CN114166968A - Method for rapidly determining content of glyphosine in glyphosate by liquid chromatography - Google Patents
Method for rapidly determining content of glyphosine in glyphosate by liquid chromatography Download PDFInfo
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- CN114166968A CN114166968A CN202111435258.0A CN202111435258A CN114166968A CN 114166968 A CN114166968 A CN 114166968A CN 202111435258 A CN202111435258 A CN 202111435258A CN 114166968 A CN114166968 A CN 114166968A
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- glyphosine
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- OXHDYFKENBXUEM-UHFFFAOYSA-N glyphosine Chemical compound OC(=O)CN(CP(O)(O)=O)CP(O)(O)=O OXHDYFKENBXUEM-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000005562 Glyphosate Substances 0.000 title claims abstract description 27
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229940097068 glyphosate Drugs 0.000 title claims abstract description 27
- 238000004811 liquid chromatography Methods 0.000 title claims abstract description 24
- 238000001514 detection method Methods 0.000 claims abstract description 25
- 238000004458 analytical method Methods 0.000 claims abstract description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 60
- 239000012071 phase Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 230000014759 maintenance of location Effects 0.000 claims description 9
- 239000007791 liquid phase Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 238000003786 synthesis reaction Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 3
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 239000003643 water by type Substances 0.000 description 2
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 240000000111 Saccharum officinarum Species 0.000 description 1
- 235000007201 Saccharum officinarum Nutrition 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 108010051210 beta-Fructofuranosidase Proteins 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 235000011073 invertase Nutrition 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
Images
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
-
- 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
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
-
- 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
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
Abstract
The invention belongs to the field of chemical detection and analysis, and particularly relates to a method for rapidly determining the content of glyphosine in glyphosate by using a liquid chromatography method. The glyphosate sample containing the glyphosine is injected into liquid chromatography quickly, eluted through a mobile phase quickly, separated by a C18 reverse phase column and the content of the glyphosine is measured. By adopting the method, the content of the glyphosine can be safely, quickly and accurately measured by adopting the liquid chromatography, and timely and accurate data guidance is provided for adjusting the technological parameters of glyphosate production.
Description
Technical Field
The invention relates to the field of chemical detection and analysis, in particular to a method for rapidly determining the content of glyphosine in glyphosate by applying liquid chromatography.
Background
The glyphosate is a high-efficiency, low-toxicity and broad-spectrum biocidal herbicide, has a systemic conduction effect, and can quickly enter a plant conduction system to generate an effect by dissolving a wax layer on the surfaces of leaves, branches and stems of weeds so as to ensure that the weeds are exhausted and die. The glyphosine is also called ripening phosphorus and glycin, and has the chemical name: n, N-bis (phosphonomethyl) glycine, a ripener, inhibits the activity of sugarcane acid invertase. Raw material glycine is used in the production of glyphosate, glyphosine is a byproduct in glyphosate synthesis reaction, and process technical guidance and process parameter adjustment can be provided for glyphosate synthesis by measuring the content of glyphosine in glyphosate, so that the method for measuring and inventing the content of glyphosine in glyphosate is very important.
The present glyphosate determination uses the liquid chromatography of the national standard method, but the column in the method only can generate glyphosate peak and the glyphosine does not generate peak, so the invention selects proper mobile phase and chromatographic column, uses the liquid chromatography to determine the glyphosine, and obtains quick and accurate result
Disclosure of Invention
The invention provides a method for rapidly measuring the content of glyphosine in glyphosate by applying liquid chromatography. The content of the glyphosine can be accurately and quickly detected.
The technical scheme adopted by the invention is as follows:
a method for rapidly determining the content of glyphosine in glyphosate by using liquid chromatography is characterized by comprising the following steps:
(1) weighing 0.1g of a glyphosine standard sample, dissolving in a solvent, fixing the volume to a 100mL volumetric flask, adjusting parameters of liquid chromatography, respectively transferring 30 muL, 40 muL and 50 muL for liquid chromatography detection, establishing a chromatogram of the glyphosine, obtaining a chromatogram peak retention time range of the glyphosine in a peak area unit microvolt, and fitting a curve;
(2) weighing 0.1-0.2g of the synthesized glyphosate sample, dissolving the glyphosate sample with a solvent, fixing the volume to 100mL, performing liquid phase analysis and detection by adopting the parameters of the liquid chromatogram in the step (1), and establishing a chromatogram map of the glyphosine to obtain the chromatographic peak retention time range of the glyphosine; in the step, quantitative sample injection is carried out, and the sample amount is 40 microliters.
(3) And (3) calculating the content of the glyphosine in the sample according to the chromatographic peak retention time range of the glyphosine obtained in the step (2) and by comparing with the curve fitted in the step (1).
In the step (1) and (2), the solvent is a mixture of acetonitrile and water, wherein the volume ratio of the acetonitrile to the water is 6-9: 1-4, preferably in a volume ratio of 6: 4.
and (2) filling the prepared sample into a bottle in the steps (1) and (2), wherein the bottle is full without any gap, and then carrying out liquid phase detection. Wherein the liquid chromatography conditions in the step (1) and the step (2) are as follows:
a chromatographic column: c18 reversed phase column;
the sample injection system comprises a column temperature: normal temperature; flow rate: 1.0 mL/min;
the mobile phase is acetonitrile: 60 parts of water: 40;
the detection system comprises: detector PDA detector.
The method can easily analyze the content ratio of the glyphosine in the production sample, has accurate detection result, saves time and has high efficiency, and provides guidance for adjusting the production process.
The invention has the beneficial effects that:
1. the mobile phase used in the present invention is acetonitrile: water 6: 4 (i.e. acetonitrile 60ml, water 40ml) solution, the peak is faster and the peak-type falls off without tailing.
2. Diluting the sample by a certain multiple with a mobile phase, injecting the solution into a liquid chromatograph, and quickly and accurately separating and measuring the content of the glyphosine within 10 min. The detection method can finish the test within 10min, greatly shortens the detection time and improves the working efficiency.
3. The method is simple and easy to implement, and has high accuracy and precision.
Drawings
FIG. 1: the glyphosine standard chromatogram in example 1.
FIG. 2: the glyphosine chromatogram in example 2-1.
FIG. 3: the glyphosine chromatograms in examples 3-4.
FIG. 4: gammaglosphine chromatograms in examples 3-6.
Detailed Description
The invention is further illustrated by the following examples, but the scope of the invention as claimed is not limited to the scope of the examples.
Example 1
The method comprises the following steps of: liquid chromatograph (waters corporation);
a method for rapidly determining the content of glyphosine in glyphosate by using liquid chromatography comprises the following steps:
(1) 0.1088g of glyphosine standard sample is weighed and dissolved in a mobile phase (acetonitrile: water: 60:40), and the volume is determined to be 100mL volumetric flask. Taking 2mL of the solution with constant volume, then using the mobile phase to fix the volume to 100mL, and sequentially filling the prepared glyphosine standard solution which is well dissolved by the mobile phase into sample vials under the action of the mobile phase; adjusting parameters of liquid chromatography, quantitatively injecting the samples, wherein the injection volumes are respectively 30 mu l (3.264 mu g), 40 mu l (4.352 mu g) and 50 mu l (5.44 mu g), filling the samples in vials with different volumes, carrying out liquid phase analysis and detection without air to obtain chromatograms and peak areas of the glyphosine, wherein the peak areas are 1819491, 2404164 and 2958001 respectively, and the retention time range of the chromatographic peak of the glyphosine obtained by the peak area unit microvolt is fitted into a curve y which is 523212X + 116865;
(2) 0.1002g of glyphosate sample obtained by synthesis is weighed, the sample is dissolved by a mobile phase (the mobile phase is acetonitrile: water: 60:40), the volume is determined to be 100mL by the mobile phase, and the solution is carefully and quickly filled into a sample vial; adjusting parameters of liquid chromatography, quantitatively feeding 50 microliters of the sample, performing liquid phase analysis and detection, and continuously determining for six times to obtain a chromatogram and a peak area of the glyphosine and obtain a chromatographic peak retention time range of the glyphosine;
(3) and (3) calculating the content of the glyphosine in the sample according to the chromatographic peak retention time range of the glyphosine obtained in the step (2) and the curve fitted in the step (1), wherein the percentage of the content of the glyphosine in the production sample can be easily analyzed by the method, the detection result is accurate, time is saved, the efficiency is high, and guidance is provided for adjusting the production process.
The parameters of the liquid chromatogram in the step are as follows:
a chromatographic column: c18 reversed phase column;
a sample introduction system: column temperature: normal temperature; flow rate: 1.0 mL/min;
the mobile phase is acetonitrile: 60 parts of water: 40;
the detection system comprises: PDA detector
Specific data are shown in table 1 below:
TABLE 1 analysis of glyphosine content in Glyphosate
| | Sample | 1% |
| 1 | 2.06 | |
| 2 | 2.15 | |
| 3 | 2.02 | |
| 4 | 2.13 | |
| 5 | 2.18 | |
| 6 | 2.17 | |
| Mean value | 2.12 | |
| RSD/％ | 3.04 |
The glyphosine chromatogram is shown in figure 1, and as can be seen from the table 1, the liquid chromatography can rapidly and accurately detect the glyphosine content in the glyphosate, and the detection result is accurate, time-saving and high-efficiency. The method can provide guidance for workshop production process timely and accurately.
Example 2
Example 2-1: the procedure and conditions were the same as in example 1, except that the column was changed to Waters Spherisorb 5.0 μm SAX and the run time was extended to 30 min.
The results of these two different columns were selected as shown in FIG. 2. Under the same conditions, even if the running time is prolonged, the glyphosine standard sample does not generate a peak at all. Indicating that neither of these two different columns was able to separate the glyphosine sample.
Example 2-2: the method and conditions were the same as in example 1 except that the column was changed to Agilent ZORBAX Bonus-RP 5.0 μm and the running time was extended to 30 min. Similarly, no peak was observed, and detection was difficult.
Example 3
Example 3-1: the method and conditions are the same as those in example 1, and only in the detection process, the mobile phase acetonitrile: the volume ratio of water is 90: 10.
Example 3-2: the method and conditions are the same as those in example 1, and only in the detection process, the mobile phase acetonitrile: the volume ratio of water was 70: 30.
Examples 3 to 3: the method and conditions are the same as those in example 1, and only in the detection process, the mobile phase acetonitrile: the volume ratio of water was 50: 50.
Examples 3 to 4: the method and conditions are the same as those in example 1, and only in the detection process, the mobile phase acetonitrile: the volume ratio of water was 40: 60.
Examples 3 to 5: the method and conditions are the same as those in example 1, and only in the detection process, the mobile phase acetonitrile: the volume ratio of water was 35: 65.
Examples 3 to 6: the method and conditions are the same as those in example 1, and only in the detection process, the mobile phase acetonitrile: the volume ratio of water is 20: 80.
In examples 3-1 to 3-2, the glyphosine chromatograms were unchanged from those in FIG. 1, and the peak appearance times were substantially the same. In examples 3-4, the glyphosine standard chromatogram is shown in FIG. 3, and the glyphosine peak shape is greatly changed and the baseline instability occurs. The peak shape of example 3-3 was similar to that of example 3-4, and the baseline was unstable.
In examples 3 to 6, the glyphosine standard chromatogram is shown in FIG. 4, and the glyphosine peak shape is greatly changed, a bifurcation peak appears, and the tailing is serious. Examples 3-5 similar to examples 3-6, tailing was observed.
In conclusion, when the Eclipse Plus C185.0 μm chromatographic column is used, the glyphosine sample can achieve better separation effect when the acetonitrile proportion in the mobile phase is more than 60%. In order to save the use amount of acetonitrile, mobile phase acetonitrile is selected: the volume ratio of water is 60: 40.
the above-described embodiments are merely preferred embodiments of the present invention, and should not be construed as limiting the present invention, and features in the embodiments and examples in the present application may be arbitrarily combined with each other without conflict. The protection scope of the present invention is defined by the claims, and includes equivalents of technical features of the claims. I.e., equivalent alterations and modifications within the scope hereof, are also intended to be within the scope of the invention.
Claims (4)
1. A method for rapidly determining the content of glyphosine in glyphosate by liquid chromatography is characterized by comprising the following steps:
(1) weighing 0.1g of a glyphosine standard sample, dissolving in a solvent, fixing the volume to a 100mL volumetric flask, adjusting parameters of liquid chromatography, respectively transferring 30 muL, 40 muL and 50 muL for liquid chromatography detection, establishing a chromatogram of the glyphosine, obtaining a chromatogram peak retention time range of the glyphosine in a peak area unit microvolt, and fitting a curve;
(2) dissolving the glyphosate sample obtained by synthesis with a solvent, fixing the volume, performing liquid phase analysis and detection by adopting the parameters of the liquid chromatogram in the step (1), establishing a chromatogram of the glyphosine, and obtaining the chromatographic peak retention time range of the glyphosine;
(3) and (3) calculating the content of the glyphosine in the sample according to the chromatographic peak retention time range of the glyphosine obtained in the step (2) and by comparing with the curve fitted in the step (1).
2. The method for rapidly determining the content of glyphosine in glyphosate by liquid chromatography as claimed in claim 1, which is characterized in that: in the step (1) and (2), the solvent is a mixture of acetonitrile and water, wherein the volume ratio of the acetonitrile to the water is 6-9: 1-4.
3. The method for rapidly determining the content of glyphosine in glyphosate by liquid chromatography as claimed in claim 1, which is characterized in that: and (2) filling the prepared sample into a bottle in the steps (1) and (2), wherein the bottle is full without any gap, and then carrying out liquid phase detection.
4. The method for rapidly determining the content of glyphosine in glyphosate by liquid chromatography as claimed in claim 1, which is characterized in that:
the liquid chromatography conditions in the step (1) and the step (2) are as follows:
a chromatographic column: c18 reversed phase column;
the sample injection system comprises a column temperature: normal temperature; flow rate: 1.0 mL/min;
the mobile phase is acetonitrile: water = 60: 40;
the detection system comprises: detector PDA detector.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101648972A (en) * | 2009-09-08 | 2010-02-17 | 浙江新安化工集团股份有限公司 | Method for recycling glyphosate from glyphosate mother liquid |
| CN108680663A (en) * | 2018-04-26 | 2018-10-19 | 广东省生物工程研究所（广州甘蔗糖业研究所） | A kind of detection method of sugarcane glyphosate and its metabolin |
| CN113185548A (en) * | 2021-05-10 | 2021-07-30 | 浙江新安化工集团股份有限公司 | Glyphosate synthesis method for improving utilization rate of dimethyl phosphite |
| CN113336790A (en) * | 2021-06-02 | 2021-09-03 | 武汉工程大学 | Method for selectively separating and recovering glyphosine from glyphosate mother liquor |
-
2021
- 2021-11-29 CN CN202111435258.0A patent/CN114166968A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101648972A (en) * | 2009-09-08 | 2010-02-17 | 浙江新安化工集团股份有限公司 | Method for recycling glyphosate from glyphosate mother liquid |
| CN108680663A (en) * | 2018-04-26 | 2018-10-19 | 广东省生物工程研究所（广州甘蔗糖业研究所） | A kind of detection method of sugarcane glyphosate and its metabolin |
| CN113185548A (en) * | 2021-05-10 | 2021-07-30 | 浙江新安化工集团股份有限公司 | Glyphosate synthesis method for improving utilization rate of dimethyl phosphite |
| CN113336790A (en) * | 2021-06-02 | 2021-09-03 | 武汉工程大学 | Method for selectively separating and recovering glyphosine from glyphosate mother liquor |
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| Title |
|---|
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