CN104614460A - Detection method for glyphosate 2,4-D compounded agent - Google Patents
Detection method for glyphosate 2,4-D compounded agent Download PDFInfo
- Publication number
- CN104614460A CN104614460A CN201510048928.1A CN201510048928A CN104614460A CN 104614460 A CN104614460 A CN 104614460A CN 201510048928 A CN201510048928 A CN 201510048928A CN 104614460 A CN104614460 A CN 104614460A
- Authority
- CN
- China
- Prior art keywords
- glyphosate
- detection method
- content
- built agent
- detection
- 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
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a detection method for glyphosate 2,4-D compounded agent, belonging to the technical field of pharmaceutical analysis. The glyphosate content in the compounded agent is detected by adopting a national standard method and chromatographic conditions, and the 2,4-D content is detected by adopting the following HPLC chromatographic conditions: a chromatographic column, namely Eclipse XDB C18 is 4.6*150 mm, the detection wavelength is 190-380nm, a mobile phase, namely the ratio of methanol to a buffering solution is 1:0. 5-1:5, the flow rate is 1.0mL/min, the sample introduction quantity is 20 microL, and the column temperature is equal to room temperature. By applying the detection method provided by the invention, the glyphosate content and the 2,4-D content can be detected respectively. During the detection of 2,4-D, glyphosate does not have response or peak under the condition of the wavelength, and 2,4-D is completely separated from 4-bromophenol, and the main peak is obvious, so that the selectivity, the resolution and the sensitivity are high, the reproducibility is good, and data is accurate and reliable.
Description
Technical field
The invention belongs to Pharmaceutical Analysis technical field, be specifically related to a kind of detection method of glyphosate 2,4-D built agent.
Background technology
Glyphosate is the herbicide of same About Monsanto Chemicals exploitation.Also known as: glyphosate, agriculture reach (Roundup), careless dry phosphine, the sweet acid of phosphine.Glyphosate is a kind of non-selective, noresidue steriland herbicide, very effective to prennical root weeds, is widely used in rubber, mulberry, tea, orchard and sugarcane field.2,4-D is the abbreviation of 2,4-dichlorphenoxyacetic acid, and it is a kind of organic solvent of low toxicity, is often used to herbicide and plant growth regulator, and is widely used in raising fruit quality and extends the aspects such as fresh keeping time.Glyphosate 2,4-D is composite to be referred to add a certain amount of 2,4-D by specific technique in gyphosate solution, thus makes gyphosate solution effect more extensive.As a kind of novel built agent, the national detection method that this product is temporarily not relevant and standard.
Summary of the invention
For prior art Problems existing, the object of the invention is to the technical scheme that design provides a kind of detection method of glyphosate 2,4-D built agent.
The detection method of described a kind of glyphosate 2,4-D built agent, it is characterized in that this built agent glyphosate content adopts national standard method and chromatographic condition to detect, 2,4-D content adopts following HPLC chromatographic condition to detect:
Chromatographic column: Eclipse XDB C18 4.6 ﹡ 150mm;
Determined wavelength: 190 ~ 380nm;
Mobile phase: methyl alcohol: damping fluid=1:0.5 ~ 1:5;
Flow velocity: 1.0mL/min;
Sample size: 20 μ L;
Column temperature: room temperature;
Above-mentioned damping fluid is: take 0.27g potassium dihydrogen phosphate, and by the water-soluble solution of 970ml, by phosphoric acid solution adjust ph to 1.9, supersonic oscillations obtain for 10 minutes.
The detection method of described a kind of glyphosate 2,4-D built agent, is characterized in that in described HPLC, detecting device adopts UV-detector or diode array detector.
The detection method of described a kind of glyphosate 2,4-D built agent, is characterized in that described mobile phase is methyl alcohol: damping fluid=1:1 ~ 1:2.
The detection method of described a kind of glyphosate 2,4-D built agent, is characterized in that described chromatographic column is C18 packed column.
The detection method of described a kind of glyphosate 2,4-D built agent, is characterized in that described determined wavelength is 190 ~ 280nm.
Apply detection method of the present invention, glyphosate content and 2,4-D content can be measured respectively.Survey 2,4-D time, glyphosate is without respond not go out peak (see accompanying drawing 4 and accompanying drawing 5) under this wavelength condition, and 2,4-D is separated completely with 4-bromophenol, and main peak obviously, selectivity, resolution, highly sensitive, and favorable reproducibility, data accurately and reliably.4-bromophenol is wherein the internal standard compound of mensuration 2,4-D required in national standard.
When surveying glyphosate, glyphosate and 2,4-D are separated completely [glyphosate appearance time 11.9 minutes (see accompanying drawing 3), 2,4-D appearance time 32.8 minutes (see accompanying drawing 6)], glyphosate and 2,4-D are separated completely with this understanding, and main peak is obvious, selectivity, resolution, highly sensitive, favorable reproducibility, data accurately and reliably.
Accompanying drawing explanation
Fig. 1 is the composite chromatogram of detection method glyphosate 2,4-D described in embodiment 1.
Fig. 2 is in the detection method described in embodiment 52,4-D and 4-bromophenol chromatogram.
Fig. 3 is glyphosate normal chromatograms wavelength is 195nm.
Fig. 4 is glyphosate is the chromatogram at 280nm place at wavelength.
Fig. 5 is the chromatogram of glyphosate under 2,4-D testing conditions.
Fig. 6 is the chromatogram of 2,4-D under glyphosate testing conditions.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but technical scheme of the present invention is not limited in following embodiment.
Embodiment 1
Take the formulated samples containing glyphosate 0.10g, detect by Chinese glyphosate national standard method, the glyphosate content in composite with external standard method calculating glyphosate 2,4-D.
Take the formulated samples containing 2,4-D0.10g, be placed in 50mL volumetric flask, be diluted to scale with mobile phase, supersonic oscillations 10min makes sample dissolve, and cooling room temperature, shakes up.Be C18 packed column by chromatographic column Eclipse XDB C18 4.6 ﹡ 150mm(chromatographic column), determined wavelength is 280nm, mobile phase is methyl alcohol: damping fluid=1:1(damping fluid is: take 0.27g potassium dihydrogen phosphate, by the water-soluble solution of 970ml, by phosphoric acid solution adjust ph to 1.9, supersonic oscillations 10 minutes), flow velocity 1.0mL/min, sample size 20 μ L.Sample detection.In this embodiment, detector adopts UV-detector or diode array detector.Then accurately take 2,4-D standard specimen 0.1g, be placed in 50mL volumetric flask, be diluted to scale with mobile phase, supersonic oscillations 10min makes sample dissolve, and cooling room temperature, shakes up.By this method sample detection, with external standard method can calculate glyphosate 2,4-D composite in 2,4-D content be 1.6%.Utilize the method, 2,4-D appearance time 17 minutes, peak type is good, and post pressure, without significant change, can guarantee the detection of the composite content of glyphosate 2,4-D preferably.Its testing result as shown in Figure 1.
Embodiment 2
Take the formulated samples containing glyphosate 0.11g, detect by Chinese glyphosate national standard method, the glyphosate content in composite with external standard method calculating glyphosate 2,4-D.
Take the formulated samples containing 2,4-D0.11g, be placed in 50mL volumetric flask, be diluted to scale with mobile phase, supersonic oscillations 10min makes sample dissolve, and cooling room temperature, shakes up.By chromatographic column Eclipse XDB C18 4.6 ﹡ 150mm, determined wavelength is 270nm, mobile phase is methyl alcohol: damping fluid=1:0.5(damping fluid is: take 0.27g potassium dihydrogen phosphate, by the water-soluble solution of 970ml, by phosphoric acid solution adjust ph to 1.9, supersonic oscillations 10 minutes), flow velocity 1.0mL/min, sample size 20 μ L.Sample detection.Then accurately take 2,4-D standard specimen 0.1g, be placed in 50mL volumetric flask, be diluted to scale with mobile phase, supersonic oscillations 10min makes sample dissolve, and cooling room temperature, shakes up.By this method sample detection, with external standard method can calculate glyphosate 2,4-D composite in 2,4-D content be 1.6%.Utilize the method, 2,4-D appearance time 17 minutes, peak type is good, and post pressure, without significant change, can guarantee the detection of the composite content of glyphosate 2,4-D preferably.
Embodiment 3
Take the formulated samples containing glyphosate 0.12g, detect by Chinese glyphosate national standard method, the glyphosate content in composite with external standard method calculating glyphosate 2,4-D.
Take the formulated samples containing 2,4-D0.12g, be placed in 50mL volumetric flask, be diluted to scale with mobile phase, supersonic oscillations 10min makes sample dissolve, and cooling room temperature, shakes up.By chromatographic column Eclipse XDB C18 4.6 ﹡ 150mm, determined wavelength is 260nm, mobile phase is methyl alcohol: damping fluid=1:2(damping fluid is: take 0.27g potassium dihydrogen phosphate, by the water-soluble solution of 970ml, by phosphoric acid solution adjust ph to 1.9, supersonic oscillations 10 minutes), flow velocity 1.0mL/min, sample size 20 μ L.Sample detection.Then accurately take 2,4-D standard specimen 0.1g, be placed in 50mL volumetric flask, be diluted to scale with mobile phase, supersonic oscillations 10min makes sample dissolve, and cooling room temperature, shakes up.By this method sample detection, with external standard method can calculate glyphosate 2,4-D composite in 2,4-D content be 1.6%.Utilize the method, 2,4-D appearance time 17 minutes, peak type is good, and post pressure, without significant change, can guarantee the detection of the composite content of glyphosate 2,4-D preferably.
Embodiment 4
Take the formulated samples containing glyphosate 0.13g, detect by Chinese glyphosate national standard method, the glyphosate content in composite with external standard method calculating glyphosate 2,4-D.
Take the formulated samples containing 2,4-D 0.13g, be placed in 50mL volumetric flask, be diluted to scale with mobile phase, supersonic oscillations 10min makes sample dissolve, and cooling room temperature, shakes up.By chromatographic column Eclipse XDB C18 4.6 ﹡ 150mm, determined wavelength is 250nm, mobile phase is methyl alcohol: damping fluid=1:5(damping fluid is: take 0.27g potassium dihydrogen phosphate, by the water-soluble solution of 970ml, by phosphoric acid solution adjust ph to 1.9, supersonic oscillations 10 minutes), flow velocity 1.0mL/min, sample size 20 μ L.Sample detection.Then accurately take 2,4-D standard specimen 0.1g, be placed in 50mL volumetric flask, be diluted to scale with mobile phase, supersonic oscillations 10min makes sample dissolve, and cooling room temperature, shakes up.By this method sample detection, with external standard method can calculate glyphosate 2,4-D composite in 2,4D content be 1.6%.Utilize the method, 2,4-D appearance time 17 minutes, peak type is good, and post pressure, without significant change, can guarantee the detection of the composite content of glyphosate 2,4-D preferably.
Embodiment 5
Take the formulated samples containing 2,4-D 0.1g, take 4-bromophenol 0.1g, 2,4-D is placed in 250mL volumetric flask together with 4-bromophenol, is diluted to scale with mobile phase, supersonic oscillations 10min makes sample dissolve, and cooling room temperature, shakes up.By chromatographic column Eclipse XDB C18 4.6 ﹡ 150mm, determined wavelength is 280nm, mobile phase is methyl alcohol: damping fluid=1:1(damping fluid is: take 0.27g potassium dihydrogen phosphate, by the water-soluble solution of 970ml, by phosphoric acid solution adjust ph to 1.9, supersonic oscillations 10 minutes), flow velocity 1.0mL/min, sample size 20 μ L.Sample detection.Utilize the method, 2,4-D appearance time 17 minutes, 4-bromophenol appearance time 9.5 minutes, two peak degree of separation are good, and peak type is good, and post pressure is without significant change.Its testing result as shown in Figure 2.
Claims (5)
1. the detection method of glyphosate 2, a 4-D built agent, it is characterized in that this built agent glyphosate content adopts national standard method and chromatographic condition to detect, 2,4-D content adopts following HPLC chromatographic condition to detect:
Chromatographic column: Eclipse XDB C18 4.6 ﹡ 150mm;
Determined wavelength: 190 ~ 380nm;
Mobile phase: methyl alcohol: damping fluid=1:0.5 ~ 1:5;
Flow velocity: 1.0mL/min;
Sample size: 20 μ L;
Column temperature: room temperature;
Above-mentioned damping fluid is: take 0.27g potassium dihydrogen phosphate, and by the water-soluble solution of 970ml, by phosphoric acid solution adjust ph to 1.9, supersonic oscillations obtain for 10 minutes.
2. the detection method of a kind of glyphosate 2,4-D built agent as claimed in claim 1, is characterized in that in described HPLC, detecting device adopts UV-detector or diode array detector.
3. the detection method of a kind of glyphosate 2,4-D built agent as claimed in claim 1, is characterized in that described mobile phase is methyl alcohol: damping fluid=1:1 ~ 1:2.
4. the detection method of a kind of glyphosate 2,4-D built agent as claimed in claim 1, is characterized in that described chromatographic column is C18 packed column.
5. the detection method of a kind of glyphosate 2,4-D built agent as claimed in claim 1, is characterized in that described determined wavelength is 190 ~ 280nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510048928.1A CN104614460A (en) | 2015-01-30 | 2015-01-30 | Detection method for glyphosate 2,4-D compounded agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510048928.1A CN104614460A (en) | 2015-01-30 | 2015-01-30 | Detection method for glyphosate 2,4-D compounded agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104614460A true CN104614460A (en) | 2015-05-13 |
Family
ID=53149002
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510048928.1A Pending CN104614460A (en) | 2015-01-30 | 2015-01-30 | Detection method for glyphosate 2,4-D compounded agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104614460A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104880518A (en) * | 2015-05-19 | 2015-09-02 | 山东省产品质量检验研究院 | Method for detecting 2,4-dichlorphenoxyacetic acid in foliar fertilizer |
| CN104977389A (en) * | 2015-06-29 | 2015-10-14 | 中国科学院东北地理与农业生态研究所 | Glyphosate pesticide detection method based on nematode approach-avoidance behavior |
| CN106841466A (en) * | 2017-02-22 | 2017-06-13 | 厦门鉴科检测技术有限公司 | A kind of liquid chromatogram pre-column derivatization for detecting water glyphosate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102207495A (en) * | 2011-03-24 | 2011-10-05 | 深圳市谱尼测试科技有限公司 | Method for determining content of glyphosate in soils by using high performance liquid chromatography method |
| CN103149289A (en) * | 2013-02-06 | 2013-06-12 | 中国烟草总公司四川省公司 | Method for determining residual amount of 2, 4-D in tobacco |
| KR20140036734A (en) * | 2012-09-18 | 2014-03-26 | 한국과학기술연구원 | Method for analyzing acidic herbicides using isotope dilution and gas chromatography/tandem mass spectrometry |
-
2015
- 2015-01-30 CN CN201510048928.1A patent/CN104614460A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102207495A (en) * | 2011-03-24 | 2011-10-05 | 深圳市谱尼测试科技有限公司 | Method for determining content of glyphosate in soils by using high performance liquid chromatography method |
| KR20140036734A (en) * | 2012-09-18 | 2014-03-26 | 한국과학기술연구원 | Method for analyzing acidic herbicides using isotope dilution and gas chromatography/tandem mass spectrometry |
| CN103149289A (en) * | 2013-02-06 | 2013-06-12 | 中国烟草总公司四川省公司 | Method for determining residual amount of 2, 4-D in tobacco |
Non-Patent Citations (6)
| Title |
|---|
| GIINTHER DITZELMIILLER 等: "Isolation and characterization of a 2,4-dichlorophenoxyacetic acid-degrading soil bacterium", 《APPL MICROBIOL BIOTECHNOL》, vol. 31, no. 1, 31 July 1989 (1989-07-31), pages 93 - 96, XP035169396, DOI: doi:10.1007/BF00252535 * |
| N. V. CUONG 等: "Development of a dipstick immunoassay for quantitative determination of 2,4-dichlorophenoxyacetic acid in water, fruit and urine samples", 《FRESENIUS J ANAL CHEM》, vol. 364, no. 6, 31 July 1999 (1999-07-31), pages 584 - 589 * |
| 夏慧 等: "高效液相色谱法同时测定豆芽中2,4-二氯苯氧乙酸残留", 《扬州大学学报（农业与生命科学版）》, vol. 32, no. 4, 31 December 2011 (2011-12-31), pages 86 - 89 * |
| 李晋国 等: "高效液相色谱法检测水源中2,4-二氯苯氧乙酸的含量", 《光谱实验室》, vol. 28, no. 1, 31 January 2011 (2011-01-31), pages 348 - 351 * |
| 梅宝贵 等: "《中华人民共和国国家标准》", 24 August 2006, article "草甘膦水剂", pages: 1-6 * |
| 綦艳 等: "高效液相色谱法同时测定果蔬中多种防腐剂", 《现代食品科技》, vol. 29, no. 6, 15 June 2013 (2013-06-15), pages 1409 - 1412 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104880518A (en) * | 2015-05-19 | 2015-09-02 | 山东省产品质量检验研究院 | Method for detecting 2,4-dichlorphenoxyacetic acid in foliar fertilizer |
| CN104880518B (en) * | 2015-05-19 | 2016-04-20 | 山东省产品质量检验研究院 | A kind of method detecting 2,4-dichlorphenoxyacetic acids in foliar fertilizer |
| CN104977389A (en) * | 2015-06-29 | 2015-10-14 | 中国科学院东北地理与农业生态研究所 | Glyphosate pesticide detection method based on nematode approach-avoidance behavior |
| CN106841466A (en) * | 2017-02-22 | 2017-06-13 | 厦门鉴科检测技术有限公司 | A kind of liquid chromatogram pre-column derivatization for detecting water glyphosate |
| CN106841466B (en) * | 2017-02-22 | 2019-09-06 | 厦门鉴科检测技术有限公司 | A kind of liquid chromatogram pre-column derivatization detecting water glyphosate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104614466B (en) | The assay method of antiseptic in tobacco juice for electronic smoke | |
| CN101526509B (en) | Method for rapidly determining content of preservatives in condiment | |
| CN105021744A (en) | Method for measuring eight carbonyl compounds in electronic cigarette tobacco tar | |
| CN104614460A (en) | Detection method for glyphosate 2,4-D compounded agent | |
| CN105067728A (en) | Method for measuring solvent compositions in nicotine liquid by combining gas chromatography and mass spectrometry | |
| CN104655775B (en) | The assay method of 3-acetyl group-2,5-thioxene in a kind of edible essence spice | |
| CN105954442A (en) | Method for determining formaldehyde in electronic cigarette liquid | |
| CN106404933B (en) | Rice field greenhouse gases measurement method based on Paddy Soil Solutions | |
| CN103743844A (en) | Determination method of alcohol content in methanol | |
| CN103323419A (en) | Method for testing nicotine alkaloid in tobacco and tobacco products | |
| CN103776929B (en) | Method for detecting polyoxins B by high performance liquid chromatography method | |
| CN104198642B (en) | The detection method of chlorine Fampridine acid residues of pesticides in a kind of barley | |
| CN104007203B (en) | A kind of method measuring methyl anthranilate in essence and flavoring agent | |
| CN104237410A (en) | Detection method of substituted benzene in environmental water | |
| CN104865334B (en) | A kind of method detecting growth regulator in foliar fertilizer | |
| CN105628802A (en) | Method for determining volatile impurity of pharmaceutical grade ethanol | |
| CN104090042A (en) | Method for measuring safrole in mainstream smoke of cigarettes | |
| CN103698463B (en) | A kind of LC-MS/MS method analyzing three kinds of phenoxy carboxylic acid herbicides residual quantities in tobacco | |
| CN104897807B (en) | A kind of method applying triacontanol content in gas chromatographic detection foliar fertilizer | |
| CN103792301A (en) | Method for measuring content of epigoitrin in anti-virus granules | |
| CN103884796B (en) | Method for detecting total propionic acid content of hybrid feed additive | |
| CN106248820A (en) | The assay method of acrylic aldehyde in a kind of tobacco juice for electronic smoke | |
| CN104880518B (en) | A kind of method detecting 2,4-dichlorphenoxyacetic acids in foliar fertilizer | |
| CN105067743B (en) | A kind of ethyl chloride method in gas chromatography determination chlortetracycline hydrochloride | |
| CN104730188A (en) | Gas chromatography analysis method for rapidly detecting nitrous oxide greenhouse gas |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150513 |
|
| RJ01 | Rejection of invention patent application after publication |