CN112986460A - Method for detecting residual quantity of iminoctadine tris in plant-derived food - Google Patents
Method for detecting residual quantity of iminoctadine tris in plant-derived food Download PDFInfo
- Publication number
- CN112986460A CN112986460A CN202110407215.5A CN202110407215A CN112986460A CN 112986460 A CN112986460 A CN 112986460A CN 202110407215 A CN202110407215 A CN 202110407215A CN 112986460 A CN112986460 A CN 112986460A
- Authority
- CN
- China
- Prior art keywords
- sample
- extracting
- column
- solution
- iminoctadine
- 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
Images
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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to a method for detecting the residual quantity of iminoctadine hydrochloride in plant food, which comprises the following steps: (1) sample extraction: weighing a sample to be detected in a detection amount in a centrifuge tube, adding dichloromethane, homogenizing and extracting by a homogenizer, centrifugally separating an organic phase, repeatedly extracting for two times, combining extracting solutions, and concentrating a sample concentrated solution; (2) sample purification: activating the weak cation solid phase extraction column WCX, transferring the sample concentrated solution to the column, and discarding all effluent liquid. Pumping out the small column under reduced pressure, eluting, collecting eluate, concentrating to near dryness, diluting with formic acid-methanol solution to constant volume, mixing, and filtering with filter membrane to obtain detection solution; (3) and (3) sample determination: the samples were measured by LC-MS/MS and monitored for ion pairs (m/z) of 178.7/100.0 (quantitative), 178.7/128.1 (qualitative).
Description
Technical Field
The invention belongs to the field of chemistry, and particularly relates to a method for detecting residual quantity of iminoctadine benzene sulfonate in plant-derived food.
Background
Biguanide trioctyl benzene sulfonate (iminoctadinetris) (albesilate), also known as a belladonna, is a contact-type broad-spectrum protective bactericide, can inhibit spore germination, germ tube elongation and formation of attached spores and hyphae by preventing synthesis and cell membrane function of ester compounds of pathogenic bacteria, has an effect on biosynthesis and cell membrane function of fungus ester compounds, and can prevent and treat various plant diseases caused by ascomycetes and adelomycetes; is mainly used for preventing and treating diseases of citrus fruits in the storage period in China.
The Iminoctadine (Iminoctadine) is a pesticide bactericide Iminoctadine and is a residue measured after the Iminoctadine is used by crops, the national standard GB 2763 and 2019 stipulates that the daily allowable intake of the Iminoctadine is 0.009mg/kg bw, and a limit is provided for Iminoctadine residues in matrixes such as watermelon, mandarin orange, tangerine, apple, tomato, cucumber and the like, the range is 0.2-3.0mg/kg, and Japan also stipulates that the Iminoctadine residues in different plant source products are 0.02-2.0 mg/kg.
In the aspect of the detection method, related literature reports are few, most of the methods are liquid chromatography, the experimental steps are complicated, and derivation is needed, so that the method which is simple and rapid to establish and operate, high in sensitivity and good in accuracy plays an important role in maintaining the benefits of the country, improving the technical level of pesticide residue detection in China, maintaining the food safety technical support system in China and the like. .
Disclosure of Invention
The invention firstly relates to a method for measuring the residual quantity of iminoctadine hydrochloride in plant food, which comprises the following steps:
(1) sample extraction: weighing a sample to be detected in a detection amount in a centrifuge tube, adding dichloromethane, homogenizing and extracting by a homogenizer, centrifugally separating an organic phase, repeatedly extracting for two times, combining extracting solutions, and concentrating a sample concentrated solution;
(2) sample purification: activating the weak cation solid phase extraction column WCX, transferring the sample concentrated solution to the column, and discarding all effluent liquid. Pumping out the small column under reduced pressure, eluting, collecting eluate, concentrating to near dryness, diluting with formic acid-methanol solution to constant volume, mixing, and filtering with filter membrane to obtain detection solution;
(3) and (3) sample determination: the samples were measured by LC-MS/MS and monitored for ion pairs (m/z) of 178.7/100.0 (quantitative), 178.7/128.1 (qualitative).
In the step (1), the sample to be detected is a plant matrix sample, and the detection amount is 2-5 g;
preferably, the sample extraction step is: weighing 2-5g of plant matrix sample, extracting with 30mL of dichloromethane for the first time, extracting with 20mL of dichloromethane twice repeatedly, wherein the rotation speed of a homogenizer is 10000r/min, the homogenizing extraction time is 1min, the rotation speed of a centrifuge is 4000r/min, the centrifugation time is 5min, and the extracting solution is concentrated to about 2 mL;
in the step (2),
the conditions for vacuum-pumping the column were as follows: negative pressure of 65KPa for 10 min;
the elution conditions were: 15mL of formic acid-methanol solution, wherein the volume ratio of the formic acid-methanol solution is as follows: 1: 9;
the concentration conditions were: concentrating in water bath at 40 deg.C until it is nearly dry;
in the step (3), the step (c),
the LC conditions were:
a chromatographic column: Phenyl-Hexyl phenylhexyl (150 mm. times.2.1 mm,3.5 μm);
mobile phase: (A) 1% aqueous formic acid; (B) 1% formic acid-methanol solution; using isocratic elution, flow phase ratio: a: b-91: 9, flow rate: 0.3 mL/min.
Column temperature: 35 ℃;
sample introduction amount: 10 mu L of the solution;
the conditions of MS/MS are as follows:
an ion source: ESI;
the scanning mode is as follows: scanning positive ions;
the detection mode is as follows: monitoring multiple reactions;
the atomizing gas, the air curtain gas, the auxiliary gas and the collision gas are all high-purity nitrogen;
electrospray voltage (IS): 5500V;
atomizing gas (GS 1): 55 psi;
assist gas (GS 2): 50 psi;
air curtain gas (CUR): 25 psi;
ion source Temperature (TEM): 550 ℃;
biguanide octylamine monitoring quantitative ion pair (m/z): 178.7/100.0, declustering voltage (DP): 90V, Collision gas energy (CE): 19V, collision cell entrance voltage (EP): 10V;
biguanide octylamine monitoring qualitative ion pair (m/z): 178.7/128.1, declustering voltage (DP): 90V, Collision gas energy (CE): 27V, collision cell entrance voltage (EP): 10V.
In the LC-MS/MS measuring method described in the step (3),
the retention time of the iminoctadine is 1.56 min;
the regression equation for quantifying iminoctadine is 3250X + 22000. (Y is the peak area; X is the concentration in mg/kg)
The invention has the beneficial effects that:
the invention provides a method for measuring the residual quantity of trioctylphenylsulfonate biguanide in plant food, which comprises the steps of extracting the trioctylphenylsulfonate residue in a sample by using dichloromethane for homogenization, purifying the residue by using a solid phase extraction column, detecting the residue by using LC-MS/MS, quantifying the residue by using an external standard method, and selecting characteristic parent ions [ M +2H ]2+ which are in double charges under a positive ion mode, wherein the M/z of the characteristic parent ions is 178.7; in addition, m/z 100.0 (shown in figure 1A) and m/z 128.1 (shown in figure 1B) are selected as fragment ions for multi-reaction monitoring, the method has the advantages of simplicity and convenience in operation, rapidness and high sensitivity, can be used for detecting the residual quantity of the iminoctadine hydrochloride in the plant-derived food, and has important significance for improving the technical level of pesticide residue detection in China.
Drawings
FIG. 1, polyion reaction monitoring chromatogram of iminoctadine standard solution (A) quantitative ion pair (m/z): 178.7/100.0, (B) qualitative ion pair (m/z): 178.7/128.1.
FIG. 2 is a chromatogram of iminoctadine in a representative actual sample (A is a positive asparagus sample, B is a negative lycium barbarum sample).
Detailed Description
Instruments and reagents:
liquid chromatography-tandem mass spectrometer: equipped with an electrospray ion source (ESI) (AB Sciex Co.),
a chromatographic column: Phenyl-Hexyl phenylhexyl (150 mm. times.2.1 mm,3.5 μm) (Watts Corp.); ,
an electronic balance: sensitivity 0.1mg, 0.01g (Shimadzu corporation); ,
homogenizers (Scientific Industries);
centrifuge (Thermo);
rotary evaporator (BUCHI);
ultra-pure water generator (Merck Mike)
Polypropylene centrifuge tube (80 mL);
heart bottle (120 mL);
0.22 μm microfiltration membrane (organic phase type) (Tianjintsushi technologies, Ltd.).
WCX weak cation solid phase extraction column: 150mg, 6mL (Watts Corp.).
Biguanide trioctane phenyl sulfonate (Albesilate), Cas No.169202-06-6, ≧ 98.6%, 1000 μ g/mL (Dr. Ehrenstontorfer Co.).
Dichloromethane (HPLC grade, Dikma), acetonitrile (HPLC grade, dima), methanol (HPLC grade, dima), formic acid (HPLC grade, Sigma-Aldrich).
Example 1 selection of conditions for extraction of iminoctadine tricaprylphonate residues from plant-derived food products
Sample source:
collecting plant source food: asparagus, medlar and wheat.
The experimental steps are as follows:
weighing 5g of asparagus, medlar or wheat sample (accurate to 0.01g), adding iminoctadine with the horizontal concentration of 1.0mg/kg into a 80mL centrifuge tube, standing and aging for more than 2 h. 6 parts of positive samples are added in each type of matrix in parallel, 30mL of acetonitrile, methanol, acetonitrile + methanol (1+1), dichloromethane, n-butanol + n-hexane and phosphate buffer solution are respectively added, and the extraction test conditions are optimized, wherein the steps are as follows:
(1) homogenizing and extracting at 10000r/min for 1min with a homogenizer, centrifuging at 4000r/min for 5min, extracting organic phase, extracting with 20mL dichloromethane twice, mixing three extractive solutions, and concentrating to about 2 mL;
(2) transferring the concentrated solution to a WCX weak cation solid phase extraction column which is activated by 6mL of methanol and 6mL of water in advance, and discarding all effluent liquid;
(3) and (2) under the negative pressure of 65KPa, carrying out decompression and suction drying on the weak cation solid phase extraction column for 10min, eluting with 15mL of formic acid-methanol, collecting the eluent in a heart-shaped bottle, carrying out rotary concentration in a water bath at 40 ℃ until the eluent is nearly dry, carrying out constant volume of 1mL of formic acid-methanol, mixing the eluent uniformly, carrying out a 0.22-micron organic phase microfiltration membrane, and then carrying out LC-MS/MS determination.
The LC conditions were:
a chromatographic column: Phenyl-Hexyl phenylhexyl (150 mm. times.2.1 mm,3.5 μm);
mobile phase: (A) 1% aqueous formic acid; (B) 1% formic acid-methanol solution; isocratic elution was used, flow phase ratio: a: b-91: 9, flow rate: 0.3 mL/min.
Column temperature: 35 ℃;
sample introduction amount: 10 mu L of the solution;
the conditions of MS/MS are as follows:
an ion source: ESI;
the scanning mode is as follows: scanning positive ions;
the detection mode is as follows: monitoring multiple reactions;
the atomizing gas, the air curtain gas, the auxiliary gas and the collision gas are all high-purity nitrogen;
electrospray voltage (IS): 5500V;
atomizing gas (GS 1): 55 psi;
assist gas (GS 2): 50 psi;
air curtain gas (CUR): 25 psi;
ion source Temperature (TEM): 550 ℃;
biguanide octylamine monitoring quantitative ion pair (m/z): 178.7/100.0, declustering voltage (DP): 90V, Collision gas energy (CE): 19V, collision cell entrance voltage (EP): 10V;
biguanide octylamine monitoring qualitative ion pair (m/z): 178.7/128.1, declustering voltage (DP): 90V, Collision gas energy (CE): 27V, collision cell entrance voltage (EP): 10V;
the retention time of the iminoctadine is 1.56min through the optimization of the instrument conditions.
Preparing a standard solution: weighing a proper amount of biguanide trioctane phenyl sulfonate standard substance, and preparing into a standard stock solution with the concentration of 1000 mug/mL (calculated by biguanide octylamine) by using acetonitrile-methanol (1+1, volume ratio); sucking a proper amount of standard stock solution, and preparing a standard working solution of 10 mu g/mL by using acetonitrile-methanol (1+1, volume ratio); the stock solution and the working solution are stored at 0-4 ℃ in the dark.
Configuring a standard working curve: the intermediate standard solution was diluted with the blank sample matrix solution as required to 0.05. mu.g/mL, 0.1. mu.g/mL, 0.2. mu.g/mL, 0.5. mu.g/mL, 1.0. mu.g/mL of the standard working solution, which was prepared as it is.
Under the experimental conditions determined by the method, the diguanide octylamine standard working solution is measured, a linear regression curve is drawn by the peak area to the concentration, and the regression equation is that Y is 3250X +22000(Y is the peak area; X is the concentration, the unit is mg/kg), (r is)20.9992). The concentration and the response value have good linear relation, and the quantitative requirement is met.
In the experiment, blank asparagus is taken as a representative substrate, iminoctadine with the concentration of 1mg/kg is added into the substrate, and the extraction effects of acetonitrile, methanol, acetonitrile + methanol (1+1), n-butanol + n-hexane, phosphate buffer solution and dichloromethane are examined. The results show that when acetonitrile, methanol, acetonitrile + methanol (1+1, v/v) and n-butanol + n-hexane (1+1, v/v) are used as extraction solvents, the recovery rate of the iminoctadine is below 20%, and the extraction recovery rates of the iminoctadine using a phosphate buffer solution and dichloromethane as extraction solvents are shown in table 1, which shows that the extraction effect of dichloromethane is the best. Further verification results show that the recovery rate of the asparagus, the medlar and the wheat is 78.1-97.2% when the addition concentration of the asparagus, the medlar and the wheat is 1mg/kg by adopting dichloromethane, so dichloromethane is selected as an extraction solvent in experiments.
Table 1 comparison of recovery of iminoctadine in phosphate buffer and dichloromethane as extraction solvents (n ═ 6)
Example 2 selection optimization of cleaning conditions for biguanide trioctylphosphine sulfonate residue in plant-derived food
The sample sources were the same as in example 1.
The purification conditions were further optimized as in the experimental procedure of example 1.
In view of the few reports reported in the literature relating to biguanide trioctylphenylsulfonic Acid, on the basis of its strong polarity, Oasis MCX (strong cation exchange), Oasis MAX (strong anion exchange), Oasis WCX (weak cation exchange), Oasis WAX (weak anion exchange), and other brands BAKERBOND Carboxylic Acid (Carboxylic Acid column), insertsep CBA (ethylcarboxyl-bound silica gel column) were selected for comparative optimization experiments.
In the first stage, the standard sample is directly loaded, eluted and put on a machine for detection. Oasis WCX, Oasis MAX and InertSep CBA are screened, and other columns are not applicable.
In the second stage, three substrates of asparagus, medlar and wheat are added according to the standard of 1mg/kg, dichloromethane is extracted for three times, three parallel experiments are carried out to investigate the average recovery rate, and the result shows that Oasis WCX is obviously superior to other two solid phase extraction columns and meets the detection requirement. Therefore, the method adopts an Oasis WCX (6cc/150mg) column for purification.
The method is used for pretreating an Oasis WCX (6cc/150mg) column: 6mL of methanol and 6mL of water are sequentially activated to ensure that the column body is wetted and loaded, and the elution solvent is 10% formic acid-methanol solution (10% formic acid is added into the methanol solution).
The method is tested according to the elution volume, 10 mu L of standard solution with the concentration of 100 mu g/mL is added into 2mL of phosphoric acid buffer solution with the pH value of 4, the solution passes through an Oasis WCX solid phase extraction column according to the conditions specified by the method, every 5mL of effluent is collected in a single test tube, 20mL of effluent is collected, the recovery rate of the iminoctadine in each section of effluent is detected, and the experimental result shows that no iminoctadine is detected in the fourth 5mL of effluent, so that the 10% formic acid-methanol solution with the volume of 15mL is determined to be used for elution.
Example 3 selection and optimization of LC-MS/MS conditions
The LC-MS/MS conditions were further selected and optimized as in the experimental procedure of example 1.
1. Selection of liquid chromatography conditions:
three liquid chromatography columns of BEH C18(100 mm. times.2.1 mm,1.7 μm), BEH HILIC (100 mm. times.2.1 mm,1.7 μm) and Phenyl-Hexyl (150 mm. times.2.1 mm,3.5 μm) were selected for the tests.
As a result of the test, it was found that Phenyl-Hexyl (150 mm. times.2.1 mm,3.5 μm) column had a satisfactory peak shape and sensitivity.
In order to further improve the sensitivity of the measured object in the positive ion mode, the influence of adding formic acid with the volume fraction of 0.1%, 0.2%, 0.5%, 1.0% and 2.0% in the mobile phase is researched,
the results show that the sensitivity is the highest without significant difference under the condition that the volume fraction of the added formic acid is 1.0 percent and 2.0 percent, and the volume fraction of the formic acid is 1.0 percent.
2. Selection of mass spectrometry conditions:
taking a diguanide octylamine standard substance with the concentration of 10 mu g/mL, injecting the diguanide octylamine standard substance into an ion source at the flow rate of 10 mu L/min, finding out qualitative and quantitative ion pairs, and simultaneously optimizing parameters such as declustering voltage (DP), collision chamber inlet voltage (EP), Collision Energy (CE), collision chamber outlet voltage (CXP) and the like.
The detection parent ions of general compounds in the positive ion detection mode are usually [ M + H ] + or [ M + Na + ] and the like, but in the practical optimization process, the sensitivity of the general quasi-molecular ions is found to be very low, and the compounds are found to be double-charged in the positive ion mode by combining the molecular structure of the compounds, so 178.7 is selected as the characteristic parent ion. The characteristic parent ion [ M +2H ]2+/2M/z of the iminoctadine is 178.7, then the daughter ion is subjected to full scanning, comprehensive factor investigation is carried out, and finally M/z 100.0 and M/z 128.1 are selected as the monitored daughter ion.
Thus: biguanide octylamine monitoring quantitative ion pair (m/z): 178.7/100.0, declustering voltage (DP): 90V, Collision gas energy (CE): 19V, collision cell entrance voltage (EP): 10V;
biguanide octylamine monitoring qualitative ion pair (m/z): 178.7/128.1, declustering voltage (DP): 90V, Collision gas energy (CE): 27V, collision cell entrance voltage (EP): 10V.
Example 4 measurement of residual amount of iminoctadine tris (hydroxymethyl) benzenesulfonate in commercially available plant-derived food
15 parts of commercially available plant source food comprising 3 parts of asparagus juice, 4 parts of asparagus, 4 parts of medlar, 2 parts of cucumber and 2 parts of flour are collected, and the residual quantity of the trioctyl benzene sulfonate in the biguanide is measured by adopting the method disclosed by the invention.
The determination result shows that the biguanide trioctyl benzene sulfonate residue is not detected in other samples except asparagus and products thereof; the content of iminoctadine detected by 1 sample of 3 asparagus juice is 0.032mg/kg, the content detected by 2 samples of 4 asparagus is 0.058mg/kg and 0.629mg/kg respectively, and the chromatographic charts of iminoctadine in representative positive and negative samples are shown in figure 2. The detection results show that the residue of the iminoctadine tris is relatively high in asparagus and products thereof.
Finally, it should be noted that the above examples are only used to help those skilled in the art understand the essence of the present invention, and should not be used as a limitation to the protection scope of the present invention.
Claims (6)
1. A method for measuring the residual quantity of iminoctadine hydrochloride in plant food comprises the following steps:
(1) sample extraction: weighing a sample to be detected in a detection amount in a centrifuge tube, adding dichloromethane, homogenizing and extracting by a homogenizer, centrifugally separating an organic phase, repeatedly extracting for two times, combining extracting solutions, and concentrating a sample concentrated solution;
(2) sample purification: activating the weak cation solid phase extraction column WCX, transferring the sample concentrated solution to the column, and discarding all effluent liquid. Pumping out the small column under reduced pressure, eluting, collecting eluate, concentrating to near dryness, diluting with formic acid-methanol solution to constant volume, mixing, and filtering with filter membrane to obtain detection solution;
(3) and (3) sample determination: the samples were measured by LC-MS/MS and monitored for ion pairs (m/z) of 178.7/100.0 (quantitative), 178.7/128.1 (qualitative).
2. The assay method according to claim 1, wherein in step (1), the sample to be assayed is a plant substrate sample, and the amount detected is 2 to 5 g;
preferably, the sample extraction step is: weighing 2-5g of plant matrix sample, extracting with 30mL of dichloromethane for the first time, extracting with 20mL of dichloromethane twice, wherein the rotation speed of a homogenizer is 10000r/min, the homogenizing extraction time is 1min, the rotation speed of a centrifuge is 4000r/min, the centrifugation time is 5min, and the extracting solution is concentrated to about 2 mL.
3. The method according to claim 1 to 2, wherein in the step (2),
the conditions for vacuum-pumping the column were as follows: negative pressure of 65KPa for 10 min;
the elution conditions were: 15mL of formic acid-methanol solution, wherein the volume ratio of the formic acid-methanol solution is as follows: 1: 9;
the concentration conditions were: concentrating to near dryness by rotation in a water bath at 40 ℃.
4. The method according to claim 1 to 2, wherein in the step (3),
the LC conditions were:
a chromatographic column: Phenyl-Hexyl phenylhexyl (150 mm. times.2.1 mm,3.5 μm);
mobile phase: (A) 1% aqueous formic acid; (B) 1% formic acid-methanol solution; isocratic elution was used, flow phase ratio: a: b-91: 9, flow rate: 0.3 mL/min;
column temperature: 35 ℃;
sample introduction amount: 10 μ L.
5. The method according to claim 4, wherein in the step (3),
the conditions of MS/MS are as follows:
an ion source: ESI;
the scanning mode is as follows: scanning positive ions;
the detection mode is as follows: monitoring multiple reactions;
the atomizing gas, the air curtain gas, the auxiliary gas and the collision gas are all high-purity nitrogen;
electrospray voltage (IS): 5500V;
atomizing gas (GS 1): 55 psi;
assist gas (GS 2): 50 psi;
air curtain gas (CUR): 25 psi;
ion source Temperature (TEM): 550 ℃;
biguanide octylamine monitoring quantitative ion pair (m/z): 178.7/100.0, declustering voltage (DP): 90V, Collision gas energy (CE): 19V, collision cell entrance voltage (EP): 10V;
biguanide octylamine monitoring qualitative ion pair (m/z): 178.7/128.1, declustering voltage (DP): 90V, Collision gas energy (CE): 27V, collision cell entrance voltage (EP): 10V.
6. The method of measuring according to claim 4,
in the LC-MS/MS measuring method described in the step (3),
the retention time of the iminoctadine is 1.56 min;
the regression equation for quantifying iminoctadine was 3250X +22000(Y is the peak area; X is the concentration in mg/kg).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110407215.5A CN112986460A (en) | 2021-04-15 | 2021-04-15 | Method for detecting residual quantity of iminoctadine tris in plant-derived food |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110407215.5A CN112986460A (en) | 2021-04-15 | 2021-04-15 | Method for detecting residual quantity of iminoctadine tris in plant-derived food |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112986460A true CN112986460A (en) | 2021-06-18 |
Family
ID=76340712
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110407215.5A Pending CN112986460A (en) | 2021-04-15 | 2021-04-15 | Method for detecting residual quantity of iminoctadine tris in plant-derived food |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112986460A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101133022A (en) * | 2004-07-12 | 2008-02-27 | 拜尔农作物科学股份公司 | Substituted 2-pyrrolidone derivatives as fungicides and insecticides |
| WO2012044650A1 (en) * | 2010-09-29 | 2012-04-05 | E. I. Du Pont De Nemours And Company | Fungicidal imidazoles |
-
2021
- 2021-04-15 CN CN202110407215.5A patent/CN112986460A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101133022A (en) * | 2004-07-12 | 2008-02-27 | 拜尔农作物科学股份公司 | Substituted 2-pyrrolidone derivatives as fungicides and insecticides |
| WO2012044650A1 (en) * | 2010-09-29 | 2012-04-05 | E. I. Du Pont De Nemours And Company | Fungicidal imidazoles |
Non-Patent Citations (7)
| Title |
|---|
| DREASSI ET AL.: "LC/ESI/MS Method for the Quantitative Detection of Guazatine Residues in Cereals", 《 J. AGRIC. FOOD CHEM.》 * |
| EMMANUEL ILESANMI ADEYEYE ET AL: "ASSESSMENT OF PESTICIDES RESIDUES IN WATER, SEDIMENT AND FISH PARTS: CASE STUDY OF FISH POND IN ADO-EKITI, NIGERIA", 《ASIAN JR. OF MICROBIOL. BIOTECH. ENV. SC.》 * |
| 吴珉等: "高效液相色谱法测定番茄与土壤中双胍三辛烷苯基磺酸盐残留量", 《农药》 * |
| 小林 憲弘等: "水道水中のイミノクタジン・ジクワット・パラコートLC/MS/MS一斉分析法の妥当性評価", 《環境科学会誌》 * |
| 小林裕子: "液体クロマトグラフィー/質量分析及び液体クロマトグラフィー/タンデム質量分析法による残留農薬分析", 《分析化学》 * |
| 李云飞等: "超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查食品中3种杀菌剂", 《食品科技》 * |
| 石守江等: "固相萃取-液相色谱法测定柑橘中百可得残留量", 《浙江农业科学》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111366652A (en) | Method for determining 16 mycotoxins in tea by using ultra-high performance liquid chromatography-tandem mass spectrometry | |
| CN108918711B (en) | Detection method of polyphenol compounds in tobacco leaves | |
| CN111912926A (en) | Method for determining reduced glutathione content in rice by ultra-high performance liquid chromatography-tandem mass spectrometry | |
| CN111289637B (en) | Method for detecting patulin in apple juice | |
| CN106990191A (en) | The method for detecting 7 kinds of sweeteners in fruit juice simultaneously using ultra performance liquid chromatography tandem mass spectrometry | |
| CN106706826A (en) | Analysis method of plant hormones in milligram-grade plants | |
| CN112014509A (en) | Method for synchronously determining angiotensin I and aldosterone in sample | |
| Chen et al. | Determination of ellagic acid in wine by solid-phase extraction–ultra-high performance liquid chromatography–tandem mass spectrometry | |
| CN108414643A (en) | The triple level four bars Mass Spectrometry detection methods of liquid chromatogram-of biogenic amine in a kind of cold freshly-slaughtered poultry | |
| CN112986460A (en) | Method for detecting residual quantity of iminoctadine tris in plant-derived food | |
| CN112649523A (en) | Method for detecting ustilagin A or ustilagin B in food | |
| CN108663464B (en) | Method for detecting fenhexamid in fruits, vegetables or soil | |
| CN111220722A (en) | Method for simultaneously determining 8 p-hydroxybenzoate compounds in soil | |
| CN109444293A (en) | The detection method of endogenous water-soluble B vitamin in a kind of fresh tobacco leaves | |
| CN111366643B (en) | Detection method of OLED material intermediate | |
| CN107515262B (en) | Liquid chromatography-mass spectrometry method for simultaneously determining lincomycin and gentamicin in animal plasma | |
| CN113433233A (en) | Centrifugal ultrafiltration-ion chromatography-triple quadrupole mass spectrometry detection method for ethephon in fruits and vegetables | |
| CN111272939A (en) | Method for determining penicillic acid content in fruits | |
| CN108896677A (en) | The method for quickly detecting metrafenone in water using LC-MS technology | |
| CN112198249A (en) | Detection method of ethanolamine compound in soil | |
| CN109324139A (en) | Ribosylzeatin liquid-liquid extraction-liquid chromatography-tandem mass spectrometry measuring method in a kind of tobacco leaf | |
| CN112305129B (en) | Method for detecting residual content of acarbose in mushroom dregs | |
| CN115144494B (en) | Method for detecting oligosaccharide in mammal milk | |
| CN113049705B (en) | UPLC-MS/MS detection method for T6P and Tre in fusarium graminearum | |
| CN110618212B (en) | Method for simultaneously detecting residual quantity of multiple plant growth regulators in vegetables |
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 |