CN116337800A - Iris seed oil quality evaluation method based on ATR-FTIR - Google Patents
Iris seed oil quality evaluation method based on ATR-FTIR Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/55—Specular reflectivity
- G01N21/552—Attenuated total reflection
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention discloses an ATR-FTIR-based iris seed oil quality evaluation method, belongs to the technical field of quality evaluation, and combines an ATR-FTIR method and a chemometry method to establish a quantitative model of total polyphenol content, main unsaturated fatty acid and saturated fatty acid ratio and antioxidant capacity of iris seed oil. The invention utilizes ATR-FTIR to determine the applicability quantitative model of quality parameters such as Total Polyphenol Content (TPC), main unsaturated fatty acid and saturated fatty acid ratio (U/S), antioxidant Capacity (AC) and the like of the iris seed oil, can effectively evaluate the quality of the iris seed oil and promote the stable development of the quality of the iris seed oil product.
Description
Technical Field
The invention relates to the technical field of quality evaluation, in particular to an Iris seed oil quality evaluation method based on ATR-FTIR.
Background
Iris lactea pall.var.chinensis (Fisch.) Koidz.) is a variety of Iridaceae Iris white Iris, perennial herb perennial root plant. Distributed in korea, russia, india and china. In China, except for the coastal zone of southeast, more than twenty provinces are distributed in a large scale, and the resource amount is huge. The species mainly grows on barren lands, roadside hillside grasslands, especially on salinized grasslands which are overgrazed. Has better salt tolerance and ornamental value, and also has tolerance to heavy metal elements such as lead, cadmium and the like. Is often used as a saline-alkali indicator of a saline-alkali grassland, and is used for vegetation recovery in the saline-alkali grassland and petroleum pollution areas. Besides ecological value, iris seed has high pharmaceutical value.
It is reported that "Anka" extracted from the seed coat of Iris seed is mainly used as a radiation sensitizer, and the seed core is discarded as an industrial byproduct. In recent years, iris seed has received attention for its high oil content. The oil content of Iris seed kernel is about 10.56%, wherein fatty acids are mainly linoleic acid (65.35%) and oleic acid (28.51%) after Soxhlet extraction. At present, the determination of the content and activity of the compound in the iris seed oil mainly depends on chemical methods, such as gas chromatography-mass spectrometry (GC-MS), and the methods have the problems of long time consumption and large pollution, so that a quick, accurate and environment-friendly detection method is necessary to be established, the comprehensive control of the iris seed oil is realized, more sufficient basis is provided for the quality evaluation of the iris seed oil, and the method has important significance.
ATR-FTIR has the advantages of simplicity, rapidness, no damage, and time and effort saving, and researchers have attempted to apply this technique to characterization and compound identification of different oils. However, no quality control of Iris seed oil has been reported to date with ATR-FTIR.
Disclosure of Invention
The invention aims to solve the problems of the prior art for measuring compounds in iris seed oil and provides an ATR-FTIR-based iris seed oil quality evaluation method.
The aim of the invention is realized by the following technical scheme: the quality evaluation method of Iris seed oil based on ATR-FTIR comprises the following steps:
measuring the content of quality evaluation components to be measured in iris seed oil;
collecting ATR-FTIR spectra;
preprocessing by constant, standard Normalized Variable (SNV) and Multiplicative Scatter Correction (MSC) methods;
establishing a principal component regression prediction model of TPC, U/S and AC;
evaluating the performance of the model by adopting the correlation coefficient of the calibration set, the correlation coefficient of the prediction set, the root mean square error of the calibration set, the root mean square error of the prediction set and the residual prediction deviation;
and (3) analyzing the correlation between the actual value and the predicted value, wherein the correlation coefficient of the calibration set and the predicted set of the built model is close to 1, and the quality evaluation of the iris seed oil can be carried out by using the model.
In a preferred embodiment of the present invention, the preparation method of the iris seed oil comprises: pulverizing and sieving Iris seed with seed coat removed, and extracting with supercritical carbon dioxide.
In a preferred embodiment of the present invention, the conditions for supercritical carbon dioxide extraction are: extracting at 40-50 deg.c and 25-34 MPa for 70-95 min.
In a preferred embodiment of the present invention, when the method is used for quality evaluation of iris seed oil, the determination of the content of the component to be quality evaluated in each Tibetan medicine sample specifically includes: detecting the total polyphenol content, detecting the fatty acid component, and detecting the in vitro antioxidant activity.
As a preferred embodiment of the invention, the total polyphenol content detection, fatty acid component determination and in-vitro antioxidant activity detection can be carried out by adopting the conventional technical means in the field.
In a preferred embodiment of the present invention, the method for detecting the total polyphenol content comprises the following steps: and (3) weighing Iris seed oil, dissolving in a solvent, performing column extraction, eluting with an alcohol solution, collecting an eluent, evaporating the solvent, performing ultrasonic dissolution on residues, and using gallic acid working solutions with different concentrations to establish a standard curve so as to calculate the content of total polyphenol.
In a preferred embodiment of the present invention, the method for determining the fatty acid composition comprises: weighing Iris seed oil, adding KOH-CH 3 Reflux of OH solution until oil drops disappear, adding BF 3 -CH 3 Continuously refluxing the OH solution for 1-5 min, cooling to room temperature, adding an organic solvent and a saturated sodium chloride solution, standing for layering, and suckingAdding the upper layer solution into anhydrous sodium sulfate, shaking and standing, sucking the upper layer solution, and measuring by adopting GC-MS;
further, the GC-MS measurement conditions are as follows: adopting a capillary chromatographic column, wherein the temperature of a sample inlet is 275-285 ℃; the carrier gas is helium; the sample injection amount is 0.5-2 mu L; the split ratio (15-30) is 1, the temperature programmed is kept at 40-55 ℃ for 0.5-3 min, the temperature is increased to 170-180 ℃ at 20-30 ℃/min, the temperature is increased to 220-240 ℃ at 2-6 ℃/min, and the temperature is kept for 3-6 min; the ionization mode is electron bombardment ion source, column head pressure is 220-235 KPa, and transmission line temperature is 270-285 ℃.
In a preferred embodiment of the present invention, the method for detecting in vitro antioxidant activity comprises the following steps: preparing Iris seed oil with different concentrations by using ethanol and petroleum ether, preparing positive control and blank control, adding DPPH-ethanol solution into the Iris seed oil, measuring absorbance after light-shielding reaction, and calculating the DPPH free radical clearance of the Iris seed oil.
In a preferred embodiment of the invention, the spectrum is 4000-400 cm when the ATR-FTIR spectrum is acquired -1 Scanning for 5-12 times in the region of (2), the scanning time is 28-37 s, the resolution is 4cm -1 With air as the background.
In a preferred embodiment of the invention, the samples are randomly divided into calibration and prediction groups at a ratio of 2:1 during the pretreatment.
In a preferred embodiment of the present invention, modeling ranges of the TPC and AC models are respectively: 1567-1800 cm -1 、1567～1804cm -1 ；
The modeling interval of the U/S model is 2800-3040 cm -1 And 640-1700 cm -1 。
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, 9 crowd-based iris seed samples are collected in Qinghai province in China, after the iris seed oil is quantified by adopting a supercritical fluid extraction method, an attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) technology is used, infrared spectra of the iris seed oil are collected, an optimal prediction model for measuring the Total Polyphenol Content (TPC), the ratio (U/S) of main unsaturated fatty acid to saturated fatty acid and the Antioxidant Capacity (AC) content of the iris seed oil is established, and the total polyphenol, fatty acid and antioxidant activity content in the iris seed oil can be rapidly detected by adopting the model constructed by the invention, so that the quality of the iris seed oil can be rapidly evaluated, and the quality evaluation of the iris seed oil can be realized. Compared with detection methods such as liquid phase mass spectrum and gas phase mass spectrum, the method has the advantages of high efficiency, safety, environmental protection, high flux, simple equipment, low cost and the like.
Drawings
FIG. 1 is an iris seed sampling information diagram, P-crowd;
FIG. 2 is a graph showing oil yield and total polyphenol content of Iris lactea seeds of different dwelling groups;
FIG. 3 is a graph showing antioxidant activity of Iris seed oil of different dwelling groups;
FIG. 4 is an average ATR-FTIR plot;
FIG. 5 is a PCR model of three index indicators, A is a total polyphenol content model; b, U/S model; and C, an antioxidant capacity model.
Detailed Description
The following description of the embodiments of the present invention will be made apparent and fully understood from the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
It should be noted that the experimental methods used in the following examples are conventional methods unless otherwise specified, and the materials, reagents, etc. used in the following examples are commercially available unless otherwise specified.
The terms "comprising," "including," "having," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, or article of manufacture that comprises a list of elements is not necessarily limited to only those elements, but may include other elements not expressly listed or inherent to such composition, step, method, or article of manufacture.
Example 1
1. Materials and methods
1.1 materials
A total of 9 clusters of iris seeds were collected in Qinghai province of china for 9 months and detailed information on the sampling population is provided in figure 1. These samples were identified by the institute of high-speed biological northwest of the national academy of sciences as dry mature seeds of Iris lactea pall. Credential specimens (accession numbers: 2018-144, 2018-145, and 2018-146) were deposited at the northwest high-protozoa institute. The kernel and the powder thereof are obtained through two steps of crushing.
1.2 method
1.2.1 obtaining Iris seed oil
The grease content of Iris pallas is quantified by supercritical fluid extraction. In an HA221-40-12 supercritical extractor (Nantong Yichuang laboratory instruments Co., ltd., nantong, china), spare kernel powder (500 g) of Iris irish was extracted with supercritical carbon dioxide, and extracted at 45℃and a pressure of 28.5MPa for 81 minutes.
1.2.2 detection of Total Polyphenol content
(1) 2.00g of iris seed oil is precisely weighed and dissolved in 6mL of normal hexane, the solution is passed through a glycol-based solid phase extraction column at a flow rate of 1.0mL/min, then the extraction column is leached by 10mL of normal hexane, all effluent liquid is discarded, finally 10mL of methanol is used for eluting, all the eluent is collected, the solvent is rotationally evaporated in a water bath at 45 ℃, the residue is dissolved in 2mL of methanol-water solution, ultrasonic dissolution is carried out for 1min, and freezing is carried out for 16h at-18 ℃. Centrifuging at 10000rpm for 5min at 4deg.C, and collecting supernatant.
(2) Drawing a standard curve: gallic acid working solutions at concentrations of 10, 20, 30, 40 and 50 μg/mL were respectively prepared to establish a standard curve. 1mL of gallic acid working solutions with different concentrations are respectively taken, and then 0.5mL of Fu Lin Fen reagent, 2mL of 7.5% sodium carbonate solution and 6.5mL of water are added. Shaking 1mAfter in, the reaction was carried out in a water bath at 70℃for 30min, and then absorbance was measured at a wavelength of 750 nm. A standard curve with gallic acid concentration (x) as an independent variable and absorbance (y) as a dependent variable was drawn as follows, y= -0.00278+0.0088x (r) 2 = 0.9992). After measuring the sample to be measured by the above method, the content of total polyphenols was calculated using gallic acid equivalent according to the following formula:
X＝[(c×2/1000)/m]×1000
x is the content of total polyphenol in the oil, and the unit is mg/kg; c is the total polyphenol concentration measured according to a standard curve in μg/mL.2 is the constant volume of the eluate after evaporation in mL. m is the mass of the sample and the unit is g.
1.2.3 fatty acid constituent determination
(1) Preparation of the samples: 0.01g of Iris seed oil is weighed into a 100mL flat bottom flask, 8mL of 2% KOH-CH is added 3 The OH solution was refluxed on a water bath at 80℃until the oil droplets disappeared, and 7ml of 15% BF was added from the upper end of the reflux condenser 3 -CH 3 And (3) continuously refluxing the OH solution for 2min, cooling to room temperature, accurately adding 10mL of n-heptane, shaking for 2min, adding saturated NaCl solution, shaking, standing, layering, sucking 5mL of the n-heptane extract of the upper layer into a test tube, adding about 3-5 g of anhydrous sodium sulfate, shaking for 1min, standing for 5min, and sucking the upper layer solution into a sample bottle to be measured.
(2) GC-MS analysis conditions: the capillary chromatographic column is Agilent DB-FFPA column (100 m×0.25mm i.d.0.25 μm); the temperature of the sample inlet is 280 ℃; the carrier gas is helium; the sample injection amount is 1 mu L; split ratio 20:1, a step of; heating to 50deg.C for 1min, heating to 175 deg.C at 25deg.C/min, heating to 230deg.C at 4deg.C/min, and maintaining for 5min; the ionization mode is electron bombardment ion source (EI); the column head pressure is 230KPa; the transmission line temperature was 280 ℃. Analyzing fatty acid components of Iris seed oil by GC-MS method, processing data by area normalization method, and analyzing main components in the map by searching Nist14 database.
1.2.4 in vitro antioxidant Activity assay
Stock solutions of oils (1.75, 3.5, 7, 14 and 28 mg/mL) were formulated with ethanol and petroleum ether (2:1), positive control vitamin C (1.75, 3.5, 7, 14 and 28 mg/mL) and DPPH solutions (0.2 mmol/L) were prepared with ethanol. In addition, absolute ethanol was used as a blank. Taking 2mL of iris seed oil solution with different mass concentration, adding 2mL of DPPH-ethanol solution with 0.2m mol/mL respectively, uniformly mixing, carrying out light-proof reaction at normal temperature for 30min, measuring absorbance (As) at wavelength of 517nm, taking absolute ethyl alcohol As blank control (Ab), taking Vc As positive control, and calculating the clearance rate of DPPH according to the following formula.
DPPH radical clearance = 1-As/Ab x 100%
According to the clearance rate of iris seed oil with different mass concentrations and combining with SPSS25.0 data processing software, the mass concentration of the solution required when the clearance rate of DPPH free radical is50 percent is calculated, namely IC 50 In IC 50 The value represents the DPPH free radical eliminating capacity of iris seed oil and IC 50 The smaller the value, the stronger the purge capability.
Acquisition of 1.2.5ATR-FTIR spectra
ATR-FTIR spectra for each sample were collected by fourier transform infrared spectrometer (Nicolet iS50, thermoFisher, USA) with corresponding module. The spectrum is 400-4000 cm -1 Is scanned (n=6), operated by Omnic 9. The number of scans was 32, the resolution was 4cm -1 With air as the background. A total of 54 ATR-FTIR spectra were obtained.
1.2.6 modeling
ATR correction was performed on ATR-FTIR spectra using OMNIC software. The spectrum is also preprocessed by a constant, standard Normalized Variable (SNV) or Multiplicative Scattering Correction (MSC) method (a preprocessing method corresponding to the minimum RMSEP is the best method by taking the RMSEP as a response value), so that noise is removed, and interference factors such as light scattering are eliminated. Samples were randomly divided into a calibration (Cal) group and a prediction (Pre) group at a ratio of 2:1. Principal Component Regression (PCR) predictive models for TPC, U/S and AC were established using TQ-analysis software. The performance of the model was evaluated with the following parameters: calibration set correlation coefficient (Rc) and prediction set correlation coefficient (Rp), root mean square error of calibration set (RMSEC), root mean square error of prediction set (RMSEP), and residual prediction bias (RPD).
2 results and discussion
2.1 detection results of chemical component content of Iris seed oil
FIG. 2 shows the oil content of ILS and TPC of Iris seed oil in 9 populations. As a result, oil production rates of ILS at 9 different points were found to be between 8.49% and 10.68%. TPC was between 29.18 and 104.91 mg/kg Gallic Acid Equivalent (GAE) using solid phase microextraction and n-hexane extraction methods. At present, no research on TPC in different populations of iris seed oil is published. This level is similar to sunflower oil (10-120 mg/kg). There was a considerable difference in TPC from vegetable oils ranging from 18.65 mg/kg to 12630.00 mg/kg.
For iris seed oil in 9 populations, the TPC level of P6 was found to be highest with a Coefficient of Variation (CV) of 0.45%. Average TPC of Iris seed oil is 49.83mg GAE/kg. By comparison, the TPC of iris seed oil was found to be higher than 8 oils in the Liu test (Liu Huimin. Correlation study of the trace components of different vegetable oils with antioxidant capacity. University of south of the river, 2015.) including wheat germ oil, peanut oil, sunflower seed oil, rapeseed oil, corn oil, coconut oil, palm oil and palm kernel oil.
Of these 9 populations, 9 unsaturated fatty acids (U), 9 saturated fatty acids (S), U/S of Iris seed oil are listed in Table 1. The average proportion of saturated fatty acids was 14.17%, with palmitic acid being the main component and the average content being 8.16%. The two highest levels were stearic acid (4.84%) and arachic acid (1.62%). Lauric acid was the lowest, 0.04%, and was not detected in P1 and P9. Unsaturated fatty acid accounts for most of total fatty acid in iris seed oil sample, and the average proportion is 84.92%. Oleic acid and linoleic acid were the highest concentrations of unsaturated fatty acids found in iris seed oil evaluated in this study. The average linoleic acid content was 43.06% and oleic acid content was 36.82%. The average U/S is equal to 6.19, while P1 has a U/S of 8.86 at the highest. The fatty acid composition and relative content of Iris seed oil are very similar to those of sesame oil.
TABLE 1 Iris seed oil fatty acid composition
Note that: RT: average expected retention time; s: saturated fatty acids; u: unsaturated fatty acids; U/S: the ratio of the main unsaturated fatty acid to the saturated fatty acid.
2.2 detection results of antioxidant activity content of Iris seed oil
The antioxidant effect was evaluated using ascorbic acid as a positive control, and the results are given in fig. 3. The antioxidant activity of iris seed oil at the same concentration varies among different populations. At the same time, it is concentration-dependent, increasing from 0.875-28.000 mg/ml in all samples. At the inflection point (14 mg/ml), DPPH clearance was near the maximum. Then, it slowly increases and stabilizes at 83.830-86.342%. IC of P1 to P9 50 Values 5.134, 4.974, 4.968, 5.419, 4.798, 3.532, 4.992, 4.909 and 5.398 mg/ml, respectively. The iris seed oil obtained by the invention has better antioxidant activity than common oils (such as olive oil) which are considered to have high antioxidant activity, which indicates that the iris seed oil can be used as an antioxidant for promoting health in human diets.
2.3ATR-FTIR spectroscopic analysis
The average spectrum of the ATR-FTIR spectra of all samples is shown in FIG. 4, which shows that the main absorption peak of Iris seed oil is 3009cm -1 、2925cm -1 、2854cm -1 、1746cm -1 、1652cm -1 、1465cm -1 、1378cm -1 、1237cm -1 、1163cm -1 、1099cm -1 And 723cm -1 Where it is located. The presence of large amounts of CH in fatty acids 3 And CH (CH) 2 Wherein the stretching vibration of the C-H bond results in a stretching vibration of 2925cm -1 、2854cm -1 、1465cm -1 And 1378cm -1 Two strong absorption peaks are formed nearby, 1746cm -1 The peak represents c=o in the ester group. 1652cm -1 And 723cm -1 The peaks of (C) indicate the presence of c=c in the sample. 1237cm -1 And 1163cm -1 The peaks of (C) represent the tensile and flexural vibrations of C-O and C-H, respectively。1099cm -1 The peak at which is the tensile vibration of C-O.
2.4 modeling
PCR is an effective method for compressing spectrum data and extracting information, and the result can be more reliable and accurate by extracting several main components. The PCR models of the 3 quality control indexes are shown in Table 2.
TABLE 2 PCR model of three quality control indicators
Note RMSEC: the root mean square error of the calibration; rc: calibrating coefficients; RMSEP: a predicted root mean square error; rp: a prediction coefficient; RPD: residual prediction bias; TPC: total polyphenol content; U/S: the ratio of the primary unsaturated fatty acid to the saturated fatty acid; AC: antioxidant capacity; SNV: standard normalized variables.
Correlation analysis shows that IC for eliminating DPPH by iris seed oil 50 Pearson correlation coefficient with TPC was-0.881, indicating that TPC was highly correlated with AC (P<0.01). 1650cm of oxygen radical absorption capacity model -1 The band of (2) contributes to the highest positive correlation. Thus 1567-1800 cm -1 And 1567-1804 cm -1 Are selected as modeling ranges for TPC and AC. TPC and AC models are satisfactory, with sufficiently high Rc, rp #>0.95 And RPD>3.50 A) value.
All C-H, C-O and c=c groups were used to construct the U/S model with modeling interval 3040-2800cm -1 And 1700-640cm -1 . The U/S model also has good model effect, and RMSEC, RMSEP, rc, rp and RPD values are 0.478, 0.423, 0.941, 0.943, and 3.16, respectively.
The RPD value is considered an important parameter in estimating the predictive performance of the model. The higher the RPD value, the better the model performance. When RPD >2.5, this model is shown to have acceptable predictive power. The RPD values of both TPC and U/S models were greater than 2.5, indicating that the established models can be used for the determination. RPD values >5 in the AC model indicate that the model has good predictive effect. Fig. 5 shows the prediction results of the three parameters for each model. There is a good correlation between the actual and predicted values of the Cal and Pre sets. The above results demonstrate the high predictive power of this model, particularly showing the possibility of quality control of Iris seed oil with ATR-FTIR.
The quantitative model of total polyphenol content, main unsaturated fatty acid and saturated fatty acid proportion and antioxidant capacity of iris seed oil is established by using an ATR-FTIR and chemometrics combined method. The results show that the AC model has a higher Rc (0.988) and Rp (0.987), and a lower RMSEC (0.081) and RMSEP (0.088). In addition, the RPD value of the model is higher and is 5.96, and no abnormal value exists, so that the model has good prediction performance. Both TPC and U/S models have higher Rc and Rp values (> 0.940) and RPD values (> 3.00), showing higher prediction accuracy. Therefore, the model provided by the invention can be used for routine analysis of iris seed oil, and has small workload for quality control of iris seed oil. Meanwhile, the ATR-FTIR method is innovatively applied to rapid evaluation of the seed oil AC, and guidance can be provided for quality evaluation of other plant seed oils.
The foregoing detailed description of the invention is provided for illustration, and it is not to be construed that the detailed description of the invention is limited to only those illustration, but that several simple deductions and substitutions can be made by those skilled in the art without departing from the spirit of the invention, and are to be considered as falling within the scope of the invention.
Claims (10)
1. The quality evaluation method of the Iris seed oil based on ATR-FTIR is characterized by comprising the following steps:
measuring the content of quality evaluation components to be measured in iris seed oil;
collecting ATR-FTIR spectra;
preprocessing by constant, standard Normalized Variable (SNV) and Multiplicative Scatter Correction (MSC) methods;
establishing a principal component regression prediction model of TPC, U/S and AC;
evaluating the performance of the model by adopting the correlation coefficient of the calibration set, the correlation coefficient of the prediction set, the root mean square error of the calibration set, the root mean square error of the prediction set and the residual prediction deviation;
and (3) analyzing the correlation between the actual value and the predicted value, wherein the correlation coefficient of the calibration set and the predicted set of the built model is close to 1, and the quality evaluation of the iris seed oil can be carried out by using the model.
2. The quality evaluation method of iris seed oil according to claim 1, wherein the preparation method of iris seed oil comprises the following steps: pulverizing and sieving Iris seed with seed coat removed, and extracting with supercritical carbon dioxide.
3. The method for evaluating quality of iris seed oil according to claim 2, wherein the conditions of supercritical carbon dioxide extraction are as follows: extracting at 40-50 deg.c and 25-34 MPa for 70-95 min.
4. The method for evaluating quality of iris seed oil according to claim 1, wherein the method for evaluating quality of iris seed oil comprises the steps of: detecting the total polyphenol content, detecting the fatty acid component, and detecting the in vitro antioxidant activity.
5. The quality evaluation method of iris seed oil according to claim 4, wherein the method for detecting the total polyphenol content comprises the following steps: and (3) weighing Iris seed oil, dissolving in a solvent, performing column extraction, eluting with an alcohol solution, collecting an eluent, evaporating the solvent, performing ultrasonic dissolution on residues, and using gallic acid working solutions with different concentrations to establish a standard curve so as to calculate the content of total polyphenol.
6. The method for evaluating quality of iris seed oil according to claim 4, wherein the method for determining fatty acid components comprises the following steps: weighing Iris seed oil, adding KOH-CH 3 Reflux of OH solution until oil drops disappear, adding BF 3 -CH 3 Continuously refluxing the OH solution for 1-5 min, cooling to room temperature, addingStanding and layering an organic solvent and a saturated sodium chloride solution, sucking an upper layer solution, adding the upper layer solution into anhydrous sodium sulfate, shaking and standing, sucking the upper layer solution, and measuring by adopting GC-MS;
further, the GC-MS measurement conditions are as follows: adopting a capillary chromatographic column, wherein the temperature of a sample inlet is 275-285 ℃; the carrier gas is helium; the sample injection amount is 0.5-2 mu L; the split ratio (15-30) is 1, the temperature programmed is kept at 40-55 ℃ for 0.5-3 min, the temperature is increased to 170-180 ℃ at 20-30 ℃/min, the temperature is increased to 220-240 ℃ at 2-6 ℃/min, and the temperature is kept for 3-6 min; the ionization mode is electron bombardment ion source, column head pressure is 220-235 KPa, and transmission line temperature is 270-285 ℃.
7. The method for evaluating quality of iris seed oil according to claim 4, wherein the method for detecting in vitro antioxidant activity comprises the following steps: preparing Iris seed oil with different concentrations by using ethanol and petroleum ether, preparing positive control and blank control, adding DPPH-ethanol solution into the Iris seed oil, measuring absorbance after light-shielding reaction, and calculating the DPPH free radical clearance of the Iris seed oil.
8. The quality evaluation method of Iris seed oil according to claim 1, wherein the spectrum is 4000-400 cm when collecting ATR-FTIR spectrum -1 Is scanned 32 times in the region of (2), the scanning time is 28-37 s, the resolution is 4cm -1 With air as the background.
9. The method for evaluating quality of iris seed oil according to claim 1, wherein the samples are randomly divided into a calibration group and a prediction group according to a ratio of 2:1 during the pretreatment.
10. The iris seed oil quality evaluation method according to claim 1, wherein modeling ranges of the TPC and AC models are respectively: 1567-1800 cm -1 、1567～1804cm -1 ；
The modeling interval of the U/S model is 2800-3040 cm -1 And 640-1700 cm -1 。
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| CA2515891A1 (en) * | 2004-05-07 | 2005-11-07 | Nir Technologies Inc. | Ft-nir fatty acid determination method |
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| CN111672155A (en) * | 2020-06-16 | 2020-09-18 | 南通康之源中药材有限公司 | Supercritical fluid extraction method |
| CN114550843A (en) * | 2022-01-21 | 2022-05-27 | 梁军 | Model for predicting monosaccharide composition and content in traditional Chinese medicine polysaccharide and construction method and application thereof |
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| CA2515891A1 (en) * | 2004-05-07 | 2005-11-07 | Nir Technologies Inc. | Ft-nir fatty acid determination method |
| US20170299506A1 (en) * | 2016-04-18 | 2017-10-19 | Hormoz Azizian | Verification Of Olive Oil Composition |
| CN109423358A (en) * | 2017-09-04 | 2019-03-05 | 中国科学院西北高原生物研究所 | A kind of extracting method of Chinese small iris volatile oil |
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