CN112255339B - Method for rapidly determining contents of three sesame lignans in sesame oil - Google Patents
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Abstract
The invention provides a method for rapidly determining the contents of three sesame lignans in sesame oil, belonging to the field of food detection. The method comprises the following steps: analyzing a standard working solution containing three types of sesame lignans by adopting a gas chromatography-mass spectrometry coupling technology to obtain retention time of each substance, monitoring ions and abundance ratio of the monitoring ions, and performing linear regression analysis on the concentration of each substance by using peak area of each substance quantitative ion in the standard working solution to obtain a standard working curve of each substance; extracting a sesame oil sample by adopting methanol, and taking supernate to obtain a solution to be detected; analyzing the liquid to be detected by adopting a gas chromatography-mass spectrometry combined technology, judging whether the sesame oil contains three types of sesame lignans according to the retention time, the monitoring ions and the abundance ratio of the monitoring ions, and calculating the concentration of each substance in the sesame oil by adopting an external standard method according to a standard working curve. The method can be used for measuring the contents of the three sesame lignans in the sesame oil simply and rapidly, and has the advantages of good selectivity, high sensitivity and high accuracy.
Description
Technical Field
The invention belongs to the field of food detection, and particularly relates to a method for rapidly determining the contents of three sesame lignans in sesame oil.
Background
Sesame oil is a fat having excellent antioxidant stability, which is related not only to its abundant tocopherol content but also to a specific class of sesame lignan compounds. Sesame lignan compounds have attracted great attention of researchers, and particularly have excellent oxidation resistance and health-care efficacy; such as promoting alcohol metabolism or liver detoxification, regulating blood lipid, and resisting cancer. The sesame lignan compounds include various substances, mainly Sesamin (Sesamin), Sesamolin (Sesamolin), Sesamol (Sesamol), Asarinin (Asarinin), and the like.
There is a transformation phenomenon between some sesame lignan compounds during the production of sesame oil. For example, under certain conditions sesamin can undergo significant epimerization during acid clay bleaching to convert to asarin. On the one hand, sesamolin is a specific compound of sesame oil, and has not been found in other vegetable oils than sesame oil; on the other hand, the cold-pressed sesame oil does not contain the asarinin, and the extracted sesame oil is easy to produce the asarinin after being refined, so that a simple and quick detection technology for the sesamin, the sesamolin and the asarinin in the sesame oil is established, and the method has practical significance for identifying the authenticity of a sesame oil sample and identifying the doped extracted sesame oil in the cold-pressed sesame oil.
Currently, Thin Layer Chromatography (TLC) and High Performance Liquid Chromatography (HPLC) are mainly used as detection methods for determining sesame lignan in sesame oil; whereas HPLC is commonly used for quantitative analysis. The TLC method is complex in operation, high in requirement on operators and incapable of accurately quantifying; the HPLC method belongs to a primary screening method, interference phenomena are easy to occur, and once the asarin detection phenomenon occurs, further technical confirmation is needed.
Disclosure of Invention
The invention aims to provide an analysis method for simultaneously measuring the contents of three sesamol lignans in sesame oil, which is simple and rapid, has good selectivity, high sensitivity and high accuracy, so as to simplify the detection procedures for measuring the contents of sesamin, sesamolin and asarum in the sesame oil and improve the analysis efficiency.
In order to achieve the above object, the present invention adopts the following technical solutions.
A method for rapidly determining the contents of three sesame lignans in sesame oil comprises the following steps:
(1) analyzing a standard working solution containing three types of sesame lignans by adopting a gas chromatography-mass spectrometry coupling technology to obtain retention time of each substance, monitoring ions and abundance ratio of the monitoring ions, and performing linear regression analysis on the concentration of each substance by using peak area of each substance quantitative ion in the standard working solution to obtain a standard working curve of each substance;
(2) extracting a sesame oil sample by adopting methanol, and taking supernate to obtain a solution to be detected;
(3) analyzing the liquid to be detected by adopting a gas chromatography-mass spectrometry combined technology, judging whether the sesame oil contains three types of sesame lignans according to retention time, monitoring ions and the abundance ratio of the monitoring ions, and calculating the concentration of each substance in the sesame oil by adopting an external standard method according to a standard working curve;
the specific conditions of the gas chromatography-mass spectrometry technology are as follows: a chromatographic column: DB-5ms elastic quartz capillary column (Agilent company, USA), the column length is 30m, the inner diameter is 0.25mm, the film thickness is 0.25 μm; column temperature: heating by program, wherein the initial temperature is 60 ℃, the temperature is increased to 270 ℃ at the speed of 30 ℃/min, the temperature is increased to 300 ℃ at the speed of 5 ℃/min, and the temperature is kept for 5 min; carrier gas: high purity helium gas; flow rate of carrier gas: 1.0 mL/min; sample injector temperature: 300 ℃; sample introduction amount: 1 mu L, no shunt sample introduction, and the opening time of a shunt valve is 1.50 min; ion source temperature: 250 ℃; quadrupole temperature: 150 ℃; ionization mode: positive chemical ion source, electron energy: 230 eV; solvent delay time: 7.00 min; and (3) data acquisition mode: the ion monitoring mode is selected in time segments.
In a preferred technical scheme, the three sesame lignans comprise sesamin, sesamolin and asarin.
In the preferred technical scheme, the method for extracting the three sesame lignans in the sesame oil by adopting methanol comprises the following steps: adding 10mL of methanol into a sesame oil sample, carrying out vortex mixing and ultrasonic dissolution, and taking supernatant fluid to obtain the liquid to be detected.
In a preferred technical scheme, the standard working solution is obtained by dissolving sesamin, sesamolin and asarum standard stock solution by using methanol and diluting the sesamolin, sesamolin and asarum standard stock solution step by step.
The sesame oil in the present invention can be classified into pressed sesame oil, water-milled sesame oil, and extracted sesame oil, etc.
According to the method, accurate qualitative and reliable quantitative detection of the three sesame lignans in the sesame oil sample can be realized simultaneously only by performing liquid-liquid extraction on the sample once, then performing separation analysis by a gas chromatography-mass spectrometry combined technology, and comparing the retention time of the obtained target object, the abundance ratio of the monitoring ions and the abundance ratio of the monitoring ions with the corresponding target object in the standard working solution. The method disclosed by the invention is simple in principle, convenient and quick in actual operation, good in selectivity, high in sensitivity and high in accuracy, the lower limit of the determination can meet the detection requirement of various countries in the world on the sesamolin compounds in the sesame oil, and particularly, the method disclosed by the invention further has the following advantages:
(1) the amount of sample required for detection is small. Only 0.1g of sample is needed to meet the detection requirement.
(2) The pretreatment is simple and quick, and batch treatment is easy to realize. The extraction and purification requirements can be realized only by one-step liquid-liquid extraction.
(3) The consumption of sample pretreatment reagent consumables is low, and the method is more environment-friendly. Only 10mL of methanol is needed to meet the pretreatment requirement, and other consumables are not consumed, so that the influence on the environment is reduced to the minimum.
(4) The gas chromatography-mass spectrometry combined technology is used for determining the sesame lignans for the first time. Firstly, a gas chromatography-mass spectrometry technology is adopted for the analysis of sesame lignans for the first time, on one hand, the gas chromatography technology can effectively separate three sesame lignans compounds, on the other hand, the gas chromatography-mass spectrometry technology belongs to the field of confirmation technology and can directly confirm a positive detection result from a liquid chromatography; secondly, a positive chemical ion source technology is adopted for detecting the sesame lignan compounds for the first time, and the positive chemical ion source technology belongs to a soft ionization technology, so that detailed molecular ion peak and adduct molecular ion peak information can be obtained when the sesame lignan compounds are analyzed, and the qualitative reliability of the method can be obviously improved; finally, the invention utilizes the characteristic that the positive chemical source technology basically has no response to the loss of the sample matrix and the column, and overcomes the defect that the electron bombardment source technology commonly used in the gas chromatography-mass spectrometry is easily interfered by the loss of the column and the components of the matrix.
Drawings
FIG. 1 is a total ion flow chromatogram of a standard working solution (each substance concentration is 1. mu.g/mL) containing sesamin, sesamolin and asarin.
FIG. 2 is a full scan mass spectrum of asarin.
FIG. 3 is a full scan mass spectrum of sesamin.
FIG. 4 is a full scan mass spectrum of sesamolin.
The specific implementation mode is as follows:
example 1 method for measuring the content of three sesame lignans in sesame oil
A method for rapidly determining the contents of three sesamolin in sesame oil specifically comprises detecting sesamin, sesamolin and asarinin. The method adopts a gas chromatography-mass spectrometry combined technology.
1. Drawing of standard working curve
The standard working curve is drawn as follows:
(1) preparation of standard working solutions
Accurately weighing 1.0mg to 10mL of sesamin standard substance in a volumetric flask, dissolving by adopting chromatographic pure methanol, and fixing the volume to a scale mark to prepare a sesamin standard stock solution with the concentration of 100 mg/L. In addition, 100mg/L sesamolin standard stock solution and 100mg/L asarin standard stock solution are prepared by the same method. Transferring 1.0mL of the standard stock solutions of the three substances into the same 10mL volumetric flask, and adopting chromatographic pure methanol to fix the volume to a scale mark to prepare a mixed standard stock solution with the concentration of each substance being 10 mg/L. And taking a 1.0 mL-10 mL volumetric flask of the mixed standard stock solution with the concentration of each substance of 10mg/L, and metering the volume to 10mL by adopting methanol to obtain the mixed standard working solution with the concentration of each substance of 1 mg/L. The 1mg/L mixed standard working solution was diluted with methanol and prepared into 500, 200, 100, 50 and 20. mu.g/L series of standard working solutions.
(2) Drawing of standard working curve and detection of sample
And analyzing the series of standard working solutions by adopting a gas chromatography-mass spectrometry combined technology to respectively obtain retention time of sesamin, sesamolin and asarum, monitoring ions and abundance ratio of the monitoring ions. In the gas chromatography-mass spectrometry technology, the specific instrument parameters are as follows: the chromatographic column is a DB-5ms elastic quartz capillary column (Agilent, USA), and has a length of 30m, an inner diameter of 0.25mm, and a film thickness of 0.25 μm. Column temperature: the temperature is programmed to rise to an initial temperature of 60 ℃ at a speed of 30 ℃/min to 270 ℃, then to 300 ℃ at a speed of 5 ℃/min, and is kept at 300 ℃ for 5 min. Carrier gas: high purity helium gas. Flow rate of carrier gas: 1.0 mL/min. Sample injector temperature: at 300 ℃. Sample introduction amount: 1 μ L, no split injection, and the split valve opening time of 1.50 min. Ion source temperature: at 250 ℃ to obtain a mixture. Quadrupole temperature: at 150 ℃. Ionization mode: positive chemical ion source, electron energy: 230 eV. Solvent delay time: 7.00 min. And (3) data acquisition mode: the ion monitoring mode is selected according to time intervals, and specific parameters are shown in table 1.
Table 1 analysis target selection ion table
Note: the band in table 1 is the quantitative ion. Coefficient of correlation R2Corresponding to a standard operating curve.
The total ion chromatogram of the standard working solution containing sesamin, sesamolin and asarum is shown in FIG. 1, and the mass chromatograms of sesamin, sesamolin and asarum are shown in FIGS. 2-4.
Taking the peak areas of the three sesame lignan quantitative ions as a vertical coordinate Y, the mass concentration of each substance as a horizontal coordinate X (the unit is mu g/L), drawing a 5-point standard working curve of each target substance within the concentration range of 20-500 mu g/L, and referring to table 1 for corresponding linear equations and related coefficients thereof.
2. Content determination of three sesame lignans in sesame oil sample
Adding accurately weighed sesame oil samples of 0.0500g (four digits after being accurate to a decimal point) into a 50mL test tube, then adding 5mL of chromatographic pure methanol, carrying out vortex mixing for 1min, carrying out ultrasonic dissolution for 10min, centrifuging for 5min at the rotating speed of 5000r/min, absorbing 1mL of supernate as a liquid to be detected, and directly feeding the liquid to be detected.
Separating and analyzing the liquid to be detected by adopting a gas chromatography-mass spectrometry combined technology, wherein the specific instrument parameters are as follows: the chromatographic column is a DB-5ms elastic quartz capillary column (Agilent, USA), and has a length of 30m, an inner diameter of 0.25mm, and a film thickness of 0.25 μm. Column temperature: the temperature is programmed to rise to an initial temperature of 60 ℃ at a speed of 30 ℃/min to 270 ℃, then to 300 ℃ at a speed of 5 ℃/min, and is kept at 300 ℃ for 5 min. Carrier gas: high purity helium gas. Flow rate of carrier gas: 1.0 mL/min. Sample injector temperature: at 300 ℃. Sample introduction amount: 1 μ L, no split injection, and the split valve opening time of 1.50 min. Ion source temperature: at 250 ℃ to obtain a mixture. Quadrupole temperature: at 150 ℃. Ionization mode: positive chemical ion source, electron energy: 230 eV. Solvent delay time: 7.00 min. And (3) data acquisition mode: the ion monitoring mode is selected in time segments.
Whether the target substance exists in the sesame oil or not needs to meet the following factors: and if the total ion current chromatograms of the solution to be detected and the standard working solution have spectral peaks at the same retention time, and the selected monitoring ions appear in the sample mass spectrogram after the background is subtracted, and the abundance ratio of the selected monitoring ions is consistent with that of the corresponding ions in the standard solution, determining that the target object is contained in the sample. And calculating the mass concentrations of the three sesame lignans in the sesame oil by adopting an external standard method according to the standard working curve. Each target in the sample solution should be within the linear range of the instrumental measurement.
3. Characteristics of the detection method
(1) Detection limit and quantification limit
The detection limit and the quantification limit researched by the invention refer to the detection Limit (LOD) and the quantification Limit (LOQ) of the instrument, and after the standard working solution is diluted step by step, the corresponding concentrations when the signal-to-noise ratio (S/N) is 3 and 10 are respectively used as the detection Limit (LOD) and the quantification Limit (LOQ) of the instrument. The detection limits of the gas chromatography-mass spectrometry technology on the asarin, the sesamin and the sesamolin are respectively 0.1, 0.1 and 0.2mg/kg (table 1), and the quantification limits of the asarin, the sesamin and the sesamolin are respectively 0.4, 0.4 and 0.8 mg/kg.
(2) Recovery and precision of the added standard
From the same soybean oil sample not containing the target substances asarin, sesamin and sesamolin, 19 samples were taken, each 0.0500g, one was randomly selected as a blank control, and the rest was averagely divided into three groups (first to third groups), each 6 samples. The blank control sample was subjected to the method described in the title 2 of this example to obtain a test solution, which was directly tested by the method described in the title 2 of this example. The first to third groups were used for the spiked recovery test, wherein 20. mu.L of a mixed standard stock solution (prepared in title 1 of this example) having a concentration of each of the substances (asarin, sesamin and sesamolin) of 10mg/L was added to each of the samples of the first group, 50. mu.L of a mixed standard stock solution (prepared in title 1 of this example) having a concentration of each of the substances (asarin, sesamin and sesamolin) of 10mg/L was added to each of the samples of the second group, 100. mu.L of a mixed standard stock solution (prepared in title 1 of this example) having a concentration of each of the substances (asarin, sesamin and sesamolin) of 10mg/L was added to each of the samples of the third group, and then the solutions to be tested were obtained by the method in title 2 of this example, and the Average Recovery (AR) and the Relative Standard Deviation (RSD) were calculated by the gas chromatography-mass spectrometry technique described above, the results are shown in Table 2.
Table 2 soybean oil standard recovery test results (%)
As can be seen from the data in Table 2, the average recovery rate of the three sesame lignan compounds is 88.9-96.9% at the three addition levels, and the relative standard deviation is lower than 4.5%, which indicates that the data accuracy and precision measured by the gas chromatography-mass spectrometry combined technology are good.
Claims (3)
1. A method for rapidly determining the contents of three sesame lignans in sesame oil is characterized by comprising the following steps:
(1) analyzing a standard working solution containing three types of sesame lignans by adopting a gas chromatography-mass spectrometry coupling technology to obtain retention time of each substance, monitoring ions and abundance ratio of the monitoring ions, and performing linear regression analysis on the concentration of each substance by using peak area of each substance quantitative ion in the standard working solution to obtain a standard working curve of each substance;
(2) extracting a sesame oil sample by adopting methanol, and taking supernate to obtain a solution to be detected;
(3) analyzing the liquid to be detected by adopting a gas chromatography-mass spectrometry combined technology, judging whether the sesame oil contains three types of sesame lignans according to retention time, monitoring ions and the abundance ratio of the monitoring ions, and calculating the concentration of each substance in the sesame oil by adopting an external standard method according to a standard working curve;
the specific conditions of the gas chromatography-mass spectrometry technology are as follows: a chromatographic column: DB-5ms elastic quartz capillary column (Agilent company, USA), the column length is 30m, the inner diameter is 0.25mm, the film thickness is 0.25 μm; column temperature: heating by program, wherein the initial temperature is 60 ℃, the temperature is increased to 270 ℃ at the speed of 30 ℃/min, the temperature is increased to 300 ℃ at the speed of 5 ℃/min, and the temperature is kept for 5 min; carrier gas: high purity helium gas; flow rate of carrier gas: 1.0 mL/min; sample injector temperature: 300 ℃; sample introduction amount: 1 mu L, no shunt sample introduction, and the opening time of a shunt valve is 1.50 min; ion source temperature: 250 ℃; quadrupole temperature: 150 ℃; ionization mode: positive chemical ion source, electron energy: 230 eV; solvent delay time: 7.00 min; and (3) data acquisition mode: selecting an ion monitoring mode in different time periods; the three sesame lignans include sesamin, sesamolin and asarum.
2. The method according to claim 1, wherein the three sesamolignans in the sesame oil are extracted with methanol by the following method: adding 10mL of methanol into a sesame oil sample, carrying out vortex mixing and ultrasonic dissolution, and taking supernatant fluid to obtain the liquid to be detected.
3. The method of claim 2, wherein the standard working solution is prepared by dissolving and diluting the standard stock solutions of sesamin, sesamolin and asarum with methanol.
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