfy water fruits and vegetables ethephon (CEPHA),2-(chloroethyl) phosphonic acid medicine
The requirement of object residual quantity quantitative detection.
Detailed description of the invention
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only one recorded in the present invention
A little embodiments are also possible to obtain other drawings based on these drawings for those of ordinary skill in the art.
Fig. 1 is the response result of different incubation temperatures provided by the invention；
Fig. 2 is the response result of different brooding times provided by the invention；
Fig. 3 is the response result of different concentration of potassium hydroxide provided by the invention；
Fig. 4 is the response result of different distilled water and potassium hydroxide base liquor capacity ratio provided by the invention.
Specific embodiment
In order to make those skilled in the art more fully understand technical solution of the present invention, below in conjunction with attached drawing to this hair
It is bright to be further detailed.Obviously, described embodiments are only a part of the embodiments of the present invention, rather than whole
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without making creative work
The every other embodiment obtained, shall fall within the protection scope of the present invention.Experimental method in following embodiments, such as without special theory
It is bright, it is conventional method.Test material as used in the following examples is unless otherwise specified from conventional biochemical reagent quotient
What shop was commercially available.Kiwi berry used in embodiment, mango, banana, cucumber, cucurbita pepo, tomato are purchased from Jilin Changchun
Supermarket.
1 headspace gas method of embodiment measures the condition selection of ethephon (CEPHA),2-(chloroethyl) phosphonic acid
The preparation of standard working solution:
Ethephon (CEPHA),2-(chloroethyl) phosphonic acid standard substance (No. CAS: the 16672-87-0) 25.0mg for weighing purity >=98.5% (is accurate to
0.01mg), it is placed in the 25mL brown volumetric flask equipped with about 2-3mL0.081mol/L hydrochloric acid solution, mixes dissolution, with
0.081mol/L hydrochloric acid solution constant volume, being configured to concentration is 1000 μ g/mL, stored refrigerated, validity period 6 months.Then it gradually uses
0.081mol/L hydrochloric acid solution is configured to the standard working solution of 0.2,1.0,2.0,4.0 and 10.0 μ g/mL.
Detection method: distilled water and hydroxide is added in headspace sample bottle in sample to be tested 2.0g (being accurate to 0.001g)
Potassium solution, and headspace sampling under constant temperature conditions, with the content of hydrogen flame detector detection ethephon (CEPHA),2-(chloroethyl) phosphonic acid, quantified by external standard method.Gas phase
Chromatographic condition is as follows:
Chromatographic column: 1701 quartz capillary column of DB: 30m × 0.32mm × 0.25 μm (or suitable column)；
Chromatogram column temperature: 60 DEG C (keeping 4min), 250 DEG C (keeping 2min) are warming up to 30 DEG C/min；
Injector temperature: 250 DEG C；
Sample volume: 1 μ L；
Input mode: split sampling (split ratio 5:1)；
Column flow rate: 1.0mL/min；
Detector temperature: 280 DEG C；
Carrier gas: nitrogen.
(1) select same concentration ethephon (CEPHA),2-(chloroethyl) phosphonic acid standard working solution, other conditions under the same conditions, incubator temperature choosing
50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C have been selected, have been measured respectively, the ratio of incubator temperature (X-axis) and response (Y-axis)
As shown in Figure 1.According to testing result, 60-90 DEG C of incubator temperature when, when response is up to 13000 or more, 80 DEG C, response reaches
15000 or more, therefore, select 80 DEG C of optimum temperatures as incubator.
(2) select same concentration ethephon (CEPHA),2-(chloroethyl) phosphonic acid standard working solution, other conditions under the same conditions, brooding time selection
20min, 30min, 40min, 50min, 60min, are measured, the ratio of brooding time (X-axis) and response (Y-axis) respectively
As shown in Figure 2.According to testing result, brooding time exists, when 30-60min, response up to 15000 or more, in order to energy saving and
Time, therefore select best brooding time of the 30min as incubator.
(3) the ethephon (CEPHA),2-(chloroethyl) phosphonic acid standard working solution of same concentration, instrument condition condition identical with other Pretreatments are selected
Under, potassium hydroxide alkaline concentration has selected 0.1g/mL, 0.2g/mL, 0.5g/mL, 1.0g/mL, 2.0g/mL, 3.0g/mL, point
It is not measured, concentration of potassium hydroxide (g/mL) (X-axis) and the ratio of response (Y-axis) are as shown in Figure 3.According to testing result,
For potassium hydroxide solution concentration in 1-3g/mL, response reaches peak up to 14000 or more, and in 1g/mL, and also to
Reagent is saved, therefore selects potassium hydroxide solution concentration 1g/mL as the optium concentration of potassium hydroxide solution in pre-treatment.
(4) the ethephon (CEPHA),2-(chloroethyl) phosphonic acid standard working solution of same concentration is selected, potassium hydroxide alkaline concentration is 1g/mL, at other
Under the same conditions, distilled water and potassium hydroxide base liquor capacity ratio have selected 1:4,1:2,3:5,3:4,4:5,1:1 to part, respectively
It is measured, distilled water and potassium hydroxide base liquor capacity ratio (X-axis) and the ratio of response (Y-axis) are as shown in Figure 4.According to inspection
It surveys as a result, distilled water and potassium hydroxide base liquor capacity ratio are in 1:1-1:2, response is up to 14000 or more, and volume ratio is in 3:5
When reach peak, therefore select 3:5 as the optimum volume ratio of distilled water and potassium hydroxide aqueous slkali.
2 range of linearity of embodiment, detection limit and quantitative limit evaluation
The range of linearity: using the standard working solution for the various concentration that embodiment is prepared, using peak area as ordinate, standard work
The mass concentration for making liquid is that abscissa draws standard curve, as the result is shown within the scope of 0.2~10.0 μ g/mL, the quality of ethephon (CEPHA),2-(chloroethyl) phosphonic acid
Linear relationship is good between concentration and corresponding peak area, and related coefficient is greater than 0.999.
Detection limit and quantitative limit: standard working solution will be added respectively in blank sample, be configured to final concentration of 0mg/kg,
The ethephon (CEPHA),2-(chloroethyl) phosphonic acid standard solution of 0.025mg/kg, 0.05mg/kg, 0.1mg/kg, 0.2mg/kg, according to the test method of embodiment 1,
Its signal-to-noise ratio is tested, detection line and quantitative limit is determined respectively, is with the detection limit (LOD) that signal-to-noise ratio S/N >=3 obtain object
0.05mg/kg obtains quantifying for object with signal-to-noise ratio S/N >=10 and is limited to 0.2mg/kg.
The 3 sample detection rate of recovery of embodiment and precision
1, negative fruits and vegetables sample Kiwi berry, mango, banana, cucumber, cucurbita pepo and tomato homogenate sample pre-treatments: are taken
It is good, add the ethephon (CEPHA),2-(chloroethyl) phosphonic acid of 0.0100,0.0200 and 0.0500mg/kg, tri- concentration levels respectively in different substrates sample, point
It also known as takes the mark-on sample 2.0g of different substrates in headspace sample bottle, 3mL distilled water and 5mL potassium hydroxide solution is added, steam
Distilled water is secondary distillation water, and potassium hydroxide solution concentration is 1g/mL.
2, sample detection: each concentration standard working solution 1mL of extraction embodiment preparation adds in 20mL ml headspace bottle respectively
Distilled water 3mL and 1g/mL potassium hydroxide solution 5mL, seals, with sample to be tested with machine in condition, under conditions of 80 DEG C
Constant temperature headspace sampling, each mark-on horizontal parallel measure 3 times, using the gas chromatograph with flame ionization ditector into
Row detection, GC conditions such as embodiment 1, Head-space equipment condition: equilibrium temperature: 80 DEG C, equilibration time: 30min, needle temperature
Degree: 85 DEG C.
3, testing result: preparing standard curve, brings the peak area of sample to be tested into standard curve, checks in corresponding dense
Degree calculates the content of ethephon (CEPHA),2-(chloroethyl) phosphonic acid in determinand.Its average recovery rate range is 85.3%~102.4%, and relative standard deviation is small
In 6%, concrete outcome is shown in Table 1.
1 ethephon (CEPHA),2-(chloroethyl) phosphonic acid recovery of standard addition of table and relative standard deviation (n=3)
It is above that certain exemplary embodiments of the invention are only described by way of explanation, undoubtedly, for ability
The those of ordinary skill in domain without departing from the spirit and scope of the present invention can be with a variety of different modes to institute
The embodiment of description is modified.Therefore, above-mentioned attached drawing and description are regarded as illustrative in nature, and should not be construed as to the present invention
The limitation of claims.
Claims (10)
1. a kind of method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables, which comprises the following steps:
Step S1, the sample to be tested being homogenized is soaked in ml headspace bottle by distilled water and potassium hydroxide solution；
Step S2, ml headspace bottle is placed in constant temperature in automatic incubator, make to decomposite the ethylene come in water with reach flat in air
Weighing apparatus；
Step S3, it with nitrogen as carrier gas, is detected, is determined using the gas chromatograph with flame ionization ditector
The residual quantity of ethephon (CEPHA),2-(chloroethyl) phosphonic acid in fruits and vegetables.
2. the method for ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables according to claim 1, which is characterized in that distilled in step S1
The volume ratio of water and potassium hydroxide solution is 1~3:1~6, and potassium hydroxide solution concentration is 1-3g/mL.
3. the method for ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables according to claim 2, which is characterized in that distilled in step S1
The volume ratio of water and potassium hydroxide solution is 3:5, and potassium hydroxide solution concentration is 1g/mL.
4. the method for ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables according to claim 1, which is characterized in that distilled in step S1
Water is secondary distillation water.
5. the method for ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables according to claim 1, which is characterized in that constant temperature in step S2
Temperature be 60-90 DEG C, time 30-60min.
6. the method for ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables according to claim 5, which is characterized in that constant temperature in step S2
Temperature be 80 DEG C, time 30min.
7. the method for ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables according to claim 1, which is characterized in that gas phase in step S3
Chromatographic condition is as follows:
Chromatographic column: 1701 quartz capillary column of DB: 30m × 0.32mm × 0.25 μm；
Chromatogram column temperature:, keeping 4min by 60 DEG C, is warming up to 250 DEG C with 30 DEG C/min, keeps 2min；
Injector temperature: 250 DEG C；
Sample volume: 1 μ L；
Input mode: split sampling, split ratio 5:1；
Column flow rate: 1.0mL/min；
Detector temperature: 280 DEG C.
8. the method for ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables according to claim 1, which is characterized in that including following step
It is rapid:
Step S1, by the sample to be tested 2.0g being homogenized in headspace sample bottle, 3mL distilled water is added and 5mL potassium hydroxide is molten
Liquid, distilled water are secondary distillation water, and potassium hydroxide solution concentration is 1g/mL；
Step S2, ml headspace bottle is placed in 80 DEG C of constant temperature 30min in automatic incubator, makes the ethylene decomposited in water and air
In reach balance；
Step S3, the preparation of standard items:
The standard substance ethephon (CEPHA),2-(chloroethyl) phosphonic acid 25.0mg for weighing purity >=98.5%, being placed in equipped with 2-3mL concentration is 0.081mol/L hydrochloric acid
In the 25mL brown volumetric flask of solution, dissolution is mixed, with 0.081mol/L hydrochloric acid solution constant volume, being configured to concentration is 1000 μ g/
ML, 2-8 DEG C of preservations；Then the mark of 0.2,1.0,2.0,4.0 and 10.0 μ g/mL is gradually configured to 0.081mol/L hydrochloric acid solution
Quasi- working solution；
Step S4, each concentration standard working solution 1mL is drawn respectively in 20mL ml headspace bottle, adds distilled water 3mL and 1g/mL hydrogen-oxygen
Change potassium solution 5mL, seals, with sample to be tested with machine in condition, constant temperature headspace sampling under conditions of 80 DEG C, using having
The gas chromatograph of flame ionization ditector is detected, and GC conditions are as follows:
Chromatographic column: 1701 quartz capillary column of DB: 30m × 0.32mm × 0.25 μm；
Chromatogram column temperature:, keeping 4min by 60 DEG C, is warming up to 250 DEG C with 30 DEG C/min, keeps 2min；
Injector temperature: 250 DEG C；
Sample volume: 1 μ L；
Input mode: split sampling, split ratio 5:1；
Column flow rate: 1.0mL/min；
Detector temperature: 280 DEG C；
Carrier gas: nitrogen；
Head-space equipment condition: equilibrium temperature: 80 DEG C, equilibration time: 30min, needle temperature: 85 DEG C；
Step S5, prepare standard curve, bring the peak area of sample to be tested into standard curve, check in corresponding concentration, calculate to
Survey the content of ethephon (CEPHA),2-(chloroethyl) phosphonic acid in object.
9. the method for ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables according to claim 1-8, which is characterized in that described
Fruit is selected from Kiwi berry, mango or banana.
10. the method for ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables according to claim 1-8, which is characterized in that institute
It states vegetables and is selected from cucumber, cucurbita pepo or tomato.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910756484.5A CN110470759A (en) | 2019-08-16 | 2019-08-16 | A kind of method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910756484.5A CN110470759A (en) | 2019-08-16 | 2019-08-16 | A kind of method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110470759A true CN110470759A (en) | 2019-11-19 |
Family
ID=68510142
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910756484.5A Pending CN110470759A (en) | 2019-08-16 | 2019-08-16 | A kind of method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110470759A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103575798A (en) * | 2013-09-12 | 2014-02-12 | 浙江出入境检验检疫局检验检疫技术中心 | Method for measuring residues of ethephon, thidiazuron and diuron in cotton by using liquid chromatography tandem mass spectrometry |
| CN103969363A (en) * | 2014-04-09 | 2014-08-06 | 温州市质量技术监督检测院 | Detection method for plant growth regulator residues in fruits |
| CN108760949A (en) * | 2018-04-20 | 2018-11-06 | 公安部物证鉴定中心 | The detection method of plant growth regulator ethephon (CEPHA),2-(chloroethyl) phosphonic acid in biological fluid |
| CN109725085A (en) * | 2019-03-04 | 2019-05-07 | 杭州普洛赛斯检测科技有限公司 | A method of detection ethephon (CEPHA),2-(chloroethyl) phosphonic acid |
-
2019
- 2019-08-16 CN CN201910756484.5A patent/CN110470759A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103575798A (en) * | 2013-09-12 | 2014-02-12 | 浙江出入境检验检疫局检验检疫技术中心 | Method for measuring residues of ethephon, thidiazuron and diuron in cotton by using liquid chromatography tandem mass spectrometry |
| CN103969363A (en) * | 2014-04-09 | 2014-08-06 | 温州市质量技术监督检测院 | Detection method for plant growth regulator residues in fruits |
| CN108760949A (en) * | 2018-04-20 | 2018-11-06 | 公安部物证鉴定中心 | The detection method of plant growth regulator ethephon (CEPHA),2-(chloroethyl) phosphonic acid in biological fluid |
| CN109725085A (en) * | 2019-03-04 | 2019-05-07 | 杭州普洛赛斯检测科技有限公司 | A method of detection ethephon (CEPHA),2-(chloroethyl) phosphonic acid |
Non-Patent Citations (3)
| Title |
|---|
| 周艳明 等: "水果、蔬菜中乙烯利残留量的测定方法", 《食品科学》 * |
| 姚伟琴 等: "自动顶空气相色谱法测定番茄酱中乙烯利的残留量", 《中国卫生检验杂志》 * |
| 孔祥虹 等: "顶空气相色谱法快速测定肉及肉制品中乙烯利的残留量", 《分析试验室》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| FELLE | Proton transport and pH control in Sinapis alba root hairs: a study carried out with double-barrelled pH micro-electrodes | |
| Andersen et al. | Structure-antifungal activity relationships among volatile C6 and C9 aliphatic aldehydes, ketones, and alcohols | |
| CN106596774B (en) | A kind of detection method of biocontrol microorganisms Volatile Metabolites | |
| CN102590195A (en) | Method for testing nitrite and nitrate in pickled vegetables | |
| Esti et al. | Determination of amines in fresh and modified atmosphere packaged fruits using electrochemical biosensors | |
| CN110470759A (en) | A kind of method of ethephon (CEPHA),2-(chloroethyl) phosphonic acid residual quantity in measurement fruits and vegetables | |
| CN108760949A (en) | The detection method of plant growth regulator ethephon (CEPHA),2-(chloroethyl) phosphonic acid in biological fluid | |
| Zhang et al. | Aroma in freshly squeezed strawberry juice during cold storage detected by E-nose, HS–SPME–GC–MS and GC-IMS | |
| Horvat | Identification of some volatile compounds in cooked chicken | |
| Shimoji et al. | Validation study of histamine test for the determination of histamine in selected fish products | |
| SHIMOKAWA et al. | BIOGENESIS OF ETHYLENE IN APPLE TISSUE: I. FORMATION OF ETHYLENE FROM GLUCOSE, ACETATE, PYRUVATE, AND ACETALDEHYDE IN APPLE TISSUE | |
| CN102268471A (en) | Microbiological method for detecting acephate residues in food | |
| Calbo et al. | Intercellular volume and resistance to air flow of fruits and vegetables | |
| CN107478478A (en) | A kind of fumonisin B1Substrate standard substance and preparation method thereof | |
| Yang et al. | Accumulation, migration and health risk of trace metals in a soil-strawberry-human system of the Yangtze River Delta region, China | |
| CN102517230B (en) | Bifidobacterium breve and detection method of methamidopho pesticide residue in foodstuff | |
| CN109022536A (en) | The method of aerogenic bacteria in bromocresol purple and Du Shi tubule combined highly effective detection vinegar | |
| Chang et al. | Automated dual-chamber sampling system to follow dynamics of volatile organic compounds emitted by biological specimens | |
| CN110208426A (en) | A kind of pork freshness evaluation method based on biogenic amine | |
| CN110412022A (en) | A kind of quickly detection organic solid castoff NH3The gel test paper and its application method of volatility | |
| Jat et al. | Knowledge level of farmers about improved tomato production technology | |
| CN104280557A (en) | Enzyme linked immunoassay kit for detecting abamectin and preparation method and detection method of enzyme linked immunoassay kit | |
| CN106636215A (en) | Method of increasing active component content of phellinus igniarius | |
| CN102304482B (en) | Cifidobacterium longum strain | |
| CN102156175A (en) | Method for measuring high and low-density lipoprotein cholesterol content of animal meat |
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: 20191119 |
|
| RJ01 | Rejection of invention patent application after publication |