CN114994228A - Method for measuring residual quantity of pyrimethanil in vegetables and fruits - Google Patents
Method for measuring residual quantity of pyrimethanil in vegetables and fruits Download PDFInfo
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- CN114994228A CN114994228A CN202210437968.5A CN202210437968A CN114994228A CN 114994228 A CN114994228 A CN 114994228A CN 202210437968 A CN202210437968 A CN 202210437968A CN 114994228 A CN114994228 A CN 114994228A
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- ZLIBICFPKPWGIZ-UHFFFAOYSA-N pyrimethanil Chemical compound CC1=CC(C)=NC(NC=2C=CC=CC=2)=N1 ZLIBICFPKPWGIZ-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000005828 Pyrimethanil Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 16
- 235000013399 edible fruits Nutrition 0.000 title claims abstract description 15
- 235000013311 vegetables Nutrition 0.000 title claims abstract description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000001514 detection method Methods 0.000 claims abstract description 18
- 238000000605 extraction Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 6
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 5
- 239000000523 sample Substances 0.000 claims description 37
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 33
- 239000012086 standard solution Substances 0.000 claims description 20
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 18
- 239000012488 sample solution Substances 0.000 claims description 15
- 230000014759 maintenance of location Effects 0.000 claims description 12
- 239000000575 pesticide Substances 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000012521 purified sample Substances 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- 238000003556 assay Methods 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008014 freezing Effects 0.000 claims description 4
- 238000007710 freezing Methods 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 4
- 239000011550 stock solution Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 238000011002 quantification Methods 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 239000012071 phase Substances 0.000 description 16
- 240000008067 Cucumis sativus Species 0.000 description 3
- 235000010799 Cucumis sativus var sativus Nutrition 0.000 description 3
- 241000220324 Pyrus Species 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 235000014443 Pyrus communis Nutrition 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 235000012055 fruits and vegetables Nutrition 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004452 microanalysis Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 235000021017 pears Nutrition 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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Classifications
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- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
-
- 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
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- 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)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a method for measuring the residual amount of pyrimethanil in vegetables and fruits, which comprises the following steps: sample preparation, extraction, purification, measurement, qualitative analysis and quantitative analysis. According to the invention, by designing the ratio of the mobile phase methanol to the water and the time in the ultraviolet detector of the liquid chromatograph, the pyrimethanil residue in vegetables and fruits is measured, the minimum detection limit is 0.006mg/kg, the recovery rate range is 92.0-98.0%, the relative standard deviation range is 2.5-5.6%, the detection accuracy is high, the efficiency is high, and the cost is low.
Description
Technical Field
The invention relates to a pesticide determination method, and particularly relates to a determination method of pyrimethanil residue in vegetables and fruits.
Background
At present, GB 23200.8-2016 gas chromatography-mass spectrometry for measuring the residual quantity of 500 pesticides and related chemicals in fruits and vegetables in national food safety standard is adopted to measure the residual quantity of pyrimethanil in the fruits and vegetables, but a gas chromatography-mass spectrometry combined instrument is expensive, and meanwhile, equipment and consumables matched with a detection process have strict requirements on precision and high detection cost, and meanwhile, the minimum detection limit of the pyrimethanil in the existing detection method is only 0.0126mg/kg, so that the further detection requirements cannot be met.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the technical problems in the prior art, the invention aims to provide a method for measuring the residual amount of pyrimethanil, which has the advantages of low detection cost, accurate detection and high efficiency.
The technical scheme is as follows: the invention provides a method for measuring the residual amount of pyrimethanil in vegetables and fruits, which comprises the following steps:
(1) preparing a sample: crushing edible parts in the vegetable and fruit samples to prepare samples to be detected, and sealing and freezing the samples for later use;
(2) extraction: mixing a sample and acetonitrile, homogenizing, filtering by using filter paper to a colorimetric tube with a plug and containing 5-8g of sodium chloride, collecting filtrate, sealing and vibrating, standing at room temperature, and layering an acetonitrile phase and a water phase;
(3) purifying: absorbing the acetonitrile phase extracting solution, evaporating in a water bath until the acetonitrile phase extracting solution is nearly dry, taking methanol and dichloromethane as leacheate, purifying by using an amino column, fixing the volume by using methanol, and filtering by using a filter membrane to obtain the pyrimethanil residue to be detected;
(4) and (3) determination: respectively sucking the prepared standard solution and the purified sample by an automatic sample injector, injecting the standard solution and the purified sample into an ultraviolet detector of a liquid chromatograph, determining the nature of the sample by retention time, and comparing the peak area of the sample with the peak area of the standard sample for quantification;
(5) and (3) qualitative analysis: comparing the retention time of the pyrimethanil in the sample solution and the standard solution, and if the retention time difference of the pyrimethanil in the sample solution and the standard solution is within +/-0.02 min, determining that the pyrimethanil is pyrimethanil;
(6) quantitative analysis: the pyrimethanil content of the sample was calculated as follows:
x-the content of the pesticide in mg/kg, A-the area of the peak in the sample, A S Peak area in the Standard, V 1 Total volume of extraction solvent in mL, V 2 The total volume of extraction solution used for the assay is aspirated in mL, V 3 -the volumetric volume of the sample solution in mL, M-the mass of the sample in g, p-the mass concentration of the pesticide in the standard solution in mg/kg.
Further, the freezing temperature in the step (1) is-20 ℃ to-16 ℃.
Further, the filter membrane in the step (2) is an organic phase solvent membrane with the thickness of 0.22 μm.
Further, in the step (3), the volume ratio of methanol to dichloromethane is 5: 95.
further, the preparation of the standard solution in the step (4) is as follows: the pyrimethanil standard substance is weighed and prepared into 0.10mg/L single pesticide standard stock solution by methanol, and the stock solution is stored in a refrigerator below 18 ℃ below zero.
Further, the chromatographic conditions of the ultraviolet detector of the liquid chromatograph in the step (4) are as follows: a chromatographic column: XDB-C18, 5 μm, 4.6X 150mm, mobile phase: b is ultrapure water, C is methanol, and gradient elution is carried out: 0-6min, wherein B% is 55:45 and C% is 45; 7-13min, wherein B% and C% are 25: 75; 14-19min, wherein B% is 0: 100; 20-30min, wherein B% and C% are 55: 45; flow rate: 0.8mL/min, and a detection wavelength of 275 nm.
The invention principle is as follows: the ultraviolet detector of the liquid chromatograph is designed based on the principle that solute molecules absorb ultraviolet light, and the working principle of the ultraviolet detector is the Lambert-Beer law, namely when a beam of monochromatic light penetrates through the flow cell, if the mobile phase does not absorb the light, the absorption A is in direct proportion to the concentration C of the light absorption component and the optical path length L of the flow cell. The ultraviolet detector has high sensitivity, low noise, wide linear range and good selectivity, and is not sensitive to environmental temperature, mobile phase composition change and flow velocity fluctuation, so that the ultraviolet detector can be used for microanalysis of substances with small light absorption and low extinction coefficient.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: by designing the proportion and time of the mobile phase methanol and the water in the ultraviolet detector of the liquid chromatograph, the invention can realize the minimum detection limit of 0.006mg/kg, the recovery rate range of 92.0-98.0%, the relative standard deviation range of 2.5-5.6%, the relative standard deviation of less than 10%, high detection precision, high efficiency and low cost.
Drawings
FIG. 1 is a liquid chromatography peak chart of pyrimethanil in example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the following specific embodiments and the accompanying drawings.
Example 1: the method for measuring the residual amount of the pyrimethanil in the cucumber comprises the following steps:
(1) sample preparation
Taking a cucumber sample, removing non-edible parts, crushing by using a food conditioner to prepare a sample to be detected, putting the sample into a container, and sealing and storing at the temperature of between 20 ℃ below zero and 16 ℃ below zero for later use;
(2) extraction of
Accurately weighing 20.0g of cucumber sample into a 250mL triangular flask, adding 40mL of acetonitrile, homogenizing at high speed in a homogenizer for 2min, filtering with filter paper, collecting filtrate into a 100mL colorimetric tube with a plug and containing 8g of sodium chloride, collecting 30mL of filtrate, covering a cover, violently shaking for 1min, and standing at room temperature for 20min to separate an acetonitrile phase from a water phase;
(3) purification
Sucking 10mL of the extracting solution into a 100mL beaker by using a pipette, evaporating in a water bath until the extracting solution is nearly dry, purifying by using an amino column by using methanol and dichloromethane (5: 95) as eluent, metering the volume to 2.5mL by using methanol, and filtering by using a membrane to obtain the pyrimethanil residue to be detected;
(4) and (3) determination: 20 mu L0.10mg/L of standard solution and purified sample are sucked and injected into a liquid chromatograph ultraviolet detector, qualitative according to retention time, and quantitative according to comparison of sample peak area and standard peak area, and a chromatographic column: XDB-C18, 5 μm, 4.6X 150mm, mobile phase: b is ultrapure water, C is methanol, and gradient elution is carried out: 0-6min, wherein B% and C% are 55: 45; 7-13min, wherein B% and C% are 25: 75; 14-19min, wherein B% and C% are 0: 100; 20-30min, wherein B% and C% are 55: 45; flow rate: 0.8mL/min, and the detection wavelength is 275 nm;
(5) and (3) qualitative analysis: comparing the retention time of the pyrimethanil in the sample solution and the standard solution, and if the retention time difference of the pyrimethanil in the sample solution and the standard solution is within +/-0.02 min, determining that the pyrimethanil is pyrimethanil;
(6) quantitative analysis: the pyrimethanil content of the sample is calculated according to the following formula:
x-the content of the pesticide in mg/kg, A-the area of the peak in the sample, A S Peak area in the Standard, V 1 Total volume of extraction solvent in ml, V 2 The total volume of extraction solution used for the assay is aspirated in mL, V 3 The volume of the sample solution is determined by the volume of the sample solution, wherein the volume is determined by the unit of mL, the mass of the M sample is determined by the unit of g, rho, and the mass concentration of the pesticide in the standard solution is determined by the unit of mg/kg.
(7) Statistics of results
(8) Analysis of results
The precision of the invention is expressed by the relative standard deviation of the parallel test, and the accuracy is expressed by the recovery rate of the addition recovery. In the experiment, four pyrimethanil standard samples with concentration levels of 0.006mg/kg, 0.05mg/kg, 0.1mg/kg and 0.2mg/kg are added, the recovery rate ranges from 93.0% to 96.0%, and the relative standard deviation ranges from 2.7% to 4.9%, which shows that the pyrimethanil residue detection method has good accuracy and precision and can meet the measurement requirements of different pyrimethanil residue amounts.
Example 2: and (3) determining the residual amount of pyrimethanil in the pears:
(1) sample preparation
Taking a pear sample, removing non-edible parts, crushing by using a food conditioner to prepare a sample to be detected, putting the sample into a container, and storing at the temperature of between 20 ℃ below zero and 16 ℃ below zero for later use;
(2) extraction of
Accurately weighing 20.0g of pear sample, adding 40mL of acetonitrile into a 250mL triangular flask, homogenizing at high speed in a homogenizer for 1.5min, filtering by using filter paper, collecting filtrate into a 100mL colorimetric tube with a plug and containing 5g of sodium chloride, collecting 20mL of filtrate, covering a cover, violently shaking for 1min, and standing at room temperature for 15min to ensure that an acetonitrile phase and a water phase are layered;
(3) purification
Sucking 10mL of the extracting solution into a 100mL beaker by using a pipette, evaporating in a water bath until the extracting solution is nearly dry, purifying by using an amino column by using methanol and dichloromethane (5: 95) as eluent, metering the volume to 2.5mL by using methanol, and filtering by using a membrane to obtain the pyrimethanil residue to be detected;
(4) and (3) determination: 20 mu L0.10mg/L of standard solution and purified sample are sucked and injected into a liquid chromatograph ultraviolet detector, qualitative according to retention time, and quantitative according to comparison of sample peak area and standard peak area, and a chromatographic column: XDB-C18, 5 μm, 4.6X 150mm, mobile phase: b is ultrapure water, C is methanol, and gradient elution is carried out: 0-6min, wherein B% and C% are 55: 45; 7-13min, wherein B% and C% are 25: 75; 14-19min, wherein B% and C% are 0: 100; 20-30min, wherein B% and C% are 55: 45; flow rate: 0.8mL/min, and a detection wavelength of 275 nm. (ii) a
(5) And (3) qualitative analysis: comparing the retention time of the pyrimethanil in the sample solution and the standard solution, and if the retention time difference of the pyrimethanil in the sample solution and the standard solution is within +/-0.02 min, determining that the pyrimethanil is pyrimethanil;
(6) quantitative analysis: the pyrimethanil content of the sample was calculated as follows:
x-the content of the pesticide in mg/kg, A-the area of the peak in the sample, A S Peak area in the Standard, V 1 Total volume of extraction solvent in ml, V 2 The total volume of extraction solution used for the assay is aspirated in mL, V 3 The volume of the sample solution is determined by the volume of the sample solution, wherein the volume is determined by the unit of mL, the mass of the M sample is determined by the unit of g, rho, and the mass concentration of the pesticide in the standard solution is determined by the unit of mg/kg.
(7) Statistics of results
(8) Analysis of results
The precision of the invention is expressed by the relative standard deviation of the parallel test, and the accuracy is expressed by the recovery rate of the addition recovery. In the experiment, the pyrimethanil standard samples with four concentration levels of 0.006mg/kg, 0.05mg/kg, 0.1mg/kg and 0.2mg/kg are added, the recovery rate ranges from 92.0% to 98.0%, and the relative standard deviation ranges from 2.5% to 5.6%, which shows that the pyrimethanil residue detection method has good accuracy and precision and can meet the measurement requirements of different pyrimethanil residue amounts.
Comparative example 1: the difference from example 1 is that the chromatographic conditions are: a chromatographic column: XDB-C18, 5 μm, 4.6X 150mm, mobile phase: b is ultrapure water, C is methanol, and gradient elution is carried out: 0-5min, B% and C% being 40: 60; 6-11min, wherein B% and C% are 50: 50; 12-19min, wherein B% and C% are 20: 80; 20-30min, wherein B% and C% are 40: 60; flow rate: 1mL/min, and the detection wavelength is 275 nm.
Because the proportions of the mobile phases are different, the flow rate is 1mL/min, the flow rate is too high, the peak-off time is high, the sample peak and the impurity peak are overlapped and are not well separated, the problems that the peak-off separation effect is poor, the peak type is not normally distributed and has tailing and the like are caused, and the quantitative analysis result is influenced.
Claims (7)
1. A method for measuring the residual amount of pyrimethanil in vegetables and fruits is characterized by mainly comprising the following steps:
(1) preparing a sample: crushing edible parts in the vegetable and fruit samples to prepare samples to be detected, and sealing and freezing the samples for later use;
(2) extraction: mixing a sample to be tested with acetonitrile, homogenizing, filtering by using filter paper into a colorimetric tube with a plug and sodium chloride, collecting filtrate, sealing and oscillating, standing at room temperature, and layering an acetonitrile phase and a water phase;
(3) purifying: absorbing the extract of the acetonitrile phase, evaporating in water bath until the extract is nearly dry, taking methanol and dichloromethane as leacheate, purifying by using an amino column, metering the volume by using methanol, and filtering by using a filter membrane to obtain the residual amount of the pyrimethanil to be detected;
(4) and (3) determination: respectively sucking the prepared standard solution and the purified sample by an automatic sample injector, injecting the standard solution and the purified sample into an ultraviolet detector of a liquid chromatograph, determining the nature of the sample by retention time, and comparing the peak area of the sample with the peak area of the standard sample for quantification;
(5) and (3) qualitative analysis: comparing the retention time of the pyrimethanil in the sample solution and the standard solution, and if the retention time difference of the pyrimethanil in the sample solution and the standard solution is within +/-0.02 min, determining that the pyrimethanil is pyrimethanil;
(6) quantitative analysis: the pyrimethanil content of the sample is calculated according to the following formula:
x-the content of the pesticide in mg/kg, A-the area of the peak in the sample, A S Peak area in the Standard, V 1 Total volume of extraction solvent in mL, V 2 The total volume of extraction solution used for the assay is aspirated in mL, V 3 The volume of the sample solution is determined by the volume of the sample solution, wherein the volume is determined by the unit of mL, the mass of the M sample is determined by the unit of g, rho, and the mass concentration of the pesticide in the standard solution is determined by the unit of mg/kg.
2. The method for measuring the residual amount of pyrimethanil in vegetables and fruits according to claim 1, wherein the freezing temperature in the step (1) is from-20 ℃ to-16 ℃.
3. The method for measuring the residual amount of pyrimethanil in vegetables and fruits according to claim 1, wherein the filter membrane in the step (2) is a 0.22 μm organic solvent membrane.
4. The method for measuring the residual amount of pyrimethanil in vegetables and fruits according to claim 1, characterized in that the mass of sodium chloride in the step (2) is 5-8 g.
5. The method for measuring the residual amount of pyrimethanil in vegetables and fruits according to claim 1, wherein the volume ratio of methanol + dichloromethane in the step (3) is 5: 95.
6. the method for measuring the residual amount of pyrimethanil in vegetables and fruits according to claim 1, wherein the standard solution in the step (4) is prepared by: the pyrimethanil standard substance is weighed, and is prepared into 0.10mg/L single pesticide standard stock solution by using methanol, and the stock solution is stored in a refrigerator below 18 ℃.
7. The method for measuring the residual amount of pyrimethanil in vegetables and fruits according to claim 1, wherein the chromatographic conditions of the ultraviolet detector of the liquid chromatograph in the step (4) are as follows: and (3) chromatographic column: XDB-C18, 5 μm, 4.6X 150mm, mobile phase: b is ultrapure water, C is methanol, and gradient elution is carried out: 0-6min, wherein B% and C% are 55: 45; 7-13min, wherein B% and C% are 25: 75; 14-19min, wherein B% and C% are 0: 100; 20-30min, wherein B% and C% are 55: 45; flow rate: 0.8mL/min, and a detection wavelength of 275 nm.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008096320A (en) * | 2006-10-13 | 2008-04-24 | Nippon Flour Mills Co Ltd | Method for analyzing agricultural chemical using liquid chromatography-tandem mass spectrometry (lc-ms/ms) |
| CN102221589A (en) * | 2011-03-28 | 2011-10-19 | 中国水稻研究所 | Method for detecting residual quantity of pesticides in vegetable sample by utilizing liquid chromatogram-high resolution mass spectrometer |
| CN103512993A (en) * | 2013-10-12 | 2014-01-15 | 崔淑华 | Hot pepper and determining method for 96 pesticide residues in product of hot pepper |
| CN105974015A (en) * | 2016-05-07 | 2016-09-28 | 中国热带农业科学院农产品加工研究所 | Method for determining dimethomorph and gibberellin residual quantity of vegetables and fruits |
| CN109298111A (en) * | 2018-12-07 | 2019-02-01 | 昌邑市检验检测中心 | In fruits and vegetables a variety of agricultures it is residual and meanwhile detection method |
-
2022
- 2022-04-25 CN CN202210437968.5A patent/CN114994228A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008096320A (en) * | 2006-10-13 | 2008-04-24 | Nippon Flour Mills Co Ltd | Method for analyzing agricultural chemical using liquid chromatography-tandem mass spectrometry (lc-ms/ms) |
| CN102221589A (en) * | 2011-03-28 | 2011-10-19 | 中国水稻研究所 | Method for detecting residual quantity of pesticides in vegetable sample by utilizing liquid chromatogram-high resolution mass spectrometer |
| CN103512993A (en) * | 2013-10-12 | 2014-01-15 | 崔淑华 | Hot pepper and determining method for 96 pesticide residues in product of hot pepper |
| CN105974015A (en) * | 2016-05-07 | 2016-09-28 | 中国热带农业科学院农产品加工研究所 | Method for determining dimethomorph and gibberellin residual quantity of vegetables and fruits |
| CN109298111A (en) * | 2018-12-07 | 2019-02-01 | 昌邑市检验检测中心 | In fruits and vegetables a variety of agricultures it is residual and meanwhile detection method |
Non-Patent Citations (1)
| Title |
|---|
| 程文杰等: "高效液相色谱法测定黄瓜中嘧霉胺和烯酰吗啉农药残留" * |
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