CN114878720A - Method for determining impurities in pesticide boscalid - Google Patents
Method for determining impurities in pesticide boscalid Download PDFInfo
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- CN114878720A CN114878720A CN202210618864.4A CN202210618864A CN114878720A CN 114878720 A CN114878720 A CN 114878720A CN 202210618864 A CN202210618864 A CN 202210618864A CN 114878720 A CN114878720 A CN 114878720A
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- boscalid
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- 239000012535 impurity Substances 0.000 title claims abstract description 72
- 239000005740 Boscalid Substances 0.000 title claims abstract description 54
- WYEMLYFITZORAB-UHFFFAOYSA-N boscalid Chemical compound C1=CC(Cl)=CC=C1C1=CC=CC=C1NC(=O)C1=CC=CN=C1Cl WYEMLYFITZORAB-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229940118790 boscalid Drugs 0.000 title claims abstract description 54
- 239000000575 pesticide Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000013558 reference substance Substances 0.000 claims abstract description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 18
- 150000002500 ions Chemical group 0.000 claims abstract description 15
- 239000012452 mother liquor Substances 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000012488 sample solution Substances 0.000 claims abstract description 9
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 238000004817 gas chromatography Methods 0.000 claims abstract description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 14
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- 239000000523 sample Substances 0.000 claims description 7
- 239000012159 carrier gas Substances 0.000 claims description 6
- 239000003814 drug Substances 0.000 claims description 4
- LLPUJNYVYYGTEP-UHFFFAOYSA-N 2-chloro-n-(2-phenylphenyl)pyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1C1=CC=CC=C1 LLPUJNYVYYGTEP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 229940079593 drug Drugs 0.000 claims description 3
- 238000004949 mass spectrometry Methods 0.000 claims description 3
- 238000001819 mass spectrum Methods 0.000 abstract description 13
- 238000001514 detection method Methods 0.000 abstract description 5
- 239000006227 byproduct Substances 0.000 abstract description 4
- -1 compound ions Chemical class 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 6
- 230000014759 maintenance of location Effects 0.000 description 3
- DFPAKSUCGFBDDF-UHFFFAOYSA-N Nicotinamide Chemical compound NC(=O)C1=CC=CN=C1 DFPAKSUCGFBDDF-UHFFFAOYSA-N 0.000 description 2
- 150000001793 charged compounds Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 239000010413 mother solution Substances 0.000 description 2
- 239000012088 reference solution Substances 0.000 description 2
- 230000007017 scission Effects 0.000 description 2
- FOUDIDNRZBCJFZ-UHFFFAOYSA-N 2-chloro-n-(2-chlorophenyl)pyridine-3-carboxamide Chemical compound ClC1=CC=CC=C1NC(=O)C1=CC=CN=C1Cl FOUDIDNRZBCJFZ-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- TWFZGCMQGLPBSX-UHFFFAOYSA-N Carbendazim Natural products C1=CC=C2NC(NC(=O)OC)=NC2=C1 TWFZGCMQGLPBSX-UHFFFAOYSA-N 0.000 description 1
- 241000221785 Erysiphales Species 0.000 description 1
- 208000031888 Mycoses Diseases 0.000 description 1
- 206010034133 Pathogen resistance Diseases 0.000 description 1
- 239000005820 Prochloraz Substances 0.000 description 1
- 241000221662 Sclerotinia Species 0.000 description 1
- 241000219094 Vitaceae Species 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006013 carbendazim Substances 0.000 description 1
- JNPZQRQPIHJYNM-UHFFFAOYSA-N carbendazim Chemical compound C1=C[CH]C2=NC(NC(=O)OC)=NC2=C1 JNPZQRQPIHJYNM-UHFFFAOYSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 244000037666 field crops Species 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 235000021021 grapes Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229960003966 nicotinamide Drugs 0.000 description 1
- 235000005152 nicotinamide Nutrition 0.000 description 1
- 239000011570 nicotinamide Substances 0.000 description 1
- TVLSRXXIMLFWEO-UHFFFAOYSA-N prochloraz Chemical compound C1=CN=CN1C(=O)N(CCC)CCOC1=C(Cl)C=C(Cl)C=C1Cl TVLSRXXIMLFWEO-UHFFFAOYSA-N 0.000 description 1
- 235000013311 vegetables Nutrition 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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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)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to the technical field of pesticide detection, in particular to a method for determining impurities in a pesticide boscalid, which comprises the following steps: s1, respectively weighing boscalid impurity I and boscalid impurity II as reference substances, respectively preparing corresponding reference substance mother liquor 1 and reference substance mother liquor 2 by taking acetone as a solvent, and mixing in proportion to obtain an impurity mixed reference substance solution; s2, weighing the pesticide boscalid, and preparing a sample solution by using propanol as a solvent; and S3, respectively measuring the impurity mixed reference substance solution and the sample solution by using a gas chromatograph-mass spectrometer. According to the method, potential by-products and impurities of the boscalid are detected by using a gas chromatograph-mass spectrometer, a mixture of raw pesticide products is separated through gas chromatography, and the characteristics of high mass resolution and high sensitivity of a mass spectrometer are utilized to analyze and compare compound ions and ion fragments of a secondary mass spectrum, so that the impurity information contained in the boscalid pesticide can be accurately identified.
Description
Technical Field
The invention relates to the technical field of pesticide detection, in particular to a method for determining impurities in a pesticide boscalid.
Background
Boscalid (molecular formula C) 18 H 12 Cl 2 N 2 O) is a novel nicotinamide fungicide, which is active against almost all types of fungal diseases, is very effective in controlling powdery mildew, gray mold, sclerotinia, various rot diseases and the like, has resistant bacteria against other medicaments, has no cross resistance with carbendazim, prochloraz and the like, and is mainly used for controlling diseases of vegetables such as rape and the like, fruits such as grapes and field crops.
Impurities in the pesticide boscalid have certain influence on the quality of the boscalid, and a detection and analysis method for by-products and impurities possibly brought in the actual production of the pesticide is not determined in the industry at present, so that the impurities in the pesticide boscalid cannot be accurately detected.
Disclosure of Invention
The invention aims to provide a method for determining impurities in a pesticide boscalid, so as to solve the problems in the background technology.
The invention is realized by the following technical scheme:
a method for determining impurities in pesticide boscalid comprises the following steps:
s1, respectively weighing boscalid impurity I and boscalid impurity II as reference substances, respectively preparing corresponding reference substance mother liquor 1 and reference substance mother liquor 2 by taking acetone as a solvent, and mixing in proportion to obtain an impurity mixed reference substance solution;
s2, weighing a boscalid original drug, and preparing a sample solution by using propanol as a solvent;
s3, respectively measuring the impurity mixed reference substance solution and the sample solution by using a gas chromatograph-mass spectrometer;
wherein, the boscalid impurity I is 2-chloro-N- (2-chlorphenyl) nicotinamide, and the boscalid impurity II is N- ([1, 1' -biphenyl ] -2-yl) -2-chloronicotinamide, and the structural formula is as follows:
as a further scheme of the invention, in step S1, boscalid impurity I and boscalid impurity ii are respectively weighed as reference substances, dissolved by acetone and subjected to volume fixing, and the solutions subjected to volume fixing are respectively diluted by 5 times and mixed to obtain the impurity mixed reference substance solution.
As a further scheme of the invention, the gas chromatograph-mass spectrometer is characterized in that a DB-5ms capillary column (30m multiplied by 0.25mm multiplied by 0.25 mu m) is selected as a gas chromatographic column, and the chromatographic conditions are as follows: column head pressure is set to be 72.1kPa, He carrier gas (99.999%) is adopted, and the constant linear velocity of the carrier gas is 32.0 cm/s; split-flow sample injection, the sample injection amount is 1.0 mu L, and the split-flow ratio is 15.0.
Preferably, the temperature of the gas chromatographic column is gradually increased from 190 ℃ to 280 ℃, and the temperature of the sample inlet of the chromatographic column is set to be 270 ℃.
As a further scheme of the invention, in the gas chromatograph-mass spectrometer, an EI ion source is selected for mass spectrum detection, and the mass spectrum conditions are set as follows: the voltage of the ion source is set to be 70eV, the temperature of the ion source is set to be 250 ℃, the interface temperature is 230 ℃, the solvent cutting time is 4.0min, the scanning time is 4.75-15.0 min, and the scanning range is 45-500 amu.
Preferably, the purities of the reference boscalid impurity I and the reference boscalid impurity II are 98.0-99.0%.
Compared with the prior art, the invention has the beneficial effects that:
according to the method, potential by-products and impurities of the boscalid are detected by using a gas chromatograph-mass spectrometer, a mixture of raw pesticide products is separated through gas chromatography, and the characteristics of high mass resolution and high sensitivity of a mass spectrometer are utilized to analyze and compare compound ions and ion fragments of a secondary mass spectrum, so that the impurity information contained in the boscalid pesticide can be accurately identified.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used for describing the embodiments are briefly introduced below, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a total ion flow diagram of an impurity mixed reference solution in accordance with the present invention;
FIG. 2 is a mass spectrum of impurity I of boscalid as a reference substance of the invention;
FIG. 3 is a mass spectrogram of a reference substance boscalid impurity II of the invention;
FIG. 4 is a total ion flow diagram of the pesticide boscalid of the invention;
FIG. 5 is a mass spectrum of impurity I in the pesticide boscalid of the invention;
FIG. 6 is a mass spectrum diagram of an impurity II in the pesticide boscalid of the invention;
FIG. 7 is a schematic diagram showing the structural formula of impurity I and the cleavage mode of mass spectrum according to the present invention;
FIG. 8 is a schematic diagram showing the structural formula of impurity II and the cleavage mode of mass spectrum.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The materials used in the examples are readily available from commercial companies unless otherwise specified. Under the same operation condition, the retention time of the impurity I and the impurity II in the boscalid original drug is the same as that of a reference substance, and the relative peak intensity of each mass-to-charge ratio of the mass spectrum is also consistent.
The embodiment provides a method for determining impurities in a pesticide boscalid, which comprises the following steps:
s1, respectively weighing 0.012g of reference boscalid impurity I (the content is 99.0%) and 0.012g of reference boscalid impurity II (the content is 98.0%) in a 25mL volumetric flask, respectively adding acetone for dissolving and fixing the volume to obtain solutions with the numbers of I1A and I2A; accurately transferring 5mL of solutions with numbers I1A and I2A into corresponding 25mL volumetric flasks by using a pipette, respectively adding acetone to dissolve the solutions and fixing the volumes to obtain a reference mother solution 1 with the number I1B and a reference mother solution 2 with the number I2B; transferring 1mL of reference mother liquor 1 and 1mL of reference mother liquor 2 by using a pipette respectively, mixing the reference mother liquor and the reference mother liquor in a 25mL volumetric flask, diluting with acetone, and performing constant volume to obtain an impurity mixed reference solution;
s2, weighing 0.1g of pesticide boscalid in a 10mL volumetric flask, dissolving the pesticide boscalid in acetone serving as a solvent, and fixing the volume to prepare a sample solution;
s3, respectively measuring the impurity mixed reference substance solution and the sample solution by using a gas chromatograph-mass spectrometer, wherein:
the gas chromatographic column adopts a DB-5ms capillary column (30m multiplied by 0.25mm multiplied by 0.25 mu m), and the chromatographic conditions are as follows: column head pressure is set to be 72.1kPa, He carrier gas (99.999%) is adopted, and the constant linear velocity of the carrier gas is 32.0 cm/s; split-flow sample injection with sample injection amount of 1.0 μ L and split-flow ratio of 15.0. In addition, the inlet temperature of the column was set to 270 ℃, and the column temperature program was set to: 190 deg.C → 20 deg.C/min to 270 deg.C (maintaining for 9min) → 20 deg.C/min to 280 deg.C (maintaining for 1.5min), and the running time is 15 min.
EI ion source is selected for mass spectrometry, and the parameters are set as follows: the voltage of the ion source is set to be 70eV, the temperature of the ion source is set to be 250 ℃, the interface temperature is 230 ℃, the solvent cutting time is 4.0min, the scanning time is 4.75-15.0 min, and the scanning range is 45-500 amu.
According to the detection method, the impurity mixed reference substance solution and the sample solution are respectively measured to obtain a corresponding total ion flow diagram and a corresponding mass spectrogram.
As shown in attached fig. 1-6, the component with retention time of 5.1min is impurity I, the molecular ion peak is m/z 266, according to the reaction route, the impurities possibly generated and the fragment peak mass-to-charge ratio of the impurity spectrogram, the impurity I is N- (2-chlorophenyl) -2-chloronicotinamide, and the structural formula and the mass spectrum cracking mode are shown in fig. 7.
As shown in the attached figures 1-6, the component with retention time of 8.5min is impurity ii, the molecular ion peak is m/z 308, the impurity ii is N- ([1, 1' -biphenyl ] -2-yl) -2-chloronicotinamide according to the reaction route, the impurities possibly generated and the fragment peak mass-to-charge ratio of the impurity spectrogram, and the structural formula and the mass spectrum cracking mode are shown in fig. 8.
According to the method, by-products and impurities possibly existing in the pesticide boscalid are measured by using the gas chromatograph-mass spectrometer, and the impurity I, the impurity II and ion fragments of the secondary mass spectrum are analyzed and compared by using the gas chromatograph-mass spectrometer, so that the impurity information contained in the pesticide boscalid can be accurately identified.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (6)
1. A method for determining impurities in pesticide boscalid is characterized by comprising the following steps:
s1, respectively weighing boscalid impurity I and boscalid impurity II as reference substances, respectively preparing corresponding reference substance mother liquor 1 and reference substance mother liquor 2 by taking acetone as a solvent, and mixing in proportion to obtain an impurity mixed reference substance solution;
s2, weighing a boscalid original drug, and preparing a sample solution by using propanol as a solvent;
s3, respectively measuring the impurity mixed reference substance solution and the sample solution by using a gas chromatograph-mass spectrometer;
wherein, the boscalid impurity I is 2-chloro-N- (2-chlorphenyl) nicotinamide, and the boscalid impurity II is N- ([1, 1' -biphenyl ] -2-yl) -2-chloronicotinamide.
2. The method for determining the impurities in the pesticide boscalid according to claim 1, wherein in the step S1, boscalid impurity I and boscalid impurity II are respectively weighed as reference substances, dissolved by acetone and subjected to volume fixing, and the solutions subjected to volume fixing are respectively diluted by 5 times and mixed to obtain the impurity mixed reference substance solution.
3. The method for determining the impurities in the pesticide boscalid according to claim 1, characterized in that a DB-5ms capillary column (30m x 0.25mm x 0.25 μm) is used as a gas chromatography column in a gas chromatograph-mass spectrometer, and the chromatographic conditions are as follows: column head pressure is set to be 72.1kPa, He carrier gas (99.999%) is adopted, and the constant linear velocity of the carrier gas is 32.0 cm/s; split-flow sample injection with sample injection amount of 1.0 μ L and split-flow ratio of 15.0.
4. The method for determining the impurities in the pesticide boscalid according to claim 3, wherein the temperature of the gas chromatographic column is gradually increased from 190 ℃ to 280 ℃, and the temperature of the injection port of the chromatographic column is set to 270 ℃.
5. The method for determining the impurities in the pesticide boscalid according to claim 1, characterized in that EI ion sources are selected for mass spectrometry in a gas chromatograph-mass spectrometer, and the mass spectrometry conditions are set as follows: the voltage of the ion source is set to be 70eV, the temperature of the ion source is set to be 250 ℃, the interface temperature is 230 ℃, the solvent cutting time is 4.0min, the scanning time is 4.75-15.0 min, and the scanning range is 45-500 amu.
6. The method for determining the impurities in the pesticide boscalid according to claim 1, wherein the purity of the reference boscalid impurity I and the reference boscalid impurity II is 98.0-99.0%.
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| CN202210618864.4A CN114878720B (en) | 2022-05-31 | 2022-05-31 | Method for determining impurities in pesticide boscalid |
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