CN114487166B - Method for detecting content of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine - Google Patents
Method for detecting content of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine Download PDFInfo
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- JRLZWXISQMMITA-UHFFFAOYSA-N 2-hydroxy-6-oxo-4-(trifluoromethyl)-1h-pyridine-3-carbonitrile Chemical compound OC=1NC(=O)C=C(C(F)(F)F)C=1C#N JRLZWXISQMMITA-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000001514 detection method Methods 0.000 claims abstract description 23
- 239000000126 substance Substances 0.000 claims abstract description 13
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 12
- 238000004364 calculation method Methods 0.000 claims abstract description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 84
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 239000005900 Flonicamid Substances 0.000 abstract description 6
- RLQJEEJISHYWON-UHFFFAOYSA-N flonicamid Chemical compound FC(F)(F)C1=CC=NC=C1C(=O)NCC#N RLQJEEJISHYWON-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000575 pesticide Substances 0.000 abstract description 6
- 239000000543 intermediate Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 238000003908 quality control method Methods 0.000 abstract description 2
- 238000013441 quality evaluation Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 53
- 238000012360 testing method Methods 0.000 description 15
- 238000002360 preparation method Methods 0.000 description 11
- 238000001816 cooling Methods 0.000 description 10
- 238000007865 diluting Methods 0.000 description 10
- 238000004090 dissolution Methods 0.000 description 10
- 230000010355 oscillation Effects 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
- 230000004044 response Effects 0.000 description 8
- 238000002347 injection Methods 0.000 description 6
- 239000007924 injection Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 241000238631 Hexapoda Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003630 growth substance Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- IBBMAWULFFBRKK-UHFFFAOYSA-N picolinamide Chemical compound NC(=O)C1=CC=CC=N1 IBBMAWULFFBRKK-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- QEVHRUUCFGRFIF-MDEJGZGSSA-N reserpine Chemical compound O([C@H]1[C@@H]([C@H]([C@H]2C[C@@H]3C4=C(C5=CC=C(OC)C=C5N4)CCN3C[C@H]2C1)C(=O)OC)OC)C(=O)C1=CC(OC)=C(OC)C(OC)=C1 QEVHRUUCFGRFIF-MDEJGZGSSA-N 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
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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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- 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
- G01N30/60—Construction of the column
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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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
- G01N30/86—Signal analysis
- G01N30/8603—Signal analysis with integration or differentiation
- G01N30/8606—Integration
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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
- G01N2030/042—Standards
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Abstract
The invention relates to the technical field of chemical analysis, in particular to a method for detecting the content of 2, 6-dihydroxyl-3-cyano-4-trifluoromethylpyridine, which specifically adopts high performance liquid chromatography to detect the content of 2, 6-dihydroxyl-3-cyano-4-trifluoromethylpyridine in a system to be detected. The detection method provided by the invention fills the blank in the field, and the mass fraction of the 2, 6-dihydroxy-3-cyano-4-trifluoromethyl pyridine is detected by adopting the method, so that the chromatographic peak shape is good, the integral calculation result is accurate, the repeatability is good, and the obtained result has high reliability and is more accurate and instant; the method has strong specificity and good precision, is particularly suitable for quality evaluation and control of intermediates and raw pesticide flonicamid, can meet the production requirement of high-quality pesticides, and has important effect and practical significance for guaranteeing the quality of final products.
Description
Technical Field
The invention relates to the technical field of chemical analysis, in particular to a method for detecting the content of 2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine.
Background
Flonicamid belongs to a novel low-toxicity pyridine amide insect growth regulator pesticide. In recent years, flonicamid bactericidal active compounds are increasingly reused in pesticide research due to the characteristics of wide bactericidal spectrum, high toxicity and small dosage. 2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine is taken as an important intermediate in the synthesis process, has important significance for improving the yield of flonicamid, shortening the production time and reducing the reaction energy consumption and waste discharge, so that the search for a high-efficiency detection method of 2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine is very necessary, and has important guiding significance for the production of flonicamid.
In the prior art, no report is found about the method for detecting the content of 2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine.
Disclosure of Invention
Aiming at the problem that the prior art for detecting the content of 2, 6-dihydroxyl-3-cyano-4-trifluoromethylpyridine has blank technology, the invention provides a method for detecting the content of 2, 6-dihydroxyl-3-cyano-4-trifluoromethylpyridine, which has the advantages of accurate detection result, good repeatability and high reliability.
The invention provides a method for detecting the content of 2, 6-dihydroxyl-3-cyano-4-trifluoromethylpyridine, which specifically adopts a high performance liquid chromatography to detect the content of 2, 6-dihydroxyl-3-cyano-4-trifluoromethylpyridine in a system to be detected.
Further, the method for detecting the content of the 2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine specifically comprises the following steps:
(1) Respectively dissolving a standard substance and a sample to be tested by adopting a solvent to obtain a standard sample and a sample;
(2) Setting the detection wavelength of a high performance liquid chromatograph, sequentially injecting samples according to the sequence of a standard sample, a sample and the standard sample after the baseline of the instrument is stable, and respectively calculating the average value of the peak areas of the 2, 6-dihydroxy-3-cyano-4-trifluoromethyl pyridine in the chromatograms of the standard sample and the sample to obtain the average value of the peak areas;
(3) Calculating mass fraction X 1 of 2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine in the sample according to a calculation formula shown as formula (1),
In the formula (1):
A 1 -standard, peak area average value of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine;
a 2 -average peak area of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine in sample;
m 1 -mass of standard;
m 2 -mass of sample;
p 1 -mass fraction of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine in the standard;
X 1 -mass fraction of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine in the sample.
Further, the mobile phase of the high performance liquid chromatograph is a mixed solution of acetonitrile and an ammonium formate aqueous solution, and the volume ratio of the acetonitrile to the ammonium formate aqueous solution is 10-20: 90-80.
Further, the flow rate of the mobile phase is 0.8-1.2 mL/min.
Further, the concentration of the aqueous ammonium formate solution is 10 to 100mmol/L.
Further, the chromatographic column adopted by the high performance liquid chromatograph is a packed column of silica gel bonded C18, the column length of the chromatographic column is 150mm, the inner diameter of the column is 3-4.6mm, the particle size is 4-5 mu m, and the column temperature is 30 ℃.
Further, the detection wavelength of the high performance liquid chromatograph is set to 260 to 280nm.
Further, the sample injection amount of each sample was 5. Mu.L.
Further, in the step (1), the solvent is acetonitrile.
Further, the concentration of the standard substance in the standard sample is 0.5-2g/L, and the concentration of the sample to be detected in the sample is 0.5-2g/L.
The method for detecting the content of the 2, 6-dihydroxyl-3-cyano-4-trifluoromethylpyridine by using the high performance liquid chromatography has the advantages that the method for detecting the content of the 2, 6-dihydroxyl-3-cyano-4-trifluoromethylpyridine by using the method makes up the blank in the field, the mass fraction of the 2, 6-dihydroxyl-3-cyano-4-trifluoromethylpyridine is detected by using the method, the chromatographic peak shape is good, the integral calculation result is accurate, the repeatability is good, and the reliability of the obtained result is high and more accurate and instant; the method has strong specificity and good precision, is particularly suitable for quality evaluation and control of intermediates and raw pesticide flonicamid, can meet the production requirement of high-quality pesticides, and has important effect and practical significance for guaranteeing the quality of final products.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the description of the embodiments or the prior art will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
FIG. 1 is a chromatogram of a standard sample of example 1 according to an embodiment of the present invention.
FIG. 2 shows a sample chromatogram of example 1 according to an embodiment of the present invention.
FIG. 3 is a graph showing the linear relationship obtained in test example 2 according to the embodiment of the present invention.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
The high performance liquid chromatograph adopted in the embodiment and the test example of the invention is an LC-20ATvp infusion pump and an SPD-20Avp ultraviolet detector of Shimadzu corporation, the chromatographic column is a packed column (Dalian Lite Hypersil ODS2150 x 4.6mm grain size 5 μm) with silica gel bonded with C18, the column temperature is 30 ℃, the mixed solution of acetonitrile and ammonium formate aqueous solution is taken as a mobile phase, the flow rate is 1.0mL/min, and the volume ratio of acetonitrile to ammonium formate aqueous solution is 15:85, the concentration of the aqueous ammonium formate solution was 50mmol/L.
Example 1
The sample to be tested in the embodiment is 500 kg of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine produced in a workshop, and the content of the sample to be tested is detected, and the detection method specifically comprises the following steps:
(1) Standard sample preparation
Accurately weighing 0.0518g (0.0002 g accurate) of a2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine standard substance, placing the standard substance in a 100mL volumetric flask, adding 40mL of acetonitrile, carrying out ultrasonic oscillation dissolution, cooling to room temperature, and diluting with acetonitrile to a scale to obtain a standard sample;
(2) Sample preparation
Accurately weighing 0.0523g (0.0002 g accurate) of 2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine, placing the sample in a 100mL volumetric flask, adding 40mL of acetonitrile, carrying out ultrasonic oscillation and dissolution, cooling to room temperature, and diluting to a scale with acetonitrile to obtain a sample;
(3) High performance liquid chromatography detection
After the machine self-checking is started, under the specified operation condition, after the instrument baseline is stable, a plurality of needle standard samples are continuously injected, the relative response value of each needle is calculated, after the change of the relative response value of two adjacent needles is less than 1.5%, sample injection is sequentially carried out according to the sequence of the standard samples, the samples and the standard samples, the sample injection volume is 5 mu L each time, the detection is carried out at the wavelength of 270nm, the chromatograms are shown in figures 1 and 2, and the data shown in the following table 1 are obtained:
Table 1 chromatographic test results of samples and standard samples in example 1
The mass fraction X 1 = 94.74% of the sample containing 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine in this example was calculated according to formula (1).
Example 2
The sample to be tested in the embodiment is 600 kg of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine produced in a workshop, and the content of the sample to be tested is detected, and the detection method specifically comprises the following steps:
(1) Standard sample preparation
Accurately weighing 0.0512g (accurate to 0.0002 g) of a2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine standard substance, placing into a 100mL volumetric flask, adding 40mL of acetonitrile, carrying out ultrasonic oscillation and dissolution, cooling to room temperature, and diluting to a scale with acetonitrile to obtain a standard sample;
(2) Sample preparation
Accurately weighing 0.0515g (accurate to 0.0002 g) of 2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine, placing the sample in a 100mL volumetric flask, adding 40mL of acetonitrile, carrying out ultrasonic oscillation dissolution, cooling to room temperature, and diluting to a scale with acetonitrile to obtain a sample;
(3) High performance liquid chromatography detection
After the machine self-checking is started, under the specified operation condition, after the instrument baseline is stable, a plurality of needle standard samples are continuously injected, the relative response value of each needle is calculated, after the change of the relative response value of two adjacent needles is less than 1.5%, sample injection is sequentially carried out according to the sequence of the standard samples, the samples and the standard samples, the sample injection volume is 5 mu L each time, the detection is carried out under the wavelength of 270nm, and the data shown in the following table 2 are obtained:
table 2 chromatographic test results of samples and standard samples in example 2
According to formula (1), the mass fraction X 1 = 94.20% of the sample containing 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine in this example was obtained by calculation.
Test example 1
(1) Standard sample preparation
Accurately weighing 0.0508g (0.0002 g accurate) of 2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine standard substance, placing into a 100mL volumetric flask, adding 40mL acetonitrile, carrying out ultrasonic oscillation and dissolution, cooling to room temperature, and diluting with acetonitrile to scale to obtain a standard sample;
(2) Sample preparation
Accurately weighing 6 parts of 2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine, respectively placing the 6 parts of samples in a 100mL volumetric flask, respectively adding 40mL of acetonitrile for ultrasonic oscillation dissolution, cooling to room temperature, and diluting to a scale with acetonitrile to obtain 6 parts of samples, wherein the mass of the 6 parts of samples is shown in a table 3;
(3) High performance liquid chromatography detection
After the machine self-checking is started, under the specified operation condition, after the instrument baseline is stable, continuously injecting a plurality of needle standard samples, calculating the relative response value of each needle, after the change of the relative response value of two adjacent needles is less than 1.5%, sequentially injecting samples according to the sequence of the standard samples, the samples and the standard samples, wherein the volume of each sample injection is 5 mu L, the detection is repeated at the wavelength of 270nm, and the content of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine in 6 samples is calculated by the formula (1), so as to obtain the data shown in the following table 3:
TABLE 3 content of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine in 6 samples of test example 1
As can be seen from Table 3, the detection method provided by the invention has good repeatability.
Test example 2
(1) Standard sample preparation
Accurately weighing 0.0508g (0.0002 g accurate) of 2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine standard substance, placing into a 100mL volumetric flask, adding 40mL acetonitrile, carrying out ultrasonic oscillation and dissolution, cooling to room temperature, and diluting with acetonitrile to scale to obtain a standard sample;
(2) Sample preparation
Accurately weighing 6 groups of samples containing 2, 6-dihydroxyl-3-cyano-4-trifluoromethylpyridine, respectively placing the samples in a 100mL volumetric flask, adding 40m acetonitrile, carrying out ultrasonic oscillation dissolution, cooling to room temperature, and diluting to a scale with acetonitrile to obtain 6 parts of sample solutions to be tested, wherein the concentration of the 2, 6-dihydroxyl-3-cyano-4-trifluoromethylpyridine is 209 mug/mL, 316 mug/mL, 425 mug/mL, 523 mug/mL, 611 mug/mL and 696 mug/mL respectively;
(3) High performance liquid chromatography detection
After the machine self-checking is started, under the specified operation condition, after the instrument baseline is stable, continuously injecting a plurality of needle standard samples, calculating the relative response value of each needle, after the change of the relative response value of two adjacent needles is less than 1.5%, sequentially sampling according to the sequence of the standard samples, the samples and the standard samples, wherein the sampling volume is 5 mu L each time, detecting the samples in the sequential group at the wavelength of 270nm, and carrying out linear regression on the concentration (ug/ml) of the x-axis sample by using the y-axis peak area (A), wherein the obtained regression equation is as follows:
y＝4018.3x-5722，R2＝0.9993；
As can be seen, the 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine has good linear relationship in the range of 200-700. Mu.g/mL.
Test example 3
(1) Standard sample preparation
Accurately weighing 0.0513g (0.0002 g accurate) of a2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine standard substance, placing the standard substance in a 100mL volumetric flask, adding 40mL of acetonitrile, carrying out ultrasonic oscillation dissolution, cooling to room temperature, and diluting with acetonitrile to a scale to obtain a standard sample;
(2) Sample preparation
6 Staff accurately weigh 6 parts of samples of 2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine in different laboratories, respectively, placing the 6 parts of samples in 100mL volumetric flasks, respectively, adding 40mL of acetonitrile respectively, carrying out ultrasonic oscillation dissolution, cooling to room temperature, and diluting to a scale with acetonitrile to obtain 6 parts of samples, wherein the mass of the 6 parts of samples is shown in a table 4;
(3) High performance liquid chromatography detection
Different persons in different laboratories respectively detect samples according to the high performance liquid chromatography detection method in example 1, and sequentially calculate the content of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine in 6 samples according to formula (1), so as to obtain the data shown in the following table 4:
TABLE 4 content of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine in 6 samples of test example 3
As can be seen from Table 4, the experimental results of the detection method provided by the invention have good intermediate precision.
Test example 4
Samples were prepared as in example 1, and were subjected to high performance liquid chromatography for 0, 1,2, 4, 8, and 24 hours after preparation, respectively, and scanning was sequentially performed at 270nm at different times to obtain good peak shapes, and the peak areas were obtained as the samples were varied with time, and the results are shown in Table 5.
TABLE 5 Peak area data in test example 4
| Time (h) | 0 | 1 | 2 | 4 | 8 | 24 | RSD％ |
| Peak area | 2087146 | 2088213 | 2084895 | 2081427 | 2080574 | 2082563 | 0.15 |
As can be seen from the data in Table 5, the test results of the detection method provided by the invention have good time stability.
Test example 5
Preparing a standard sample according to the method of the example 1 to obtain 10.516mg/ml standard sample; then precisely weighing three parts of samples 0.02 g, 0.03 g and 0.04 g in the same batch, wherein the specific mass of 9 parts of samples is shown in table 6, respectively dissolving the 9 parts of samples in a 100ml volumetric flask to obtain samples, dividing the 9 parts of samples into 3 groups, respectively adding 3.0ml, 2.0ml and 1.0ml of standard samples with the concentration of 10.516mg/ml into the 3 groups of samples to obtain 9 parts of mixed samples, performing constant volume standard adding recovery test, sequentially detecting the 9 parts of mixed samples according to the high performance liquid chromatography of the embodiment 1, calculating the content according to the formula (1), and specifically obtaining the content shown in table 6.
TABLE 6 content of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine in sample of test example 5
As can be seen from Table 6, the detection method provided by the invention has good standard adding recovery rate.
In conclusion, the method for detecting the content of the 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine provided by the invention has high accuracy and good operability, and can be widely applied to analysis and detection of the content of the 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine.
Although the present invention has been described in detail by way of preferred embodiments with reference to the accompanying drawings, the present invention is not limited thereto. Various equivalent modifications and substitutions may be made in the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and it is intended that all such modifications and substitutions be within the scope of the present invention/be within the scope of the present invention as defined by the appended claims.
Claims (5)
1. The method for detecting the content of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine is characterized in that the content of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine in a system to be detected is detected by adopting a high performance liquid chromatography; the method specifically comprises the following steps:
(1) Acetonitrile is adopted to dissolve a standard substance and a sample to be detected respectively, so as to obtain a standard sample and a sample;
(2) Setting the detection wavelength of a high performance liquid chromatograph, sequentially injecting samples according to the sequence of a standard sample, a sample and the standard sample after the baseline of the instrument is stable, and respectively calculating the average value of the peak areas of the 2, 6-dihydroxy-3-cyano-4-trifluoromethyl pyridine in the chromatograms of the standard sample and the sample to obtain the average value of the peak areas;
(3) The mass fraction X 1 of the 2, 6-dihydroxyl-3-cyano-4-trifluoromethyl pyridine in the sample is calculated according to a calculation formula, the calculation formula is as follows,
；
Wherein:
A 1 -standard, peak area average value of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine;
a 2 -average peak area of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine in sample;
m 1 -mass of standard;
m 2 -mass of sample;
p 1 -mass fraction of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine in the standard;
X 1 -mass fraction of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine in the sample;
the mobile phase of the high performance liquid chromatograph is a mixed solution of acetonitrile and an ammonium formate aqueous solution, and the volume ratio of the acetonitrile to the ammonium formate aqueous solution is 10-20: 90-80 parts;
the concentration of the ammonium formate aqueous solution is 10-100 mmol/L;
the chromatographic column adopted by the high performance liquid chromatograph is a packed column of silica gel bonded C18, and the column temperature is 30 ℃;
The detection wavelength of the high performance liquid chromatograph is set to 260-280 nm.
2. The method for detecting the content of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine according to claim 1, wherein the flow rate of a mobile phase is 0.8-1.2 mL/min.
3. The method for detecting the content of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine according to claim 1, wherein the chromatographic column has a length of 150mm, an inner diameter of 3-4.6mm, and a particle diameter of 4-5 μm.
4. The method for detecting the content of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine according to claim 1, wherein the sample introduction amount of each sample is 5 μl.
5. The method for detecting the content of 2, 6-dihydroxy-3-cyano-4-trifluoromethylpyridine according to claim 1, wherein the concentration of the standard substance in the standard sample is 0.5-2g/L, and the concentration of the sample to be detected in the sample is 0.5-2g/L.
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