CN115453006A - Method for detecting oleic acid content in raw material oil acid - Google Patents
Method for detecting oleic acid content in raw material oil acid Download PDFInfo
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- CN115453006A CN115453006A CN202211229975.2A CN202211229975A CN115453006A CN 115453006 A CN115453006 A CN 115453006A CN 202211229975 A CN202211229975 A CN 202211229975A CN 115453006 A CN115453006 A CN 115453006A
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 title claims abstract description 142
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 title claims abstract description 141
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 title claims abstract description 141
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 title claims abstract description 141
- 239000005642 Oleic acid Substances 0.000 title claims abstract description 141
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 title claims abstract description 141
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 title claims abstract description 141
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000002994 raw material Substances 0.000 title claims abstract description 30
- 239000002253 acid Substances 0.000 title abstract description 7
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000000243 solution Substances 0.000 claims abstract description 41
- 238000001514 detection method Methods 0.000 claims abstract description 34
- 239000012085 test solution Substances 0.000 claims abstract description 28
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000523 sample Substances 0.000 claims abstract description 24
- 238000012360 testing method Methods 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 238000005303 weighing Methods 0.000 claims abstract description 15
- 238000010812 external standard method Methods 0.000 claims abstract description 9
- 239000012488 sample solution Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 23
- 238000007865 diluting Methods 0.000 claims description 12
- 239000012159 carrier gas Substances 0.000 claims description 10
- 238000004817 gas chromatography Methods 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000004448 titration Methods 0.000 abstract description 5
- 239000013558 reference substance Substances 0.000 description 25
- 239000012088 reference solution Substances 0.000 description 14
- 238000011084 recovery Methods 0.000 description 11
- 238000002474 experimental method Methods 0.000 description 5
- 239000013074 reference sample Substances 0.000 description 5
- 239000003995 emulsifying agent Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000011550 stock solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000008396 flotation agent Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000002960 lipid emulsion Substances 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 239000008031 plastic plasticizer Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- JQWAHKMIYCERGA-UHFFFAOYSA-N (2-nonanoyloxy-3-octadeca-9,12-dienoyloxypropoxy)-[2-(trimethylazaniumyl)ethyl]phosphinate Chemical compound CCCCCCCCC(=O)OC(COP([O-])(=O)CC[N+](C)(C)C)COC(=O)CCCCCCCC=CCC=CCCCCC JQWAHKMIYCERGA-UHFFFAOYSA-N 0.000 description 1
- 239000004278 EU approved seasoning Substances 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 159000000009 barium salts Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012742 biochemical analysis Methods 0.000 description 1
- 201000001883 cholelithiasis Diseases 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 239000004434 industrial solvent Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- WIBFFTLQMKKBLZ-SEYXRHQNSA-N n-butyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCCCC WIBFFTLQMKKBLZ-SEYXRHQNSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000989 no adverse effect Toxicity 0.000 description 1
- QTDSLDJPJJBBLE-PFONDFGASA-N octyl (z)-octadec-9-enoate Chemical compound CCCCCCCCOC(=O)CCCCCCC\C=C/CCCCCCCC QTDSLDJPJJBBLE-PFONDFGASA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000003128 rodenticide Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 210000002268 wool Anatomy 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
-
- 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
- G01N30/26—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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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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
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
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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
- G01N2030/047—Standards external
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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
- G01N30/26—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
- G01N2030/324—Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate
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Abstract
The invention discloses a method for detecting the oleic acid content in raw material oil acid, which comprises the preparation and determination methods of a test sample solution, wherein the preparation method comprises the following steps: precisely weighing 17mg of oleic acid, placing the oleic acid in a 10ml measuring flask, uniformly mixing the oleic acid and tetrahydrofuran, and finally preparing a solution containing 1.7mg of oleic acid per 1ml as a test solution. According to the method, an external standard method is adopted, and compared with the conventional detection method which adopts a titration method for detection under the three specified conditions, the method has the advantages that the result error is larger due to the fact that the judgment of the detection result is different in the process of result judgment and actual operation according to different personnel, and the detection is carried out through a precision instrument gas chromatograph, so that the artificial error is reduced, and the oleic acid content can be accurately calculated through a reference chromatogram and a test sample chromatogram.
Description
Technical Field
The invention relates to the technical field of oleic acid content detection, in particular to a method for detecting the oleic acid content in raw material oil acid.
Background
The oleic acid raw material is widely applied, is mainly used for preparing plastic plasticizers of epoxy butyl oleate and epoxy octyl oleate, is used for preparing antistatic agents and lubricating softeners in the wool spinning industry, is used for preparing water repellent paraffin wax emulsion in the wood industry, can also be used for preparing pesticide emulsifiers, printing and dyeing auxiliaries, industrial solvents, mineral flotation agents, mold release agents and the like, can also be used for preparing copy paper, lettering paper, ball-point pen oil, various oleates and the like, can be used as a lubricating and stuck-releasing agent of drilling mud, sodium salt or sylvite of oleic acid is one of components of soap, pure sodium oleate has good decontamination capability, can be used as surfactants of emulsifiers and the like, can be used for treating cholelithiasis, other metal salts of oleic acid can also be used for waterproof fabrics, lubricants, polishing agents and the like, barium salt of oleic acid can be used as rodenticide, is used for biochemical analysis and gas chromatography standard substances, is used for preparing plastic plasticizers, pesticide emulsifiers, lubricants, factice, ore flotation agents and the like, and can be used as raw materials of detergents, fatty acid matrixes, cosmetics, chemical fiber oil agents, textile seasonings, refined plastics, engineering plastics, nylon 8 and nylon 9, and food baking raw materials;
oleic acid is also used for the production of medium/long chain fat emulsion injection and fat emulsion injection, the oleic acid raw material mainly serves as an auxiliary emulsifier, the HLB value of egg yolk lecithin can be adjusted, smaller emulsion drops can be formed easily, and the absolute value of the potential is increased, so that a stable O/W system is formed;
the oleic acid raw material has the oil acid content of 65.0-88.0% according to the quality standard, and the purity of the oleic acid raw material is detected by domestic raw material manufacturers according to a titration method of 2020 edition of Chinese pharmacopoeia at present, but the method has the problem that the accurate content of the main component oleic acid in the raw material is difficult to accurately detect due to the operation error of personnel;
therefore, it is necessary to provide a method for detecting the oleic acid content in the raw oleic acid to solve the above technical problems.
Disclosure of Invention
The invention aims to provide a method for detecting the oleic acid content in raw oil acid, which can effectively detect the oleic acid content of the variety and simultaneously improve the detection sensitivity, accuracy and reproducibility by an external standard method under three specified conditions compared with the prior art.
In order to achieve the purpose, the invention provides the following technical scheme: comprises the preparation and determination of a test solution;
(A) Preparation of control solutions: firstly, extracting a proper amount of oleic acid reference substances, accurately weighing, then adding tetrahydrofuran for dissolving, uniformly mixing tetrahydrofuran and an oleic acid solution, and diluting and dissolving the oleic acid solution to prepare a solution containing 1.7mg of oleic acid in 1ml of the oleic acid solution as a reference substance solution;
(B) Preparation of a test solution: firstly, precisely weighing 17mg of oleic acid, placing the oleic acid into a 10ml measuring flask, then adding tetrahydrofuran for diluting to a constant volume to scale, then uniformly mixing the oleic acid and the tetrahydrofuran, and finally preparing a solution containing about 1.7mg of oleic acid per 1ml as a test solution;
(C) The determination method comprises the following steps: firstly, precisely measuring 1 mu l of reference solution and 1 mu l of test solution respectively, injecting the reference solution and the test solution into a gas chromatograph, then injecting components into the gas chromatograph for analysis, recording the analysis result into a chromatogram, and finally calculating the oleic acid content by peak area according to an external standard method.
Preferably, the chromatographic conditions adopt a chromatographic column with FFAP as a capillary column of stationary liquid, and the FFAP passes through N 2 And H 2 As a gas for a gas chromatography carrier gas, N is added 2 The flow rate of (A) is set to 6.0ml/min to 8.0ml/min, and H is added 2 The flow rate of the method is set to be 35 ml/min-45 ml/min, a FID detector is adopted to carry out chromatographic detection on the oleic acid content in the oleic acid raw material, the temperature of the detector is set to be 275-285 ℃, the split ratio is set to be 10:1, dissolving with 1ul oleic acidThe liquid is used as the sample amount of the external standard method of the reference substance.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the method, an external standard method is adopted, and compared with the conventional detection method which adopts a titration method for detection under the three specified conditions, the method has the advantages that the result error is larger due to the fact that the judgment of the detection result is different in the process of result judgment and actual operation according to different personnel, and the detection is carried out through a precision instrument gas chromatograph, so that the personal error is reduced, and the oleic acid content can be accurately calculated through a reference chromatogram and a test sample chromatogram;
2. according to the method, through the measurement of 1.7mg/ml test sample solution, the peak height of the main component of the test sample in a chromatogram is about 350, the peak area is about 2615, and the peak width is about 0.13, so that the whole base line runs stably;
3. the method adopts a gas chromatograph to detect the oleic acid content in the variety under three conditions, can effectively reduce the error of artificially detecting the oleic acid content, and can improve the accuracy of detecting the oleic acid of the variety, wherein the flow rate of N2 is set to be 6.0 ml/min-8.0 ml/min, the flow rate of H2 is set to be 35 ml/min-45 ml/min, an FID detector is adopted to carry out chromatographic detection on the oleic acid content in the oleic acid raw material, the temperature of the detector is set to be 275-285 ℃, the temperature of a sample inlet is set to be 250-260 ℃, the split ratio of nitrogen is set to be 10:1, the running stability of the whole detection system can be effectively improved, compared with the prior art, the repeatability of the detection of the oleic acid content is good, the detection data meet the standard regulation, and the detection of the oleic acid content can be better met;
4. the invention sets the flow dividing ratio as 10: the method has the advantages that 1, the split ratio of the gas chromatograph comprises the proportion of gas generated by vaporization of a sample after the sample enters a sample inlet and the proportion of gas entering a color column and discharged from a sample injector, and can be adjusted through a split valve to effectively discharge most of the sample at a vent through carrier gas, so that only a fraction to a dozen of the samples enter a capillary chromatographic column for separation and analysis.
Drawings
FIG. 1 is a linear graph of the results of oleic acid detection according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Referring to fig. 1, an embodiment of the present invention: a method for detecting the content of oleic acid in an oleic acid raw material comprises the preparation and the determination of a test sample solution;
(A) Preparation of control solutions: firstly, extracting a proper amount of an oleic acid reference substance, precisely weighing, then adding tetrahydrofuran for dissolving, uniformly mixing tetrahydrofuran and an oleic acid solution, and diluting and dissolving the oleic acid solution to prepare a solution containing 1.7mg of oleic acid in 1ml as a reference substance solution;
(B) Preparation of a test solution: firstly, precisely weighing 17mg of oleic acid, placing the oleic acid into a 10ml measuring flask, then adding tetrahydrofuran for diluting to a constant volume to scale, then uniformly mixing the oleic acid and the tetrahydrofuran, and finally preparing a solution containing about 1.7mg of oleic acid per 1ml as a test solution;
(C) The determination method comprises the following steps: firstly, precisely measuring 1 mu l of reference solution and 1 mu l of test solution respectively, injecting the reference solution and the test solution into a gas chromatograph, then injecting components into the gas chromatograph for analysis, recording the analysis result into a chromatogram, and finally calculating the oleic acid content by peak area according to an external standard method.
Preferably, the chromatographic conditions adopt a chromatographic column with FFAP as a fixed liquid capillary column,by N 2 And H 2 As a gas for a gas chromatography carrier gas, N is added 2 The flow rate of (A) is set to 6.0ml/min to 8.0ml/min, and H is added 2 The flow rate of the method is set to be 35 ml/min-45 ml/min, a FID detector is adopted to carry out chromatographic detection on the oleic acid content in the oleic acid raw material, the temperature of the detector is set to be 275-285 ℃, the split ratio is set to be 10:1, adopting 1ul of oleic acid solution as the sample amount of a reference external standard method;
a method for detecting the content of oleic acid in an oleic acid raw material comprises the following steps:
example 1
Specificity experiments
(a) Blank solvent: appropriate amount of tetrahydrofuran is obtained;
(b) Preparation of a reference solution stock solution: weighing 17mg of oleic acid reference substance, placing the oleic acid reference substance in a 1ml measuring flask, adding tetrahydrofuran for diluting to a scale, shaking up, and finally preparing oleic acid reference substance solution stock solution;
(c) Preparation of control solutions: firstly weighing 17mg of an oleic acid reference substance, placing the oleic acid reference substance in a 10ml measuring flask, then adding tetrahydrofuran to dilute to a scale, and then shaking up to obtain an oleic acid reference substance solution;
(d) Preparation of a test solution: firstly weighing 17mg of oleic acid raw material, placing the oleic acid raw material into a 10ml measuring flask, then adding tetrahydrofuran for diluting to a scale, then shaking up, and finally preparing a test sample solution;
precisely measuring each solution, a blank solvent (tetrahydrofuran), a reference solution stock solution, a reference solution and a test solution by 1 μ l, injecting into a gas chromatograph, and recording a chromatogram, wherein the results are shown in Table 1:
TABLE 1 results of specificity test
The results show that: the signal-to-noise baseline of the blank solvent chromatogram is stable, and the system is proved to be stable in operation when a tetrahydrofuran solvent is used, has no adverse effect on the detection of the oleic acid, and has no interference with the peak of the oleic acid by the blank solvent and the system.
Example 2
Linear and range experiments
Accurately weighing 12.5mg of oleic acid reference substance, placing the oleic acid reference substance in a 25ml measuring flask, adding tetrahydrofuran to dissolve and dilute the oleic acid reference substance to a scale, and taking the linear 1; and respectively and precisely weighing 10mg, 15mg, 20mg and 25mg of oleic acid reference substances, placing the oleic acid reference substances into a 10ml measuring flask, adding tetrahydrofuran to dissolve and dilute the oleic acid reference substances to a scale, and finally taking the oleic acid reference substances as linear 2, linear 3, linear 4 and linear 5.
Precisely measuring 1 mu l of each solution under the chromatographic conditions of the embodiment 1, injecting the solution into a gas chromatograph, and recording a chromatogram; taking the sample concentration (mg/ml) as X and the oleic acid peak area (A) as Y, and making a linear regression equation, the results are shown in Table 2:
TABLE 2 oleic acid content Linear test results table
The results in Table 2 were plotted as a linear plot of the results of the oleic acid assay, as shown in FIG. 1.
The result shows that the oleic acid content is in the range of 0.5mg/ml to 2.5mg/ml, the oleic acid content and the oleic acid peak area have a remarkable linear relation, the regression equation is Y =1010.6X +24.1, r =0.9988, and compared with a manual titration method, the existing gas chromatography detection result is more accurate, the reproducibility is more excellent, and the traceability is remarkably improved.
Example 3
Repeatability test
Respectively preparing 6 parts of the test solution prepared by repeating the steps, precisely measuring 1 mu l of the test solution, injecting the measured solution into a gas chromatograph, and recording a chromatogram, wherein the detection results of the oleic acid content of the 6 parts of the test solution are shown in Table 3:
TABLE 3 results of the sample reproducibility examination
The result shows that the oleic acid content RSD in 6 parts of the oleic acid raw material is less than 1.5 percent and less than 2.0 percent, the sample repeatability is good, compared with a manual titration method, the sample repeatability is limited by external influence and personnel operation, the error of the detection data is large, the repeatability is poor, and the repeatability of the detection result can be obviously improved by using a gas chromatography method.
Example 4
Experiment of accuracy
Test solution: taking 42.5mg of oleic acid, placing the oleic acid in a 25ml measuring flask, dissolving and diluting the oleic acid to a scale by using tetrahydrofuran, shaking the oleic acid and the tetrahydrofuran uniformly, and finally preparing a test solution;
control solution: taking 42.5mg of oleic acid reference substance, placing the oleic acid reference substance in a 25ml measuring flask, dissolving and diluting the oleic acid reference substance to a scale by using tetrahydrofuran, shaking up the oleic acid and the tetrahydrofuran, and finally preparing a reference substance solution;
preparation of 80% horizontal solution: firstly, taking 17mg of an oleic acid test sample and 17mg of an oleic acid reference sample, precisely weighing, then placing in a 25ml measuring flask, dissolving and diluting to a scale by using tetrahydrofuran, shaking up a horizontal solution and oleic acid, and finally preparing 3 parts of the prepared 80% horizontal solution in parallel;
preparation of 100% horizontal solution: firstly, taking 21.25mg of an oleic acid test sample and 21.25mg of an oleic acid reference sample, precisely weighing, then placing in a 25ml measuring flask, dissolving and diluting to a scale by using tetrahydrofuran, and shaking up to obtain 3 parts in parallel;
preparation of 120% horizontal solution: firstly, taking 25.50mg of oleic acid test sample and 25.50mg of oleic acid reference sample, precisely weighing, then placing in a 25ml measuring flask, dissolving and diluting to scale by using tetrahydrofuran, and shaking up to obtain 3 parts in parallel;
precisely measuring 1 mu l of each standard concentration solution, injecting the solution into a gas chromatograph, recording a chromatogram, and respectively calculating the recovery rate of each concentration, wherein the recovery rate is between 90 and 108 percent under each concentration, and the RSD percent of 9 parts of concentration recovery rate is less than 3.0 percent. The accuracy test results are shown in table 4:
TABLE 4 accuracy check results
The result shows that the oleic acid content recovery is in the range of 90-108%, the average recovery rate is 100.67% (n = 9), the RSD is 2.1% < 3.0%, the method is in line with the regulation, the method is good in accuracy, and the sample recovery rate is adopted, namely, an oleic acid test sample and an oleic acid reference sample are added in the same proportion during the determination of the recovery rate, and the ratio of the difference value between the measured value of the reference sample and the measured value of the test sample to the addition amount is increased, so that the sample recovery rate is improved.
Example 5
Experiment of system applicability
According to the detection method of the embodiment 4, the reference substance solution is continuously injected for 5 times, the oleic acid peak area in the reference substance spectrum is calculated, the RSD of the reference substance solution is not more than 2.0%, and the specific result is shown in the table 5:
TABLE 5 oleic acid content systematic applicability test
The results show that: the number of theoretical plates of an oleic acid peak 116886 in the system is greater than 5000, the peak area RSD is 1.6% < 2.0%, the requirement is met, the system is stable in applicability operation and good in reproducibility under the method, and a stable experimental environment can be provided for sample detection.
Example 6
Experiment of solution stability
Respectively injecting the test solution and the reference solution at room temperature for 0h, 4h, 8h and 12h, precisely measuring the reference solution and 1 mu l of the test solution in each time period, injecting the reference solution and the test solution into a gas chromatograph, recording a chromatogram, calculating the peak area of the reference solution and the RSD of the test solution changing along with time, and obtaining the solution stability results shown in tables 6 and 7;
TABLE 6 test article solution stability results
TABLE 7 control solution stability results
The results show that the test solution and the reference solution of the oleic acid raw material have oleic acid content RSD of 2.7% and 2.5% < 4.0% within 0h, 4h, 8h and 12h and meet the specification, the detection results of the oleic acid test solution and the reference solution in 12 hours after the preparation is finished are basically consistent with the 0 time point and still have no significant change, the contents meet the specification within the storage time, and the quality of the oleic acid test solution and the reference solution on the experimental surface is stable within 12 h.
(VII) durability test
A method for detecting the oleic acid content in raw material oil acid adopts the chromatographic conditions as follows:
further, FFAP is selected as a chromatographic column of a fixed liquid capillary column, and N is passed through 2 And H 2 As a gas for a carrier gas for gas chromatography, N is added 2 The flow rate of (2) was set to 7.0ml/min, and H was added 2 The flow rate of the oleic acid is set to be 40ml/min, the FID detector is adopted to carry out chromatographic detection on the oleic acid content in the oleic acid raw material, and the temperature of the detector is set to be 280 ℃;
further, FFAP is selected as a chromatographic column of a fixed liquid capillary column, and N is passed through 2 And H 2 As a gas for a gas chromatography carrier gas, N is added 2 The flow rate of (2) was set to 6.0ml/min, and H was added 2 The flow rate of the oleic acid is set to be 35ml/min, the FID detector is adopted to carry out chromatographic detection on the oleic acid content in the oleic acid raw material, and the temperature of the detector is set to be 275 ℃;
further, FFAP is selected as a chromatographic column of a fixed liquid capillary column, and N is passed through 2 And H 2 As a gas for a carrier gas for gas chromatography, N is added 2 The flow rate of (2) was set to 8.0ml/min, and H was added 2 The flow rate of (2) was set to 45ml/min, using a FID detector pairCarrying out chromatographic detection on the oleic acid content in the oleic acid raw material, wherein the temperature of a detector is set to 285 ℃;
precisely weighing 17mg of oleic acid raw material under the conditions, placing the oleic acid raw material into a 10ml volumetric flask, adding tetrahydrofuran for dilution and fixing the volume to a scale to obtain a sample solution, and systematically changing the component carrier gas (N) 2 ) Flow rate. + -. 1.0ml/min and H 2 The flow rate is +/-5 ml/min, and the temperature change of a detector is +/-5 ℃; the method comprises the following steps: under different conditions, the recovery rate of the content relative to the initial condition is between 90.0 and 110.0 percent. The solution stability results are shown in tables 8 and 9.
TABLE 8 durability results (different carrier gas flow rates)
The results show that the sample solution of oleic acid carries the gas (N) during detection 2 ) Flow rate. + -. 1.0ml/min and H 2 The flow rate is +/-5 ml/min, the recovery rates of the oleic acid are 98.36% and 103.71% (standard specification: 90.0% -110.0%), the method meets the specification, the durability is good, the detection result of the content of the oleic acid meets the requirement under the conditions that the chromatographic condition is changed and the flow rates of the carrier gas (N2) and the H2 are adjusted, but the original chromatographic condition is the optimal parameter due to large variation and large floating.
TABLE 9 durability results (detector temperature)
The result shows that when the sample solution of the oleic acid is detected, the temperature of the detector is +/-5 ℃, the recovery rates of the oleic acid are 102.85 percent and 104.45 percent respectively (the standard specification is 90.0-110.0 percent), the detection method meets the specification, the durability is good, the detection result of the content of the oleic acid meets the requirement under the conditions that the chromatographic condition is changed and the temperature of the detector is adjusted, but the change has larger floating and the trend is not obvious, so that the original chromatographic condition is the optimal parameter.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (2)
1. A method for detecting the content of oleic acid in an oleic acid raw material comprises the preparation and the determination of a test sample solution, and is characterized in that:
(A) Preparing a test solution: firstly, precisely weighing 17mg of oleic acid, placing the oleic acid into a 10ml measuring flask, then adding tetrahydrofuran for diluting to a constant volume to scale, then uniformly mixing the oleic acid and the tetrahydrofuran, and finally preparing a solution containing 1.7mg of oleic acid per 1ml as a test solution;
(B) The determination method comprises the following steps: firstly, precisely measuring 1 mu l of test solution, injecting the test solution into a gas chromatograph, injecting components into the gas chromatograph for analysis, recording the analysis result into a chromatogram, and finally calculating the oleic acid content by peak area according to an external standard method.
2. A method for detecting the content of oleic acid in an oleic acid raw material is characterized by comprising the following steps: the chromatographic condition adopts a chromatographic column with FFAP as a fixed liquid capillary column and adopts N 2 And H 2 As a gas for a gas chromatography carrier gas, N is added 2 The flow rate of (A) is set to 6.0ml/min to 8.0ml/min, and H is added 2 The flow rate of the oleic acid is set to be 35 ml/min-45 ml/min, an FID detector is adopted to carry out chromatographic detection on the oleic acid content in the oleic acid raw material, the temperature of the detector is set to be 275-285 ℃, and the split ratio is set to be 10:1, adopting 1ul of oleic acid solution as the sample amount of a reference external standard method.
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