CN113156015A - Method for analyzing content of industrial coconut oil component by internal standard method without derivatization treatment - Google Patents
Method for analyzing content of industrial coconut oil component by internal standard method without derivatization treatment Download PDFInfo
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Abstract
A method for analyzing the content of components of industrial coconut oil by an internal standard method without derivatization treatment comprises the steps of adopting a gas chromatograph to analyze, setting the temperature of a chromatographic column to be 245 ℃, and setting a temperature rise program of a column box; the carrier gas is high-purity nitrogen with the nitrogen mass content not less than 99.999%, the carrier gas flow is 40ml/min, the sample injection amount is 10 muL-20 muL, the sample injection port temperature is 230-245 ℃, the detector of the gas chromatograph is a hydrogen flame ionization detector FID, the detector temperature is 275-315 ℃, the hydrogen flow is 40ml/min, the air flow is 400ml/min, and the analysis time is 35 min; dissolving a proper amount of industrial coconut oil and tetradecane in isopropanol, fully oscillating and shaking uniformly to obtain a sample, directly injecting the sample for analysis, and calculating an analysis result by adopting an internal standard method to obtain the content of main components in the industrial coconut oil. The method does not need derivatization treatment on the industrial coconut oil, and has the advantages of simple and convenient operation, short analysis time, accurate analysis result, high stability and good reproducibility.
Description
Technical Field
The invention belongs to the technical field of fatty acid detection, and particularly relates to a method for analyzing the content of industrial coconut oil components by an internal standard method without derivatization treatment.
Background
Coconut oil is a mixed oil composed of multiple types of medium-chain fatty acids, is easy to be rapidly absorbed by human bodies due to the characteristics of small molecular weight and easy oxidation, and can be used for treating children malnutrition by adding the coconut oil into diet. Experimental studies on mice have shown that coconut oil has anticancer effect, and blending hydrogenated coconut oil in diet can inhibit liver disease occurrence and prevent and treat colon cancer and breast tumor, so coconut oil is known as the most healthy edible oil in the world.
With the rapid development of daily chemical industry and fine chemical industry, deep-processed products taking coconut oil as a raw material are widely applied to the fields of food processing, textile industry, cosmetics, washing products and the like, and the distribution of the content of each fatty acid component in the coconut oil is a basis for measuring the quality of the coconut oil and particularly a basis for extending the industrial chain of the deep-processing of the coconut oil, so that a plurality of scholars widely research methods for analyzing fatty acids including the coconut oil.
Chinese patent CN201910327657.1 describes a method for analyzing fatty acids in soybean milk by gas chromatography-mass spectrometry, patent cn201510467654.x describes a method for analyzing fatty acid components in macadamia nut oil, and patent CN201910788750.2 describes a semi-quantitative analysis method for amino acids, acyl carnitine and fatty acids. The three methods use different devices to perform qualitative and quantitative analysis on the fatty acid, but the fatty acid can be analyzed only after derivatization treatment, the possibility of incomplete derivatization (incomplete methyl esterification) exists in the derivatization treatment process, so that analysis errors are caused, the derivatization work is complex, the detection period is long, and the analysis efficiency is low.
Disclosure of Invention
The invention aims to solve the technical problems, and provides a method for analyzing the content of components of industrial coconut oil by an internal standard method, which does not need to perform derivatization treatment on coconut oil, is simple and convenient to operate, has accurate analysis result, high stability and good reproducibility.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the method for analyzing the content of the components of the industrial coconut oil by an internal standard method without derivatization treatment adopts a gas chromatograph to analyze, and comprises the following steps:
(1) starting up: opening a gas valve of the gas chromatograph, checking a gas path, supplying carrier gas and other gases, performing leakage test on the gas chromatograph, keeping the air tightness of the instrument, turning on a power supply of the gas chromatograph, turning on a power supply of a computer for controlling the gas chromatograph, and pre-installing gas chromatograph data management software Labsolutions on the computer;
(2) starting software: double-clicking a LaSbases icon on a Windows desktop of a computer, starting software, double-clicking a gas chromatograph interface, selecting an instrument type GC, finding a required instrument and double-clicking for connection;
(3) setting analysis parameters: the temperature of the chromatographic column is 245 ℃, the temperature raising program of the column box is the initial temperature of 150 ℃, the temperature is kept for 5min, the gradient is 10 ℃/min, the equilibrium temperature is 245 ℃, and the keeping time is 30 min; the carrier gas is high-purity nitrogen with the nitrogen mass content not less than 99.999%, the carrier gas flow is 40ml/min, the sample injection amount is 10 muL-20 muL, the sample injection port temperature is 230-245 ℃, the detector of the gas chromatograph is a hydrogen flame ionization detector FID, the detector temperature is 275-315 ℃, the hydrogen flow is 40ml/min, the air flow is 400ml/min, and the analysis time is 35 min;
(4) preparing a sample: the industrial coconut oil sample does not need to be subjected to derivatization treatment, a proper amount of industrial coconut oil and tetradecane are dissolved in isopropanol and are fully shaken and shaken up, and the mass ratio of the industrial coconut oil to the tetradecane is 16:1-4: 1;
(5) sample injection analysis: shaking the prepared sample evenly, and directly injecting 10-20 mu L of sample by using a micro sample injector;
(6) and (3) calculating: calculating the analysis result by adopting an internal standard method to obtain the content of each component of the industrial coconut oil;
(7) cooling: setting a temperature reduction program, wherein the temperature of a sample introduction chamber is 25 ℃, the temperature of an FID detector is 25 ℃, the temperature of a chromatographic column is 25 ℃, the temperature of the sample introduction chamber and the chromatographic column is reduced to be below 50 ℃, and the temperature of the FID detector is reduced to be below 100 ℃;
(8) shutdown: after cooling, clicking a 'stop GC' button in a main menu on the left side of a Labsolutions software interface on a computer, closing the Labsolutions software, closing a power supply of a gas chromatograph and a power supply of the computer, and closing a gas valve of the gas chromatograph.
The gas chromatograph is GC-2010 and is provided with a hydrogen flame ionization detector FID and a DB-FFAP capillary chromatographic column.
The components of industrial coconut oil are caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, linoleic acid, oleic acid and stearic acid.
The method can directly analyze and obtain the content of the main components in the industrial coconut oil without derivatization treatment of the industrial coconut oil, has simple and convenient operation, short analysis time, accurate analysis result, high stability and good reproducibility, and an internal standard method is not influenced by the accuracy of manual sample injection.
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FIG. 1 is a sample analysis report of one embodiment of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example 1
A method for analyzing the content of industrial coconut oil components by internal standard method without derivatization treatment comprises loading hydrogen flame ionization detector FID and DB-FFAP (30# m 0.53# mm 0.25 μm) capillary chromatographic column by GC-2010 gas chromatograph. The analysis was carried out as follows:
(1) starting up: opening a gas valve of the gas chromatograph, checking a gas path, supplying carrier gas and other gases, performing leakage test on the gas chromatograph, keeping the air tightness of the instrument, turning on a power supply of the gas chromatograph, turning on a power supply of a computer for controlling the gas chromatograph, and pre-installing Labsolutions of data management software of the gas chromatograph on the computer.
(2) Starting software: double-clicking the LaSbases icon on the Windows desktop of the computer, starting software, double-clicking the interface of the gas chromatograph, selecting the type GC of the instrument, finding the required instrument and double-clicking for connection.
(3) Setting analysis parameters: the temperature of the chromatographic column is 245 ℃, the temperature raising program of the column box is the initial temperature of 150 ℃, the temperature is kept for 5min, the gradient is 10 ℃/min, the equilibrium temperature is 245 ℃, and the keeping time is 30 min; the carrier gas is high-purity nitrogen with the nitrogen content not lower than 99.999 percent by mass, the carrier gas flow is 40ml/min, the sample injection amount is 10 mu L, the sample injection port temperature is 230 ℃, the detector of the gas chromatograph is a hydrogen flame ionization detector FID, the detector temperature is 300 ℃, the hydrogen flow is 40ml/min, the air flow is 400ml/min, and the analysis time is 35 min.
The parameter setting can obtain the best analysis effect. And if the sample amount is too small, a chromatographic peak cannot be obtained by GC detection, and if the sample amount is too large, the chromatographic column is overloaded, and the analysis result is inaccurate due to the fact that a tailing peak is obtained. The temperature of the sample inlet is too low, and impurities with high boiling point can not be gasified, so that the analysis result is inaccurate. The temperature of the chromatographic column is set to 245 ℃, so that the service life of the chromatographic column can be prolonged, and the rapid analysis can be realized. In order to prevent the gasified sample from entering the chromatographic column to cause condensation, the temperature of the sample inlet is set between 230 ℃ and 245 ℃. The set flow of nitrogen, hydrogen and air can avoid influencing the retention time of chromatographic peaks as much as possible, and the retention time of chromatographic peaks is prevented from being advanced or retarded. The invention adopts the FID detector which is suitable for the analysis of industrial coconut oil, and sets the temperature of the detector to be 275-315 ℃, and other detectors are suitable for the analysis of industrial coconut oil.
(4) Preparing a sample: taking an industrial coconut oil sample 1, dissolving a proper amount of industrial coconut oil and tetradecane in isopropanol without derivatization treatment, and fully shaking up. The mass ratio of the industrial coconut oil to the tetradecane is 10:1, and the mass of the isopropanol is 8 times of the sum of the mass of the industrial coconut oil and the tetradecane.
The tetradecane is selected as a standard substance of an internal standard method, because the retention time of the chromatographic peak of the tetradecane is similar to that of the chromatographic peak of each component of the industrial coconut oil through experiments, and the tetradecane has good separation degree. Isopropanol was used as the solvent in the internal standard method because it was found experimentally that tetradecane and technical coconut oil are readily soluble in isopropanol, and that isopropanol has a low boiling point and its chromatographic peaks have good separation from the technical coconut oil component peaks and tetradecane.
(5) Sample injection analysis: shaking the prepared sample evenly, directly injecting 10 mu L of sample by using a microsyringe, and the analysis report is shown in figure 1:
in a chromatogram of a sample 1 in an analysis report, a first chromatographic peak is isopropanol as a solvent, a second chromatographic peak is tetradecane, and a third chromatographic peak and the following chromatographic peaks are caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, linoleic acid, oleic acid and stearic acid in sequence.
(6) After the gas chromatography conditions are operated according to the steps (1), (2) and (3), taking appropriate amount of chromatographically pure caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, linoleic acid, oleic acid and stearic acid samples, respectively adding tetradecane serving as a standard substance and isopropanol serving as a solvent into each sample, shaking uniformly, then respectively injecting 10 mu L of sample, analyzing to obtain chromatograms of caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, linoleic acid, oleic acid and stearic acid, and comparing and analyzing the 8 chromatograms with the chromatogram of the sample 1 obtained in the step (5) to obtain the peak emergence sequence of 8 main components with the mass content of more than 0.2 percent contained in the industrial coconut oil sample, wherein the peak emergence sequence is caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, linoleic acid, oleic acid and stearic acid in turn. Thus obtaining the contents of caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, linoleic acid, oleic acid and stearic acid contained in the industrial coconut oil. The experiment is repeated for 5 times, the analysis result is calculated by adopting an internal standard method, and the relative standard deviation RSD of the caprylic acid, the capric acid, the lauric acid, the myristic acid, the palmitic acid, the linoleic acid, the oleic acid and the stearic acid is as follows in sequence: 0.263%, 0.114%, 0.237%, 0.112%, 0.098%, 0.195%, 0.339%, 0.090%. The results of the analysis are proved to be accurate, high in stability and good in reproducibility.
(7) Cooling: setting a temperature reduction program, wherein the temperature of a sample introduction chamber is 25 ℃, the temperature of an FID detector is 25 ℃, the temperature of a chromatographic column is 25 ℃, the temperature of the sample introduction chamber and the chromatographic column is reduced to be below 50 ℃, and the temperature of the FID detector is reduced to be below 100 ℃.
(8) Shutdown: after cooling, clicking a 'stop GC' button in a main menu on the left side of a Labsolutions software interface on a computer, closing the Labsolutions software, closing a power supply of a gas chromatograph and a power supply of the computer, and closing a gas valve of the gas chromatograph.
The analytical results were corrected using the internal standard method, and the calibration curves for the various components of industrial coconut oil were determined as follows:
after the gas chromatography conditions are operated according to the steps (1), (2) and (3), 5 groups of internal standard substance tetradecane samples and 8 groups of chromatographic pure samples with different concentration gradients are prepared, the mass ratio of the tetradecane to each component is respectively 1:2, 2:3, 1:1, 3:2 and 2:1, then a proper amount of isopropanol is added for full dissolution, the mixture is shaken up and then sampled for 10 mu L, and each sample is repeatedly analyzed for 3 times. After obtaining the chromatogram, respectively calculating the mass ratio mi/ms of each component and the internal standard substance in each proportion, then calculating the peak area average value of each component in the 3-time chromatogram of each sample and the peak area average value of the internal standard substance, then calculating the ratio Ai/As of the peak area of each component and the peak area of the internal standard substance, taking mi/ms As the abscissa and Ai/As As the ordinate, and taking the obtained 5 point cross (0, 0) As a linear trend graph to respectively obtain the following correction curves: the calibration curve for caprylic acid is y-0.7881 x, R20.9991; the calibration curve of capric acid is y-0.9166 x, R20.9996; the calibration curve of lauric acid is y-0.9742, R20.9991; the calibration curve for myristic acid is y-0.9839 x, R20.9998; the calibration curve for palmitic acid is y-0.9616 x, R20.9997; the calibration curve of linoleic acid is y ═0.8189x，R20.9993; the calibration curve of oleic acid is y-0.8967 x, R20.9999; the calibration curve for stearic acid is y ═ 0.929x, R2＝0.9997。
Shaking the sample 1 evenly, injecting 10 mu L of sample by using a microsyringe, repeating the experiment for 5 times, and calculating the analysis result by adopting an internal standard method, wherein the relative standard deviation RSD of the caprylic acid, the capric acid, the lauric acid, the myristic acid, the palmitic acid, the linoleic acid, the oleic acid and the stearic acid is 0.044%, 0.015%, 0.206%, 0.047%, 0.069%, 0.022%, 0.065% and 0.017% in sequence. The relative standard deviation RSD of each component is less than 0.38 percent, which proves that the method has high stability of analysis results, good reproducibility and reliable method.
Example 2
The methods of the steps (1) and (2) are the same as those of example 1;
(3) setting analysis parameters: the temperature of the chromatographic column is 245 ℃, the temperature raising program of the column box is the initial temperature of 150 ℃, the temperature is kept for 5min, the gradient is 10 ℃/min, the equilibrium temperature is 245 ℃, and the keeping time is 30 min; the carrier gas is high-purity nitrogen with the nitrogen content not lower than 99.999 percent by mass, the carrier gas flow is 40ml/min, the sample injection amount is 15 mu L, the sample injection port temperature is 245 ℃, the detector of the gas chromatograph is a hydrogen flame ionization detector FID, the detector temperature is 275 ℃, the hydrogen flow is 40ml/min, the air flow is 400ml/min, and the analysis time is 35 min;
(4) preparing a sample: taking a proper amount of industrial coconut oil sample 2 and tetradecane, dissolving in isopropanol, fully shaking and shaking uniformly, wherein the mass ratio of the industrial coconut oil to the tetradecane is 16:1, and the mass of the isopropanol is 10 times of the mass sum of the industrial coconut oil and the tetradecane;
(5) sample injection analysis: shaking the prepared sample evenly, and directly injecting 15 mu L of sample by using a microsyringe;
(6) and (3) calculating: and calculating the contents of caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, linoleic acid, oleic acid and stearic acid in the industrial coconut oil by adopting an internal standard method according to the analysis result. The experiment is repeated for 5 times, and the relative standard deviation RSD of the caprylic acid, the capric acid, the lauric acid, the myristic acid, the palmitic acid, the linoleic acid, the oleic acid and the stearic acid is calculated by an internal standard method, and the RSD is 0.263%, 0.114%, 0.237%, 0.112%, 0.098%, 0.195%, 0.339% and 0.090% in sequence.
Example 3
The methods of the steps (1) and (2) are the same as those of example 1;
(3) setting analysis parameters: the temperature of the chromatographic column is 245 ℃, the temperature raising program of the column box is the initial temperature of 150 ℃, the temperature is kept for 5min, the gradient is 10 ℃/min, the equilibrium temperature is 245 ℃, and the keeping time is 30 min; the carrier gas is high-purity nitrogen with the nitrogen content not lower than 99.999 percent by mass, the carrier gas flow is 40ml/min, the sample injection amount is 18 mu L, the sample injection port temperature is 230 ℃, the detector of the gas chromatograph is a hydrogen flame ionization detector FID, the detector temperature is 300 ℃, the hydrogen flow is 40ml/min, the air flow is 400ml/min, and the analysis time is 35 min;
(4) preparing a sample: taking a proper amount of industrial coconut oil sample 2 and tetradecane, dissolving in isopropanol, fully shaking and shaking uniformly, wherein the mass ratio of the industrial coconut oil to the tetradecane is 6:1, and the mass of the isopropanol is 19 times of the mass sum of the industrial coconut oil and the tetradecane;
(5) sample injection analysis: shaking the prepared sample evenly, and directly injecting 18 mu L of sample by using a microsyringe;
(6) and (3) calculating: and calculating the contents of caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, linoleic acid, oleic acid and stearic acid in the industrial coconut oil by adopting an internal standard method according to the analysis result. The experiment is repeated for 5 times, and the relative standard deviation RSD of the caprylic acid, the capric acid, the lauric acid, the myristic acid, the palmitic acid, the linoleic acid, the oleic acid and the stearic acid is calculated by an internal standard method, wherein the relative standard deviation RSD of the caprylic acid, the capric acid, the lauric acid, the myristic acid, the palmitic acid, the linoleic acid, the oleic acid and the stearic acid is 0.213%, 0.161%, 0.153%, 0.122%, 0.197%, 0.192%, 0.376% and 0.285% in sequence.
Example 4
The methods of the steps (1) and (2) are the same as those of example 1;
(3) setting analysis parameters: the temperature of the chromatographic column is 245 ℃, the temperature raising program of the column box is the initial temperature of 150 ℃, the temperature is kept for 5min, the gradient is 10 ℃/min, the equilibrium temperature is 245 ℃, and the keeping time is 30 min; the carrier gas is high-purity nitrogen with the nitrogen content not lower than 99.999 percent by mass, the carrier gas flow is 40ml/min, the sample injection amount is 20 mu L, the sample injection port temperature is 240 ℃, the detector of the gas chromatograph is a hydrogen flame ionization detector FID, the detector temperature is 315 ℃, the hydrogen flow is 40ml/min, the air flow is 400ml/min, and the analysis time is 35 min;
(4) preparing a sample: taking a proper amount of industrial coconut oil sample 2 and tetradecane, dissolving in isopropanol, fully shaking and shaking uniformly, wherein the mass ratio of the industrial coconut oil to the tetradecane is 4:1, and the mass of the isopropanol is 5 times of the mass sum of the industrial coconut oil and the tetradecane;
(5) sample injection analysis: shaking the prepared sample evenly, and directly injecting 20 mu L of sample by using a microsyringe;
(6) and (3) calculating: and calculating the contents of caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, linoleic acid, oleic acid and stearic acid in the industrial coconut oil by adopting an internal standard method according to the analysis result. The experiment is repeated for 5 times, and the relative standard deviation RSD of the caprylic acid, the capric acid, the lauric acid, the myristic acid, the palmitic acid, the linoleic acid, the oleic acid and the stearic acid is calculated by an internal standard method, wherein the relative standard deviation RSD of the caprylic acid, the capric acid, the lauric acid, the myristic acid, the palmitic acid, the linoleic acid, the oleic acid and the stearic acid is 0.163%, 0.111%, 0.135%, 0.088%, 0.079%, 0.153%, 0.312% and 0.188% in sequence.
Claims (3)
1. The method for analyzing the content of the components of the industrial coconut oil by an internal standard method without derivatization treatment is characterized in that a gas chromatograph is adopted for analysis, and the method is carried out according to the following steps:
(1) starting up: opening a gas valve of the gas chromatograph, checking a gas path, supplying carrier gas and other gases, performing leakage test on the gas chromatograph, keeping the air tightness of the instrument, turning on a power supply of the gas chromatograph, turning on a power supply of a computer for controlling the gas chromatograph, and pre-installing gas chromatograph data management software Labsolutions on the computer;
(2) starting software: double-clicking a LaSbases icon on a Windows desktop of a computer, starting software, double-clicking a gas chromatograph interface, selecting an instrument type GC, finding a required instrument and double-clicking for connection;
(3) setting analysis parameters: the temperature of the chromatographic column is 245 ℃, the temperature raising program of the column box is the initial temperature of 150 ℃, the temperature is kept for 5min, the gradient is 10 ℃/min, the equilibrium temperature is 245 ℃, and the keeping time is 30 min; the carrier gas is high-purity nitrogen with the nitrogen mass content not less than 99.999%, the carrier gas flow is 40ml/min, the sample injection amount is 10 muL-20 muL, the sample injection port temperature is 230-245 ℃, the detector of the gas chromatograph is a hydrogen flame ionization detector FID, the detector temperature is 275-315 ℃, the hydrogen flow is 40ml/min, the air flow is 400ml/min, and the analysis time is 35 min;
(4) preparing a sample: the industrial coconut oil sample does not need to be subjected to derivatization treatment, a proper amount of industrial coconut oil and tetradecane are dissolved in isopropanol and are fully shaken and shaken up, and the mass ratio of the industrial coconut oil to the tetradecane is 16:1-4: 1;
(5) sample injection analysis: shaking the prepared sample evenly, and directly injecting 10-20 mu L of sample by using a micro sample injector;
(6) and (3) calculating: calculating the analysis result by adopting an internal standard method to obtain the content of each component of the industrial coconut oil;
(7) cooling: setting a temperature reduction program, wherein the temperature of a sample introduction chamber is 25 ℃, the temperature of an FID detector is 25 ℃, the temperature of a chromatographic column is 25 ℃, the temperature of the sample introduction chamber and the chromatographic column is reduced to be below 50 ℃, and the temperature of the FID detector is reduced to be below 100 ℃;
(8) shutdown: after cooling, clicking a 'stop GC' button in a main menu on the left side of a Labsolutions software interface on a computer, closing the Labsolutions software, closing a power supply of a gas chromatograph and a power supply of the computer, and closing a gas valve of the gas chromatograph.
2. The method for analyzing the content of industrial coconut oil components by the internal standard method without derivatization treatment as claimed in claim 1, wherein the gas chromatograph is GC-2010 and is equipped with a hydrogen flame ionization detector FID and a DB-FFAP capillary chromatographic column.
3. The method for analyzing the content of industrial coconut oil component by the internal standard method without derivatization treatment according to claim 1 or 2, wherein each component of the industrial coconut oil is caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, linoleic acid, oleic acid, stearic acid.
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Application publication date: 20210723 |