CN112098564B - HPLC (high performance liquid chromatography) detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil - Google Patents
HPLC (high performance liquid chromatography) detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil Download PDFInfo
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- CKAPSXZOOQJIBF-UHFFFAOYSA-N hexachlorobenzene Chemical compound ClC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl CKAPSXZOOQJIBF-UHFFFAOYSA-N 0.000 title claims abstract description 100
- ONXPZLFXDMAPRO-UHFFFAOYSA-N decachlorobiphenyl Chemical group ClC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1C1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl ONXPZLFXDMAPRO-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 238000001514 detection method Methods 0.000 title claims abstract description 81
- CRQQGFGUEAVUIL-UHFFFAOYSA-N chlorothalonil Chemical compound ClC1=C(Cl)C(C#N)=C(Cl)C(C#N)=C1Cl CRQQGFGUEAVUIL-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000005747 Chlorothalonil Substances 0.000 title claims abstract description 60
- 238000004128 high performance liquid chromatography Methods 0.000 title claims abstract description 52
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000000034 method Methods 0.000 claims abstract description 45
- 239000000523 sample Substances 0.000 claims abstract description 36
- 239000012488 sample solution Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000012224 working solution Substances 0.000 claims abstract description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 28
- 239000011550 stock solution Substances 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 9
- 238000007865 diluting Methods 0.000 claims description 8
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- 238000009210 therapy by ultrasound Methods 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 12
- 238000000926 separation method Methods 0.000 abstract description 3
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- 238000012360 testing method Methods 0.000 description 5
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- PBKONEOXTCPAFI-UHFFFAOYSA-N 1,2,4-trichlorobenzene Chemical compound ClC1=CC=C(Cl)C(Cl)=C1 PBKONEOXTCPAFI-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000003085 diluting agent Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
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- 238000011002 quantification Methods 0.000 description 3
- RFFLAFLAYFXFSW-UHFFFAOYSA-N 1,2-dichlorobenzene Chemical compound ClC1=CC=CC=C1Cl RFFLAFLAYFXFSW-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
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- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
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- ZPQOPVIELGIULI-UHFFFAOYSA-N 1,3-dichlorobenzene Chemical compound ClC1=CC=CC(Cl)=C1 ZPQOPVIELGIULI-UHFFFAOYSA-N 0.000 description 1
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 1
- RMBFBMJGBANMMK-UHFFFAOYSA-N 2,4-dinitrotoluene Chemical compound CC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O RMBFBMJGBANMMK-UHFFFAOYSA-N 0.000 description 1
- XTRDKALNCIHHNI-UHFFFAOYSA-N 2,6-dinitrotoluene Chemical compound CC1=C([N+]([O-])=O)C=CC=C1[N+]([O-])=O XTRDKALNCIHHNI-UHFFFAOYSA-N 0.000 description 1
- 241000221785 Erysiphales Species 0.000 description 1
- 241000233679 Peronosporaceae Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- SPAKMVQVTSVXES-UHFFFAOYSA-N methanol;oxolane;hydrate Chemical compound O.OC.C1CCOC1 SPAKMVQVTSVXES-UHFFFAOYSA-N 0.000 description 1
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- 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
- G01N30/16—Injection
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- 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
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
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- 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
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- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
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Abstract
The invention provides an HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil, which comprises the following steps: and (3) carrying out HPLC detection on a to-be-detected sample solution prepared from a standard working solution prepared from a hexachlorobenzene and decachlorobiphenyl standard sample and a chlorothalonil sample by using water and acetonitrile as mobile phases and adopting a C18 reversed phase chromatographic column, and calculating according to a detection result to obtain the content of hexachlorobenzene and decachlorobiphenyl in the to-be-detected sample. The method provided by the invention can simultaneously detect hexachlorobenzene and decachlorobiphenyl in chlorothalonil at one time, and has the advantages of good separation effect, high sensitivity, high accuracy and high precision.
Description
Technical Field
The invention belongs to the field of analytical chemistry, particularly relates to an HPLC (high performance liquid chromatography) detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil, and particularly relates to a high-sensitivity HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil.
Background
Chlorothalonil, chemical name of tetrachloroisophthalonitrile, is a broad-spectrum protective bactericide with high efficiency and low toxicity, and is widely used for preventing and treating rust disease, anthracnose, powdery mildew and downy mildew on fruit trees and vegetables. Hexachlorobenzene and decachlorobiphenyl are byproduct impurities in the production process of chlorothalonil original drugs, and hexachlorobenzene and decachlorobiphenyl are harmful to human bodies, are difficult to degrade in natural environments and are easy to accumulate in organisms and in the environment. At present, methods for analyzing hexachlorobenzene and decachlorobiphenyl in chlorothalonil products are reported at home and abroad, wherein the method for analyzing hexachlorobenzene or decachlorobiphenyl in chlorothalonil is a liquid chromatography method for analyzing hexachlorobenzene or decachlorobiphenyl independently, and the methods for analyzing two impurities of hexachlorobenzene and decachlorobiphenyl simultaneously mainly comprise a gas chromatography-mass spectrometry method in an FAO standard and a liquid chromatography analysis method in a GB/T9551-2017 national standard. However, the reported methods have many defects, such as high detection sensitivity, good selectivity and good accuracy of gas chromatography-mass spectrometry, but the methods are difficult to popularize and use in domestic general enterprises due to expensive equipment and high analysis cost; GB/T9551-; the independent analysis method for respectively measuring hexachlorobenzene or decachlorobiphenyl in the chlorothalonil product has the disadvantages of troublesome operation and low analysis efficiency.
CN102680437A discloses a detection method of hexachlorobenzene. The method comprises the following steps: irradiating the ethanol solution polluted by the hexachlorobenzene by using ultraviolet light, and measuring the fluorescence emission spectrum intensity of the hexachlorobenzene in the hexachlorobenzene ethanol solution by using a fluorescence spectrometer to obtain the content of the hexachlorobenzene; the above-mentionedThe wavelength range of the ultraviolet light is 340-380 nm, the wavelength of the ultraviolet light is 360nm, and the concentration of hexachlorobenzene in the hexachlorobenzene ethanol solution is 10-14-10-7M, the concentration of hexachlorobenzene in the hexachlorobenzene ethanol solution is preferably 1 x 10-9-8×10-9And M. The detection method can be used for quickly and effectively detecting trace hexachlorobenzene with high sensitivity; the method can be widely applied to the rapid trace detection of hexachlorobenzene in environment, medicine, food and biological samples. But the detection by adopting the fluorescence spectroscopy has higher requirement on detection aging.
CN110579557A discloses an HPLC analysis detection method for simultaneously detecting 12 monocyclic aromatic hydrocarbons in water, belonging to the technical field of high performance liquid chromatography analysis. The method comprises the steps of firstly preparing reference solutions of 12 monocyclic aromatic hydrocarbons, namely chlorobenzene, o-dichlorobenzene, m-dichlorobenzene, p-dichlorobenzene, hexachlorobenzene, 1,2, 4-trichlorobenzene, benzene, toluene, ethylbenzene, nitrobenzene, 2, 4-dinitrotoluene and 2, 6-dinitrotoluene, then extracting an actual water sample for later use, and finally detecting the content of the 12 monocyclic aromatic hydrocarbons by adopting a liquid chromatography-diode array detector (HPLC-PDA). The method optimizes the leacheate, gradient leaching conditions, detection wavelength, sample injection amount and the like, finally establishes a proper analysis method, can achieve better separation of all substances, has the remarkable advantages of good reproducibility, high accuracy and high precision, lays a good foundation for simultaneous online monitoring of the monocyclic aromatic hydrocarbon in the water, and can effectively save detection cost and time. However, the method cannot be used for simultaneously detecting hexachlorobenzene and decachlorobiphenyl.
The content of hexachlorobenzene and decachlorobiphenyl in chlorothalonil was determined by means of a Waters 2998 high performance liquid chromatograph (equipped with a Waters Symmetry C18 stainless steel chromatographic column) using methanol-tetrahydrofuran-water as a mobile phase at a wavelength of 217 nm. Within the range of 0.05-2.0 mg/L, the linear relation between hexachlorobenzene and deca-chlorobiphenyl is good, the average recovery rate is 98.5 percent and 97.9 percent, and the relative standard deviation of hexachlorobenzene is 3.4 percent. The method can rapidly and accurately determine the content of hexachlorobenzene and decachlorobiphenyl in chlorothalonil. However, the method has the possibility of missing detection of low-content hexachlorobenzene and decachlorobiphenyl. (the high performance liquid chromatography of the red, precious plum, lina. the pesticide of hexachlorobenzene and decachlorobiphenyl [ J ]. in chlorothalonil, 2015,054(002):103-
The problem that the method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl is low in sensitivity and selectivity exists at present, so that how to provide the method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl with high sensitivity and good selectivity becomes a problem to be solved urgently.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an HPLC (high performance liquid chromatography) detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil, and particularly provides an HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil with high sensitivity. The method provided by the invention has the advantages of high analysis efficiency, high sensitivity, good selectivity, high precision and high accuracy.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a High Performance Liquid Chromatography (HPLC) detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil, which comprises the following steps: and (3) carrying out HPLC detection on a to-be-detected sample solution prepared from a standard working solution prepared from a hexachlorobenzene and decachlorobiphenyl standard sample and a chlorothalonil sample by using water and acetonitrile as mobile phases and adopting a C18 reversed phase chromatographic column, and calculating according to a detection result to obtain the content of hexachlorobenzene and decachlorobiphenyl in the to-be-detected sample.
The method provided by the invention can simultaneously detect the contents of hexachlorobenzene and decachlorobiphenyl in chlorothalonil at one time, thereby improving the analysis efficiency; and the detection cost can be reduced by adopting an HPLC detection method.
Preferably, the preparation method of the standard working solution comprises the following steps: putting hexachlorobenzene and deca-chlorobiphenyl standard samples into a volumetric flask, and performing constant volume by using a solvent to obtain a standard stock solution; and (4) diluting the standard stock solution to obtain a standard working solution.
Preferably, the mass ratio of hexachlorobenzene to decachlorobiphenyl in the standard stock solution is 1:0.8 to 1:1.2, such as 1:0.8, 1:0.85, 1:0.9, 1:0.95, 1:1, 1:1.05, 1:1.1, 1:1.15 or 1:1.2, but not limited to the ratios listed, and other ratios not listed within the ranges of the ratios above are equally applicable.
Preferably, the solvent comprises acetone.
The acetone has better solubility for chlorothalonil and impurities of hexachlorobenzene and decachlorobiphenyl, has no interference on the measurement of hexachlorobenzene and decachlorobiphenyl in a sample, and can improve the accuracy and sensitivity of detection.
Preferably, the standard stock solution has a concentration of 0.15-0.25mg/mL, such as 0.15mg/mL, 0.16mg/mL, 0.17mg/mL, 0.18mg/mL, 0.19mg/mL, 0.2mg/mL, 0.21mg/mL, 0.22mg/mL, 0.23mg/mL, 0.24mg/mL, or 0.25mg/mL, but is not limited to the recited values, and other non-recited values within the above-recited ranges are equally applicable.
Preferably, the standard stock solution is diluted by a dilution factor of 500-2000, such as 500, 600, 700, 800, 900, 1000, 1100, 1200, 1300, 1400, 1500, 1600, 1700, 1800, 1900, 2000, etc., but not limited to the recited values, and other values not recited in the above ranges are also applicable.
The specific dilution multiple can dilute the standard stock solution into the standard working solution with the content of hexachlorobenzene and decachlorobiphenyl close to that of hexachlorobenzene and decachlorobiphenyl in the sample solution to be detected, so that the detection result is more accurate.
Preferably, the preparation method of the sample solution to be tested comprises the following steps: diluting a chlorothalonil sample with a solvent, dissolving the chlorothalonil sample by vibration under ultrasonic waves, and cooling to obtain the sample solution to be detected.
Preferably, the solvent comprises acetone.
The acetone has better solubility to chlorothalonil and impurity components, and can improve the sensitivity of a detection result.
Preferably, the frequency of the ultrasound is 35-40 kHz.
Preferably, the time of the ultrasound is 6-10 min.
Preferably, the cooling is to a temperature of 20-30 ℃.
Preferably, the chlorothalonil sample is diluted with acetone by a dilution factor of 8-12.
The frequency may be 35kHz, 35.5kHz, 36kHz, 36.5kHz, 37kHz, 37.5kHz, 38kHz, 38.5kHz, 39kHz, 39.5kHz or 40kHz, the time may be 6min, 6.5min, 7min, 7.5min, 8min, 8.5min, 9min, 9.5min or 10min, the temperature may be 20 ℃, 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃, 26 ℃, 7 ℃, 28 ℃, 29 ℃ or 30 ℃ and the like, the dilution factor may be 8, 8.5, 9, 9.5, 10, 10.5, 11, 11.5 or 12 and the like, but is not limited to the recited values, and other values not recited in the above ranges of values are also applicable.
The combination of the specific parameters can accurately prepare the sample solution, and the accuracy of the detection result is improved.
Preferably, the concentration of the sample solution to be tested is 9-15mg/mL, such as 9mg/mL, 10mg/mL, 11mg/mL, 12mg/mL, 13mg/mL, 14mg/mL or 15mg/mL, but not limited to the recited values, and other values not recited in the above numerical ranges are also applicable.
Preferably, the specification of the C18 reversed phase chromatographic column is 150 x 4.6mm, and the particle size of the packing is 5 μm.
Preferably, the column temperature of the C18 reverse phase chromatographic column is 30-40 ℃.
Preferably, in the HPLC detection, the detection wavelength is 212-220 nm.
Preferably, the flow rate of the column in the HPLC assay is 0.8-1.2 mL/min.
Preferably, the sample amount in the HPLC detection is 10-20 μ L.
Wherein the column temperature may be 30 ℃, 31 ℃, 32 ℃, 33 ℃, 34 ℃, 35 ℃, 36 ℃, 37 ℃, 38 ℃, 39 ℃ or 40 ℃ or the like, the detection wavelength may be 212nm, 213nm, 214nm, 215nm, 216nm, 217nm, 218nm, 219nm or 220nm or the like, the flow rate may be 0.8mL/min, 0.85mL/min, 0.9mL/min, 0.95mL/min, 1mL/min, 1.05mL/min, 1.1mL/min, 1.15mL/min or 1.2mL/min or the like, the amount of the sample may be 10. mu.L, 11. mu.L, 12. mu.L, 13. mu.L, 14. mu.L, 15. mu.L, 16. mu.L, 7. mu.L, 18. mu.L, 19. mu.L or 20. mu.L or the like, but is not limited to the recited values, and other values not recited in the above-recited ranges are also applicable.
Preferably, the initial volume ratio of water to acetonitrile in the mobile phase is (7-9): (91-93), such as 7:93, 7.5:92.5, 8:92, 8.5:91.5, or 9:91, but is not limited to the recited values, and other unrecited values within the above numerical ranges are equally applicable.
The mobile phase volume ratio of the specific parameters can effectively separate hexachlorobenzene, decachlorobiphenyl and other interfering substances in the sample solution to be detected, shorten the analysis time and improve the precision and the accuracy of detection.
As a preferred technical solution of the present invention, the HPLC detection employs gradient elution, which is performed according to the following procedure: at 0-5min, the volume of water in the mobile phase accounts for 8%, and the volume of acetonitrile accounts for 92%; the volume ratio of water in the mobile phase is decreased at the speed of 8%/min at the 5 th min, the volume ratio of acetonitrile is increased at the speed of 8%/min, and the mobile phase is pure acetonitrile at the 6 th min and is continued for the 12 th min; and the volume ratio of water in the mobile phase is increased at the speed of 8%/min at the 12 th min, the volume ratio of acetonitrile is decreased at the speed of 8%/min, and the volume ratio of water in the mobile phase is 8% and the volume ratio of acetonitrile is 92% at the 13 th min, and the process is continued until the 16 th min.
| Time (min) | Water (%) | Acetonitrile (%) |
| 0 | 8 | 92 |
| 5 | 8 | 92 |
| 6 | 0 | 100 |
| 12 | 0 | 100 |
| 13 | 8 | 92 |
| 16 | 8 | 92 |
By adopting the gradient elution procedure, hexachlorobenzene, decachlorobiphenyl and other interfering substances in the sample solution to be detected can be effectively separated, the analysis time is shortened, and the precision, accuracy and sensitivity of detection are improved.
Compared with the prior art, the invention has the following beneficial effects:
according to the HPLC detection method, gradient elution is adopted, and the parameters of HPLC detection are optimized, so that the HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil has the advantages of good separation effect and high precision, the standard deviation range of the hexachlorobenzene content reaches below 0.21mg/kg, the coefficient of variation reaches below 2.5%, the standard deviation range of the decachlorobiphenyl content reaches below 0.16mg/kg, and the coefficient of variation reaches below 3.3%; the accuracy is high, the average recovery rate of the hexachlorobenzene standard reaches 100.8 percent, and the average recovery rate of the decachlorobiphenyl standard reaches 99.8 percent; the sensitivity is high, the detection limit of hexachlorobenzene by the method reaches 0.003 mu g/ml, the quantitative limit of the method reaches 0.006 mu g/ml, the detection limit of decachlorobiphenyl by the method reaches 0.005 mu g/ml, and the quantitative limit of the method reaches 0.010 mu g/ml; and hexachlorobenzene and decachlorobiphenyl are detected simultaneously, so that the detection efficiency is improved.
Drawings
FIG. 1 is an HPLC chart of the first standard working solution of example 1, in which 1-hexachlorobenzene, 2-decachlorobiphenyl;
FIG. 2 is a HPLC chart of the first sample solution to be tested in example 1, in which 1-hexachlorobenzene, 2-decachlorobiphenyl;
FIG. 3 is a HPLC chart of the second test sample solution in example 1, in which 1-hexachlorobenzene, 2-decachlorobiphenyl;
FIG. 4 is an HPLC plot of the second standard working solution of example 1, wherein 1-hexachlorobenzene, 2-decachlorobiphenyl;
FIG. 5 is a graph of a hexachlorobenzene standard curve;
fig. 6 is a decachlorobiphenyl standard graph.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
In the following examples, the liquid chromatograph is an Agilent 1260 liquid chromatograph;
the chromatographic column is an Agilent ZORBAX SB-C18 column with the specification of 150 multiplied by 4.6mm and the filler particle size of 5 mu m;
the balance is available from METTLER TOLEDO, model number ME 204/02;
hexachlorobenzene standards were purchased from dr. ehrenstorfer Gmbh in a mass fraction of 99.9%;
a decachlorobiphenyl standard sample is purchased from dr.ehrenstorfer Gmbh and has a mass fraction of 98.7%;
the chlorothalonil samples are all from Jiangsu Xinhe agricultural chemical industry Co., Ltd, and the types are 98.5 percent of chlorothalonil original drugs;
other materials and reagents, unless otherwise specified, are commercially available.
Preparation of standard working solutions: respectively weighing 0.01g (accurate to 0.0001g) of hexachlorobenzene standard sample and 0.01g (accurate to 0.0001g) of decachlorobiphenyl standard sample, placing the six standard samples and the 0.01g (accurate to 0.0001g) of decachlorobiphenyl standard sample into a 50mL volumetric flask, adding acetone, shaking to dissolve the six standard samples, diluting the six standard samples to a scale with acetone, and shaking uniformly to obtain standard stock solutions; transferring 2.0mL of the standard stock solution into a 50mL volumetric flask by using a pipette, diluting the standard stock solution to a scale by using acetone, and shaking up to obtain a standard intermediate diluent; and transferring 2.0mL of the intermediate diluent into a 50mL volumetric flask by using a pipette, diluting the intermediate diluent to a scale mark by using acetone, and shaking up to obtain a standard working solution for later use.
Preparing a sample solution to be tested: weighing 0.1g (accurate to 0.0001g) of chlorothalonil sample, placing in a glass bottle with a plug, adding 10mL of acetone by a pipette, shaking for 10min in ultrasonic waves of 37kHz to dissolve the acetone, cooling to 25 ℃, and shaking uniformly for later use.
Example 1
The present embodiment provides an HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil, wherein the column temperature is 35 ℃, the detection wavelength is 216nm, the flow rate is 1.0mL/min, the sample injection amount is 20 μ L, water and acetonitrile are used as mobile phases, gradient elution is adopted, and the gradient elution procedure is as shown in table 1:
TABLE 1 gradient elution procedure
Under the chromatographic operation condition, after the baseline of the instrument is stable, continuously injecting a plurality of needles of standard working solution until the relative change of the peak areas of two adjacent needles of hexachlorobenzene (decachlorobiphenyl) is less than 10%, injecting the sample solution to be detected, injecting the standard working solution and the sample solution to be detected twice respectively, and performing sample injection determination according to the sequence of the standard working solution, the sample solution to be detected and the standard working solution to obtain the gas chromatogram of each impurity in chlorothalonil. FIGS. 1 to 4 are HPLC charts of the first standard working solution, the first sample solution to be tested, the second sample solution to be tested, and the second standard working solution, respectively, wherein 1-hexachlorobenzene and 2-decachlorobiphenyl are used.
Example 2
This example provides an HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil, wherein the steps are the same as those in example 1 except that the initial mobile phase water is 7% and the acetonitrile is 93%.
Example 3
This example provides an HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil, wherein the steps are the same as those in example 1 except that the initial mobile phase water is 9% and the acetonitrile is 91%.
Example 4
This example provides an HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil, wherein the flow rate is 1.2mL/min, and the other steps are the same as those in example 1.
Example 5
This example provides an HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil, wherein the flow rate is 0.8mL/min, and the other steps are the same as those in example 1.
Example 6
This example provides an HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil, wherein the steps are the same as those in example 1 except that the column temperature is 40 ℃.
Example 7
This example provides an HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil, wherein the detection wavelength is 220nm, and the other steps are the same as those in example 1.
Example 8
This example provides an HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil, wherein the detection wavelength is 213nm, and the other steps are the same as those in example 1.
Example 9
This example provides an HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil, wherein the steps are the same as in example 1 except that the sample amount is 10. mu.L.
And (3) counting detection results:
calculating the detection results in the embodiments 1 to 9 to obtain the contents of hexachlorobenzene and decachlorobiphenyl in the sample solution to be detected, wherein the calculation formula is as follows:
in the formula:
ω1-mass fraction of hexachlorobenzene (decachlorobiphenyl) in chlorothalonil samples, expressed in mg/kg;
A2-average value of the area of the peak of hexachlorobenzene (decachlorobiphenyl) in the sample solution to be tested;
m1-mass of hexachlorobenzene (decachlorobiphenyl) standard, g;
omega-mass fraction of hexachlorobenzene (decachlorobiphenyl) in hexachlorobenzene (decachlorobiphenyl) standard sample, expressed in%;
A1-average value of hexachlorobenzene (decachlorobiphenyl) peak area in standard working solution;
m2-mass of chlorothalonil sample, g;
n-dilution factor, n 3125.
The results are shown in Table 2:
TABLE 2 content of hexachlorobenzene and decachlorobiphenyl in the samples to be tested
The data in the table show that the detection method provided by the invention has the influence degree on the measurement result meeting the requirement when the initial mobile phase proportion, the flow rate, the column temperature, the detection wavelength and the sample injection amount are adjusted in a certain range, and the method has good durability.
Drawing a standard curve:
a mixed standard solution of hexachlorobenzene and decachlorobiphenyl was prepared at hexachlorobenzene concentrations of 0.0125. mu.g/mL, 0.0218. mu.g/mL, 0.0623. mu.g/mL, 0.1247. mu.g/mL, 0.3896. mu.g/mL, 0.6534. mu.g/mL, and decachlorobiphenyl concentrations of 0.0109. mu.g/mL, 0.0191. mu.g/mL, 0.0545. mu.g/mL, 0.1090. mu.g/mL, 0.3407. mu.g/mL, 0.5451. mu.g/mL, and introduced according to the chromatographic conditions and procedures of example 1, and the peak areas were determined, the results of which are shown in Table 3 and Table 4:
TABLE 3 Linear Range determination of hexachlorobenzene quantitative analysis
| Rank of | 1 | 2 | 3 | 4 | 5 | 6 |
| Concentration (μ g/mL) | 0.0125 | 0.0218 | 0.0623 | 0.1247 | 0.3896 | 0.6234 |
| Peak area A | 2.1 | 7.1 | 20.3 | 40.3 | 125.6 | 201.3 |
TABLE 4 quantitative analysis of decachlorobiphenyl Linear Range determination
| Rank of | 1 | 2 | 3 | 4 | 5 | 6 |
| Concentration (μ g/mL) | 0.0109 | 0.0191 | 0.0545 | 0.1090 | 0.3407 | 0.5451 |
| Peak area A | 2.6 | 4.6 | 13.2 | 26.4 | 82.4 | 132.6 |
Taking the concentration of the standard solution as an abscissa and the peak area ratio as an ordinate, drawing a standard working curve to obtain a hexachlorobenzene regression equation with Y being 322.9X +0.024 and a correlation coefficient R21.0000, the linear correlation diagram is shown in figure 5, the regression equation of the decachlorobiphenyl is that Y is 242.8X-0.025, and the correlation coefficient R2The linear dependence is shown in fig. 6, 1.0000.
And (3) precision test:
preparing 3 batches of samples with different contents of hexachlorobenzene and decachlorobiphenyl, injecting samples according to the method for preparing the sample solution and the chromatographic conditions in the example 1, measuring peak areas, and calculating the contents of hexachlorobenzene and decachlorobiphenyl in the samples according to the regression equation of the standard curve, wherein the results are shown in tables 5 and 6:
TABLE 5 results of quantitative analysis and precision measurement of hexachlorobenzene in chlorothalonil
TABLE 6 quantitative analysis precision measurement results of decachlorobiphenyl in chlorothalonil
The results in tables 5 and 6 show that the standard deviation range of the detected hexachlorobenzene content is 0.13-0.21mg/kg, and the coefficient of variation is 0.9-2.5%; the standard deviation range of the content of the decachlorobiphenyl is 0.11-0.16mg/kg, the coefficient of variation is 0.8-3.3%, and the detection method provided by the invention is high in precision.
And (3) accuracy test:
hexachlorobenzene and decachlorobiphenyl standards with different levels are respectively added into a test sample with known hexachlorobenzene and decachlorobiphenyl contents to prepare a sample with known content, sample injection is carried out according to the chromatographic conditions and the steps in the example 1, the peak area is measured, and the recovery rate is calculated, and the result is shown in tables 7 and 8:
TABLE 7 result of accuracy measurement of quantitative analysis of hexachlorobenzene
TABLE 8 results of quantitative analysis of decachlorobiphenyl
The results in tables 7 and 8 show that the average recovery rate of the hexachlorobenzene standard substance is 100.8%, and the average recovery rate of the decachlorobiphenyl standard substance is 99.8%, which indicates that the detection method provided by the invention has high accuracy in detecting the contents of hexachlorobenzene and decachlorobiphenyl.
Measuring detection limit and quantitative limit of the method:
the standard stock solutions of hexachlorobenzene and decachlorobiphenyl with known concentrations were added to the blank samples, and the chromatographic conditions and procedures in example 1 were repeated several times, and peak areas were measured, and the detection Limit (LOD) and quantification Limit (LOQ) of the method were determined with 3-fold signal-to-noise ratio and 10-fold signal-to-noise ratio, respectively, and the results are shown in tables 9 and 10:
TABLE 9 results of limit of detection and limit of quantitation of hexachlorobenzene
TABLE 10 quantitative analysis method of decachlorobiphenyl, detection limit, quantitative limit determination results
The results in tables 9 and 10 show that the method detection limit of hexachlorobenzene in the chlorothalonil sample is 0.003 mu g/ml, the method quantification limit is 0.006 mu g/ml, the method detection limit of decachlorobiphenyl is 0.005 mu g/ml and the method quantification limit is 0.010 mu g/ml, which indicates that the detection method provided by the invention has high sensitivity.
Method comparative test:
various levels of hexachlorobenzene and decachlorobiphenyl were analyzed in chlorothalonil samples using the chromatographic conditions and procedures of example 1 and FAO-2019 gas chromatography mass spectrometry (GC-MSD) analysis, respectively, with the results shown in tables 11 and 12:
TABLE 11 content of hexachlorobenzene obtained by different analytical methods
TABLE 12 content of decachlorobiphenyl obtained by different analytical methods
The results in tables 11 and 12 show that, compared with the FAO gas chromatography mass spectrometry method, the relative deviation range of the hexachlorobenzene content is 1.3-4.3%, and the relative deviation range of the decachlorobiphenyl content is 0.8-4.9%, which shows high accuracy.
The applicant states that the present invention is illustrated by the above examples of the HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil, but the present invention is not limited to the above examples, i.e. it does not mean that the present invention must be implemented by the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
Claims (10)
1. An HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil is characterized by comprising the following steps: carrying out HPLC detection on a to-be-detected sample solution prepared from a standard working solution prepared from a hexachlorobenzene and decachlorobiphenyl standard sample and a chlorothalonil sample by using water and acetonitrile as mobile phases and adopting a C18 reversed phase chromatographic column, and calculating according to a detection result to obtain the content of hexachlorobenzene and decachlorobiphenyl in the to-be-detected sample;
the preparation method of the standard working solution comprises the following steps: placing hexachlorobenzene and deca-chlorobiphenyl standard samples into a volumetric flask, adding a solvent, shaking for dissolving, and fixing the volume to obtain a standard stock solution; diluting the standard stock solution to obtain a standard working solution; the solvent added and dissolved by shaking comprises acetone;
the preparation method of the sample solution to be detected comprises the following steps: diluting a chlorothalonil sample with a solvent, dissolving the chlorothalonil sample by vibration under ultrasonic waves, and cooling to obtain a sample solution to be detected; the solvent for solvent dilution comprises acetone;
the column temperature of the C18 reversed phase chromatographic column is 30-40 ℃;
the specification of the C18 reversed phase chromatographic column is 150 multiplied by 4.6mm, and the particle size of the filler is 5 mu m;
in the HPLC detection, the detection wavelength is 212-220nm, and the flow rate of the column is 0.8-1.2 mL/min;
the HPLC assay employed a gradient elution performed according to the following procedure: at 0-5min, the volume of water in the mobile phase accounts for 8%, and the volume of acetonitrile accounts for 92%; the volume ratio of water in the mobile phase is decreased at the speed of 8%/min at the 5 th min, the volume ratio of acetonitrile is increased at the speed of 8%/min, and the mobile phase is pure acetonitrile at the 6 th min and is continued for the 12 th min; and the volume ratio of water in the mobile phase is increased at the speed of 8%/min at the 12 th min, the volume ratio of acetonitrile is decreased at the speed of 8%/min, and the volume ratio of water in the mobile phase is 8% and the volume ratio of acetonitrile is 92% at the 13 th min, and the process is continued until the 16 th min.
2. The HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil according to claim 1, wherein the mass ratio of hexachlorobenzene to decachlorobiphenyl in the standard stock solution is 1:0.8-1: 1.2.
3. The HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil according to claim 2, wherein the concentration of said standard stock solution is 0.15-0.25 mg/mL.
4. The HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil according to claim 1, wherein the dilution factor for diluting the standard stock solution is 500-2000.
5. The HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil according to claim 1, wherein the frequency of ultrasound is 35-40 kHz.
6. The HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil according to claim 1, wherein the time of ultrasonic treatment is 6-10 min.
7. The HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil according to claim 1, wherein said cooling is performed to a temperature of 20-30 ℃.
8. The HPLC detecting method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil according to claim 1, wherein the dilution factor of the chlorothalonil sample diluted with acetone is 8-12.
9. The HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil according to claim 1, wherein the concentration of the sample solution to be detected is 9-15 mg/mL.
10. The HPLC detection method for simultaneously detecting hexachlorobenzene and decachlorobiphenyl in chlorothalonil according to claim 1, wherein the sample volume in the HPLC detection is 10-20 μ L.
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