CN102890128A - Detection method for twelve kinds of pyrethroids pesticide residues in capsanthin - Google Patents
Detection method for twelve kinds of pyrethroids pesticide residues in capsanthin Download PDFInfo
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Abstract
The invention discloses a detection method for twelve kinds of pyrethroids pesticide residues in capsanthin. The detection method comprises the following steps of: ultrasonically extracting the capsanthin with an extracting solvent and then separating an extract liquor to obtain a supernatant liquor; purifying the supernatant liquor by using a gel permeation chromatography, collecting target eluant, concentrating the target eluant until dry and then making the volume constant to obtain a sample solution; and measuring the sample solution by adopting a gas chromatography-tandem mass spectrum in a selected ion monitoring mode and quantifying with an external standard method. The method is used for processing the capsanthin by adopting a GPC (gel permeation chromatography) technology, so that most of macromolecular pigment matters are moved, interference of sample matrixes on measurement is lowered greatly; and the detection method is high in accuracy and strong in applicability for the capsanthin. The detection is carried out by adopting the gas chromatography-tandem mass spectrum and selecting the ion monitoring mode, so that the method has the advantages of high sensitivity and high automation degree, is easy and fast and is capable of detecting large batches of samples easily; and generated waste liquid can be recycled and reused so as to reduce the detection cost and reduce the environmental pollution.
Description
Technical field
The present invention relates to the residual detection method of a kind of food additives middle peasant, 12 kinds of residual detection methods of pyrethroid farming in especially a kind of capsanthin.
Background technology
Capsanthin is take paprika fruit as raw material, extraction and the peony oily liquids pigment that makes is a kind of natural colorant with fortification effect, and its principal ingredient is carotenoid.Because the natural colouring matter edible safety is high, and has physiologically active, capsanthin more and more is subject to people's favor.
Capsicum is the raw material that capsanthin is produced, and for ensureing and promote the normal growth of capsicum, peasant household can use all kinds of agricultural chemicals of desinsection, sterilization, kill harmful animal (or weeds), causes ubiquity residues of pesticides in the capsicum.These residues of pesticides continuous enrichment method in the extraction process of capsicum causes the extract product such as capsanthin to have potential safety hazard.
One of main remains of pesticide in capsicum and the pepper extract is pyrethroid pesticide.Pyrethroid pesticide has efficiently, wide spectrum, the relative characteristic such as low toxicity and biodegradation, have higher desinsection than organochlorine, organophosphorus insecticide and render a service, and consumption is few, the people is poisoned little, so in the world widespread use.But show that after deliberation pyrethroid pesticide has cumulative toxicity, the long-term low dose contact also can cause chronic disease.Therefore, various countries more and more pay attention to the residual monitoring in agricultural byproducts of such agricultural chemicals.In order to guarantee the edible safety of food additives capsanthin, improve China's food safety Regulation level, citizens is healthy, promote the development of capsanthin industry, study the residual detection method of pyrethroid farming in a kind of accurate, quick, sensitive capsanthin and be of great significance for the safety in production tool of monitoring and check capsanthin.
At present, relevant pyrethroid pesticide remained detection method is existing many, comprises High Performance Liquid Chromatography/Mass Spectrometry method, gas chromatography-mass spectrography, vapor-phase chromatography and gas chromatography-tandem mass spectrometry etc.Wherein more to research report pyrethroid pesticide remained in the food such as tobacco, tealeaves, fruits and vegetables, and there is not yet report for the research of pyrethroid pesticide remained detection in the food additives capsanthin.Because contain a large amount of pigments in the capsanthin, matrix is complicated, so directly use the detection method of pyrethroid in the above-mentioned food, matrix interference is very large, can't realize effective detection.Therefore, for the capsanthin characteristic, it is very crucial to develop specially the method that is applicable to the residual detection of multiple pyrethroid farming in the capsanthin.
Summary of the invention
The technical problem to be solved in the present invention provides 12 kinds of residual detection methods of pyrethroid farming in a kind of fast and accurately capsanthin.
For solving the problems of the technologies described above, the technical solution used in the present invention is: capsanthin is carried out ultrasonic extraction with extraction solvent, then extract is separated obtaining supernatant liquor; Described supernatant liquor adopts gel permeation chromatography to purify, and collection target eluent is concentrated into dried, uses the organic solvent constant volume again, obtains sample solution; Described sample solution adopts gas chromatography-tandem mass spectrum to measure under selection ion monitoring pattern, and external standard method is quantitative.
Extraction solvent of the present invention is cyclohexane and the ethyl acetate mixed solvent of volume ratio 50:50; Described organic solvent is methylene chloride, cyclohexane, isopropyl ether, normal hexane or acetone.The mobile phase that described gel permeation chromatography purifies is that volume ratio is cyclohexane and the ethyl acetate mixed solvent of 50:50; The flow velocity of described mobile phase is 5.0mL/min, and acquisition time is 9.0～13.0min.
GC conditions of the present invention is: chromatographic column is the low pole quartz capillary column, 250～300 ℃ of injector temperatures, and 250～300 ℃ of transmission line temperature, sample size is 1.0～5.0 μ L, flow rate of carrier gas is 0.5～1.2mL/min.Described low pole quartz capillary column is selected HP-5 MS quartz capillary column, HP-17 MS quartz capillary column or HP-5 DS quartz capillary column; Specification is length 30m, internal diameter 0.25mm, thickness 0.25 μ m.
The temperature programme condition of gas chromatography of the present invention is: 80 ℃ of initial temperatures keep 1min; Be warming up to 200 ℃ with 20 ℃/min speed, keep 10min; Be warming up to 260 ℃ with 20 ℃/min speed again, keep 15min.
Mass Spectrometer Method condition of the present invention is: ion source temperature is 230 ℃, and the solvent delay time is 3.0～11.0min.
Selection ion monitoring pattern of the present invention is: Biphenthrin monitoring ion is 181
*, 166,165; Fenpropathrin monitoring ion is 265
*, 208,181; Betacyfluthrin monitoring ion is 208
*, 197,181; Acrinathrin monitoring ion is 289
*, 247,208,181; Permethrin monitoring ion is 184
*, 183,165,163; Cyfloxylate monitoring ion is 226
*, 206,199,163; Cypermethrin monitoring ion is 208
*, 181,165,163; Silafluofene monitoring ion is 286
*, 258,179; Fenvalerate monitoring ion is 225
*, 181,167,152,125; S-fenvalerate monitoring ion is 225
*, 181,167,152,125; Taufluvalinate monitoring ion is 281
*, 250,181; Decis monitoring ion is 281
*, 253,209,181.
The ultrasonic extraction time of the present invention is 10～30min, and number of times is 1～3 time; Described extract adopts high speed freezing centrifuge to carry out centrifuging; The high speed freezing centrifuge rotating speed is 4000～10000r/min, and centrifugation time is 5～10min; Described target eluent adopts Rotary Evaporators or automatic Nitrogen evaporator to concentrate.
Capsanthin consumption of the present invention is 0.5～1.5g, and the consumption of described extraction solvent is 10～25mL, and the constant volume of described organic solvent is 1.0～5.0mL.
The beneficial effect that adopts technique scheme to produce is: gel permeation chromatography (GPC) is a kind of chromatographic technique that separates according to the solute molecule size, can remove greases a large amount of in the sample and pigment, have rapidly and efficiently, save the advantages such as solvent, easy robotization.Gas chromatography-tandem mass spectrum is selected ion monitoring mode detection technology, and accuracy is high.The present invention adopts the GPC purification techniques that the capsanthin sample is processed, and selects ion monitoring mode detection technology in conjunction with gas chromatography-tandem mass spectrum, has set up a kind of method that is applicable to 12 kinds of residual detections of pyrethroid farming in the capsanthin.
The present invention adopts GPC technical finesse capsanthin, has removed most large molecule colors, has greatly reduced the interference of sample substrate to 12 kinds of residual mensuration of pyrethroid farming, and the detection method accuracy is high, and is strong to the capsanthin applicability; The present invention adopts the GPC technology to select the ion monitoring mode detection in conjunction with gas chromatography-tandem mass spectrum, and method is highly sensitive, and whole process automation degree is high, and is easy, fast, is easy to realize that batch samples detects; The waste liquid that produces in the GPC decontamination process of the present invention can recycle, and reuses, and has reduced testing cost, has reduced environmental pollution.
Description of drawings
The present invention is further detailed explanation below in conjunction with the drawings and specific embodiments.
Fig. 1 is that the gas chromatography-mass spectrum of 12 kinds of pyrethroid pesticide compounds of the present invention standard substance is selected ion (SIM) monitoring chromatogram.
Embodiment
12 kinds of residual detection methods of pyrethroid farming adopt following equipment and test condition in this capsanthin: HP-5 MS quartz capillary column, HP-17 MS quartz capillary column and HP-5 DS quartz capillary column are selected by Agilent 7890A GC system, chromatographic column; The triple level Four bar of Agilent 7000 GC/MS/MS Mass Spectrometer Method; Lab Tech Cleanup800 gel permeation chromatograph is joined the decontaminating column of 300mm * 25mm BIO-Beads S-X3 filler; Agents useful for same is chromatographically pure; Gas chromatography temperature programme condition is: 80 ℃ of initial temperatures keep 1min; Be warming up to 200 ℃ with 20 ℃/min speed, keep 10min; Be warming up to 260 ℃ with 20 ℃/min speed again, keep 15min; Mass Spectrometer Method, monitoring pattern is for selecting the ion monitoring pattern.Computer system record chromatogram, with peak area as the signal response value, to 12 kinds of residual qualitative and quantitative analysis that carry out of pyrethroids farming.Wherein, Biphenthrin monitoring ion is 181
*, 166,165; Fenpropathrin monitoring ion is 265
*, 208,181; Betacyfluthrin monitoring ion is 208
*, 197,181; Acrinathrin monitoring ion is 289
*, 247,208,181; Permethrin monitoring ion is 184
*, 183,165,163; Cyfloxylate monitoring ion is 226
*, 206,199,163; Cypermethrin monitoring ion is 208
*, 181,165,163; Silafluofene monitoring ion is 286
*, 258,179; Fenvalerate monitoring ion is 225
*, 181,167,152,125; S-fenvalerate monitoring ion is 225
*, 181,167,152,125; Taufluvalinate monitoring ion is 281
*, 250,181; Decis monitoring ion is 281
*, 253,209,181.
Embodiment 1: 12 kinds of agricultural residual detection method implementation steps of pyrethroid are as described below in this capsanthin:
(1) typical curve: it is an amount of that precision is measured 12 kinds of pyrethroid farming residual standard storing solutions respectively, become with Fisher chromatographically pure normal hexane stepwise dilution that mass concentration is respectively 0.01,0.05,0.1,0.2,0.5, the series standard solution of 1.0mg/L, measure by above-mentioned test condition sample introduction, with 12 kinds of residual peak area Y of pyrethroid farming its mass concentration X is mapped respectively.
(2) sample extraction: accurately take by weighing 1.0g(and be accurate to 0.0001g)
=200 capsanthin samples add the cyclohexane that the 12.5mL volume ratio is 50:50-ethyl acetate mixed solvent in the 25mL volumetric flask, ultrasonic 15min, and number of times 2 times is cooled to room temperature, adds volume ratio and be the cyclohexane of 50:50-ethyl acetate mixed solvent constant volume.Extract is transferred in the centrifuge tube, with the centrifugal 5min of the rotating speed of 8000r/min, gets supernatant liquor with 0.45 μ m membrane filtration under 5 ℃, and filtrate is transferred in the GPC loading bottle.
(3) to detect wavelength be 254nm to GPC purified treatment: GPC, and mobile phase is the cyclohexane-ethyl acetate mixed solvent of volume ratio 50:50, and flow velocity is 5.0mL/min.Loading 2.0mL advances the GPC purified treatment, collects the efflux of 9.0～13.0min, and it is dried to use Rotary Evaporators to be concentrated in 40 ℃, is settled to 5.0mL with the acetone ultrasonic dissolution, solution with 0.22 μ m membrane filtration after sample introduction mensuration.
(4) gas chromatography-tandem mass spectrum detects: choose HP-5 MS quartz capillary column, temperature programme, 260 ℃ of injector temperatures, 260 ℃ of transmission line temperature, flow rate of carrier gas are 1.2mL/min, sample size 2.0 μ L, select the ion monitoring pattern, ion source temperature is 230 ℃, solvent delay 11.0min.Gas chromatography-tandem mass spectrum detects the agricultural residual chromatogram of 12 kinds of pyrethroids as shown in Figure 1, and the peak sequence of 12 kinds of pyrethroid pesticide compounds is followed successively by among Fig. 1: Biphenthrin, Fenpropathrin, betacyfluthrin, acrinathrin, Permethrin, cyfloxylate, cypermethrin, silafluofene, fenvalerate, S-fenvalerate, taufluvalinate, decis.
(5) replicate determination: adopt external standard method quantitative, right
=200 capsanthin samples are done 3 Duplicate Samples, and test number is A, B, C, calculate respectively 12 kinds of residual collimation relative standard deviations of pyrethroid farming, and analysis result sees Table 1; To one of them sample replication five times, calculate respectively 12 kinds of residual precision of pyrethroids farming, analysis result sees Table 2.
(6) recovery of standard addition: the standard solution in the step (1) is joined known pyrethroid farming residual content
In=200 capsanthins, test according to above-mentioned steps, this sample is done 10 replicate determinations continuously, average, calculate recovery of standard addition, experimental result sees Table 3.
In sum, this method is applicable to fully
12 kinds of residual detections of pyrethroid farming in=200 capsanthins.
Embodiment 2: 12 kinds of agricultural residual detection method implementation steps of pyrethroid are as described below in this capsanthin:
(1) typical curve: identical with embodiment 1.
(2) sample extraction: accurately take by weighing 0.5g(and be accurate to 0.0001g)
=50 capsanthin samples add the cyclohexane that the 10mL volume ratio is 50:50-ethyl acetate mixed solvent in the 10mL volumetric flask, ultrasonic 10min is cooled to room temperature, add volume ratio and be the cyclohexane of 50:50-ethyl acetate mixed solvent constant volume.Extract is transferred in the centrifuge tube, with the centrifugal 5min of the rotating speed of 4000r/min, gets supernatant liquor with 0.45 μ m membrane filtration under 5 ℃, and filtrate is transferred in the GPC loading bottle.
(3) to detect wavelength be 254nm to GPC purified treatment: GPC, and mobile phase is the cyclohexane-ethyl acetate mixed solvent of volume ratio 50:50, and flow velocity is 5.0mL/min.Loading 2.0mL advances the GPC purified treatment, collects the efflux of 9.0～13.0min, and it is dried to use Rotary Evaporators to be concentrated in 40 ℃, is settled to 2.0mL with the isopropyl ether ultrasonic dissolution, solution with 0.22 μ m membrane filtration after sample introduction mensuration.
(4) gas chromatography-tandem mass spectrum detects: choose HP-17 MS quartz capillary column, temperature programme, 250 ℃ of injector temperatures, 250 ℃ of transmission line temperature, flow rate of carrier gas are 1.0mL/min, sample size 1.0 μ L, select the ion monitoring pattern, ion source temperature is 230 ℃, solvent delay 8.0min.
(5) replicate determination: adopt external standard method quantitative, right
=50 capsanthin samples are done 3 Duplicate Samples, test number is A, B, C, calculate respectively 12 kinds of residual collimation relative standard deviations of pyrethroid farming, get Biphenthrin 1.1%, Fenpropathrin 2.6%, betacyfluthrin 1.7%, acrinathrin 5.7%, Permethrin 4.2%, cyfloxylate 3.9%, cypermethrin 5.2%, silafluofene 7.9%, fenvalerate 3.4%, S-fenvalerate 1.2%, taufluvalinate 5.0%, decis 4.6%.To one of them sample replication five times, calculate respectively 12 kinds of residual precision of pyrethroid farming, get Biphenthrin 1.3%, Fenpropathrin 2.1%, betacyfluthrin 1.9%, acrinathrin 5.1%, Permethrin 2.3%, cyfloxylate 4.4%, cypermethrin 5.4%, silafluofene 1.8%, fenvalerate 8.3%, S-fenvalerate 2.8%, taufluvalinate 6.0% and decis 6.2%.
(6) recovery of standard addition: the standard solution in the step (1) is joined known 12 kinds of pyrethroids farming residual content
In=50 capsanthins, test according to above-mentioned steps, this sample is done 10 replicate determinations continuously, average, calculate recovery of standard addition, get Biphenthrin 85～105%, Fenpropathrin 80～96%, betacyfluthrin 90～110%, acrinathrin 80～100%, Permethrin 89～106%, cyfloxylate 92～110%, cypermethrin 79～103%, silafluofene 94～106%, fenvalerate 83～110%, S-fenvalerate 80～105%, taufluvalinate 86～110% and decis 85～95%.
To sum up, this method is applicable to
12 kinds of residual detections of pyrethroid farming in=50 capsanthins.
Embodiment 3: 12 kinds of agricultural residual detection method implementation steps of pyrethroid are as described below in this capsanthin:
(1) typical curve: identical with embodiment 1.
(2) sample extraction: accurately take by weighing 1.5g(and be accurate to 0.0001g)
=50 capsanthin samples add the cyclohexane that the 25mL volume ratio is 50:50-ethyl acetate mixed solvent in the 25mL volumetric flask, ultrasonic 30min, and number of times 3 times is cooled to room temperature, adds volume ratio and be the cyclohexane of 50:50-ethyl acetate mixed solvent constant volume.Extract is transferred in the centrifuge tube, with the centrifugal 10min of the rotating speed of 10000r/min, gets supernatant liquor with 0.45 μ m membrane filtration under 5 ℃, and filtrate is transferred in the GPC loading bottle.
(3) to detect wavelength be 254nm to GPC purified treatment: GPC, and mobile phase is the cyclohexane-ethyl acetate mixed solvent of volume ratio 50:50, and flow velocity is 5.0mL/min.Loading 2.0mL advances the GPC purified treatment, collects the efflux of 9.0～13.0min, and it is dried to use Rotary Evaporators to be concentrated in 40 ℃, is settled to 1.0mL with the normal hexane ultrasonic dissolution, solution with 0.22 μ m membrane filtration after sample introduction mensuration.
(4) gas chromatography-tandem mass spectrum detects: choose HP-5 DS quartz capillary column, temperature programme, 300 ℃ of injector temperatures, 300 ℃ of transmission line temperature, flow rate of carrier gas are 0.5mL/min, sample size 5.0 μ L, select the ion monitoring pattern, ion source temperature is 230 ℃, solvent delay 3.0min.
(5) replicate determination: adopt external standard method quantitative, right
=50 capsanthin samples are done 3 Duplicate Samples, test number is A, B, C, calculate respectively 12 kinds of residual collimation relative standard deviations of pyrethroid farming, get Biphenthrin 1.1%, Fenpropathrin 2.3%, betacyfluthrin 1.2%, acrinathrin 5.8%, Permethrin 4.6%, cyfloxylate 3.0%, cypermethrin 6.0%, silafluofene 6.2%, fenvalerate 3.2%, S-fenvalerate 1.3%, taufluvalinate 5.7% and decis 1.0%.To one of them sample replication five times, calculate respectively 12 kinds of residual precision of chrysanthemum ester class farming, get Biphenthrin 1.5%, Fenpropathrin 2.8%, betacyfluthrin 1.2%, acrinathrin 5.7%, Permethrin 2.4%, cyfloxylate 4.8%, cypermethrin 5.1%, silafluofene 1.2%, fenvalerate 8.5%, S-fenvalerate 2.1%, taufluvalinate 2.6% and decis 6.6%.
(6) recovery of standard addition: the standard solution in the step (1) is joined known 12 kinds of pyrethroids farming residual content
In=50 capsanthins, test according to above-mentioned steps, this sample is done 10 replicate determinations continuously, average, calculate recovery of standard addition, get Biphenthrin 82～106%, Fenpropathrin 80～101%, betacyfluthrin 87～105%, acrinathrin 80～106%, Permethrin 85～110%, cyfloxylate 84～110%, cypermethrin 86～105%, silafluofene 92～107%, fenvalerate 81～111%, S-fenvalerate 85～102%, taufluvalinate 91～112% and decis 90～105%.
The methylene chloride, cyclohexane, isopropyl ether, normal hexane and the acetone that are used for constant volume in this detection method all can dissolve 12 kinds of pyrethroid pesticides, therefore above-mentioned solvent all can be used for constant volume obtaining sample solution, and does not affect gas chromatography-tandem mass spectrum in the mensuration of selecting under the ion monitoring pattern.
Claims (10)
1. 12 kinds of residual detection methods of pyrethroid farming in the capsanthin, it is characterized in that: capsanthin is carried out ultrasonic extraction with extraction solvent, then extract is separated obtaining supernatant liquor; Described supernatant liquor adopts gel permeation chromatography to purify, and collection target eluent is concentrated into dried, uses the organic solvent constant volume again, obtains sample solution; Described sample solution adopts gas chromatography-tandem mass spectrum to measure under selection ion monitoring pattern, and external standard method is quantitative.
2. residual detection methods of 12 kinds of pyrethroids farming in the capsanthin according to claim 1, it is characterized in that: described extraction solvent is cyclohexane and the ethyl acetate mixed solvent of volume ratio 50:50; Described organic solvent is methylene chloride, cyclohexane, isopropyl ether, normal hexane or acetone.
3. residual detection methods of 12 kinds of pyrethroids farming in the capsanthin according to claim 2, it is characterized in that: the mobile phase that described gel permeation chromatography purifies is that volume ratio is cyclohexane and the ethyl acetate mixed solvent of 50:50; The flow velocity of described mobile phase is 5.0mL/min, and acquisition time is 9.0～13.0min.
4. residual detection methods of 12 kinds of pyrethroids farming in the capsanthin according to claim 1, it is characterized in that, described GC conditions is: chromatographic column is the low pole quartz capillary column, 250～300 ℃ of injector temperatures, 250～300 ℃ of transmission line temperature, sample size is 1.0～5.0 μ L, and flow rate of carrier gas is 0.5～1.2mL/min.
5. residual detection methods of 12 kinds of pyrethroids farming in the capsanthin according to claim 4, it is characterized in that: described low pole quartz capillary column is selected HP-5 MS quartz capillary column, HP-17 MS quartz capillary column or HP-5 DS quartz capillary column; Specification is length 30m, internal diameter 0.25mm, thickness 0.25 μ m.
6. 12 kinds of residual detection methods of pyrethroid farming in the capsanthin according to claim 1 is characterized in that the temperature programme condition of described gas chromatography is: 80 ℃ of initial temperatures, maintenance 1min; Be warming up to 200 ℃ with 20 ℃/min speed, keep 10min; Be warming up to 260 ℃ with 20 ℃/min speed again, keep 15min.
7. residual detection methods of 12 kinds of pyrethroids farming in the capsanthin according to claim 1, it is characterized in that described Mass Spectrometer Method condition is: ion source temperature is 230 ℃, the solvent delay time is 3.0～11.0min.
8. residual detection methods of 12 kinds of pyrethroids farming in the capsanthin according to claim 1, it is characterized in that described selection ion monitoring pattern is: Biphenthrin monitoring ion is 181
*, 166,165; Fenpropathrin monitoring ion is 265
*, 208,181; Betacyfluthrin monitoring ion is 208
*, 197,181; Acrinathrin monitoring ion is 289
*, 247,208,181; Permethrin monitoring ion is 184
*, 183,165,163; Cyfloxylate monitoring ion is 226
*, 206,199,163; Cypermethrin monitoring ion is 208
*, 181,165,163; Silafluofene monitoring ion is 286
*, 258,179; Fenvalerate monitoring ion is 225
*, 181,167,152,125; S-fenvalerate monitoring ion is 225
*, 181,167,152,125; Taufluvalinate monitoring ion is 281
*, 250,181; Decis monitoring ion is 281
*, 253,209,181.
9. residual detection methods of 12 kinds of pyrethroids farming in the described capsanthin of any one according to claim 1-8, it is characterized in that: the described ultrasonic extraction time is 10～30min, number of times is 1～3 time; Described extract adopts high speed freezing centrifuge to carry out centrifuging; The high speed freezing centrifuge rotating speed is 4000～10000r/min, and centrifugation time is 5～10min; Described target eluent adopts Rotary Evaporators or automatic Nitrogen evaporator to concentrate.
10. residual detection methods of 12 kinds of pyrethroids farming in the described capsanthin of any one according to claim 1-8, it is characterized in that: described capsanthin consumption is 0.5～1.5g, the consumption of described extraction solvent is 10～25mL, and the constant volume of described organic solvent is 1.0～5.0mL.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113092406A (en) * | 2021-04-08 | 2021-07-09 | 晨光生物科技集团股份有限公司 | Method for quickly predicting capsanthin appearance quality change |
| CN113466371A (en) * | 2021-06-30 | 2021-10-01 | 黔西县黔希煤化工投资有限责任公司 | Method for measuring trace diisopropyl ether in phenol water |
| CN114441700A (en) * | 2021-12-24 | 2022-05-06 | 江苏赫尔斯检测技术有限公司 | Method for determining deltamethrin in water based on gas-mass linkage method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5286393A (en) * | 1976-01-12 | 1977-07-18 | Sumitomo Chemical Co | Gas chromatography for optical isomer in pyrethroid insecticide |
| CN101498692A (en) * | 2008-08-18 | 2009-08-05 | 通标标准技术服务（天津）有限公司 | Method for measuring pesticide residue quantity in leather |
| JP2009186435A (en) * | 2008-02-08 | 2009-08-20 | Tsumura & Co | Method of purifying residual agricultural chemicals in herbal medicine sample |
| CN101598707A (en) * | 2009-05-19 | 2009-12-09 | 烟台杰科检测服务有限公司 | The residual detection method of Multiple Pesticides in a kind of oil-containing food |
| CN101915809A (en) * | 2010-07-01 | 2010-12-15 | 王冬群 | Detection method of pyrethroid pesticide remained in rice |
| JP5045282B2 (en) * | 2007-07-11 | 2012-10-10 | 株式会社ツムラ | Purification method of pesticide residues in crude drug samples |
-
2012
- 2012-09-21 CN CN201210354090.5A patent/CN102890128B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5286393A (en) * | 1976-01-12 | 1977-07-18 | Sumitomo Chemical Co | Gas chromatography for optical isomer in pyrethroid insecticide |
| JP5045282B2 (en) * | 2007-07-11 | 2012-10-10 | 株式会社ツムラ | Purification method of pesticide residues in crude drug samples |
| JP2009186435A (en) * | 2008-02-08 | 2009-08-20 | Tsumura & Co | Method of purifying residual agricultural chemicals in herbal medicine sample |
| CN101498692A (en) * | 2008-08-18 | 2009-08-05 | 通标标准技术服务（天津）有限公司 | Method for measuring pesticide residue quantity in leather |
| CN101598707A (en) * | 2009-05-19 | 2009-12-09 | 烟台杰科检测服务有限公司 | The residual detection method of Multiple Pesticides in a kind of oil-containing food |
| CN101915809A (en) * | 2010-07-01 | 2010-12-15 | 王冬群 | Detection method of pyrethroid pesticide remained in rice |
Non-Patent Citations (4)
| Title |
|---|
| 《理化检验-化学分册》 20110630 杨晓凤 等 凝胶渗透色谱净化-气相色谱法测定茶叶中30种有机氯及菊酯类农药残留量 698-700 1-10 第47卷, 第6期 * |
| 吕庆 等: "GPC-GC 法测定辣椒粉中乙草胺农药残留", 《农药研究与应用》, vol. 15, no. 1, 28 February 2011 (2011-02-28), pages 24 - 26 * |
| 杨晓凤 等: "凝胶渗透色谱净化-气相色谱法测定茶叶中30种有机氯及菊酯类农药残留量", 《理化检验—化学分册》, vol. 47, no. 6, 30 June 2011 (2011-06-30), pages 698 - 700 * |
| 王明泰 等: "GPC净化处理在测定拟除虫菊酯残留量中的应用", 《印染》, no. 6, 31 December 2007 (2007-12-31), pages 37 - 40 * |
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