CN110133120B - Construction method and application of gas chromatography-mass spectrometry wild jujube kernel oil characteristic spectrum - Google Patents
Construction method and application of gas chromatography-mass spectrometry wild jujube kernel oil characteristic spectrum Download PDFInfo
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- G—PHYSICS
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Abstract
A gas chromatography-mass spectrometry wild jujube kernel oil characteristic spectrum construction method and application belong to the technical field of detection, can solve the problem that the existing wild jujube kernel oil evaluation method is complex in treatment process, and comprises the following steps: (1) performing Soxhlet extraction on spina date seed medicinal material powder by using petroleum ether to obtain spina date seed oil, and performing derivatization and filtering to obtain a test sample; (2) determining the chemical characteristic spectrum of the wild jujube kernel oil by a gas chromatography-mass spectrometry technology; (3) the characteristic spectrum of the wild jujube kernel oil is determined to contain 9 characteristic peaks through spectrum analysis. The method has the advantages of simple and convenient sample pretreatment and good reproducibility, can accurately reflect some important characteristic information of the wild jujube kernel oil, and can be used for the quality of the wild jujube kernel oil.
Description
Technical Field
The invention belongs to the technical field of detection, and particularly relates to a construction method and application of a gas chromatography-mass spectrometry wild jujube seed oil characteristic spectrum.
Background
The spina date seed is recorded in Shen nong Ben Cao Jing of the last year in east Han, is recorded in the Chinese pharmacopoeia of 1977, is listed as a good medicine for calming heart and soothing nerves since ancient times, and is one of the traditional Chinese medicinal materials which are issued by the Ministry of health care of the national sanitation and are not only food but also traditional Chinese medicinal material substances. Researches show that the main chemical components of the spina date seed comprise secondary metabolites such as saponin, flavone and alkaloid and primary metabolites such as fatty acid, amino acid, nucleic acid and saccharide. The wild jujube kernel oil accounts for more than 30 percent, and most of the wild jujube kernel oil is fatty acid substances. Modern pharmacological research shows that the wild jujube kernel oil has the functions of tranquilizing, hypnotizing and improving learning and memory. Therefore, the wild jujube kernel oil product is active in the medical health care market as a health care product for improving sleep. The semen ziziphi spinosae is a mature seed of Ziziphus mauritiana lam, belonging to the same family as the spina date seeds, the shape of the semen ziziphi spinosae is similar to that of the spina date seeds, and the phenomenon that the semen ziziphi spinosae is used as the semen ziziphi spinosae in the medicinal material market generally exists. But the prices of the two are very different, and the spina date seed is 5 to 6 times of the price of the spina date seed. In order to prevent the bad merchants from consummating violence and damaging the interests of consumers, an effective method for controlling the quality of the wild jujube kernel oil is urgently needed to be established.
At present, Zhang Qinzhuangfei establishes a GC-MS characteristic map of fatty oil of wild jujube seeds which are medicinal materials in the north China. But the pretreatment of the sample is complex, and the wild jujube kernel are distinguished only by adopting the similarity value. The scholars of Wu and Zhen, etc. perform characteristic map research of supercritical carbon dioxide extraction of wild jujube kernel oil and evaluate the consistency of wild jujube seed medicinal materials. The method is complicated, and rapid identification of wild jujube kernel oil cannot be realized.
Disclosure of Invention
The invention provides a construction method and application of a gas chromatography-mass spectrometry wild jujube seed oil characteristic spectrum, aiming at the problem that the existing evaluation method of wild jujube seed oil is complex in treatment process.
The invention adopts the following technical scheme:
a method for constructing a characteristic spectrum of wild jujube kernel oil by gas chromatography-mass spectrometry comprises the following steps:
firstly, extracting wild jujube kernel oil: respectively taking 2g of each batch of samples, placing the samples in Soxhlet extraction, adding 90mL of petroleum ether, heating and refluxing for 4h at the temperature of 60-90 ℃, and recovering the petroleum ether to obtain the wild jujube kernel oil;
secondly, derivatization of the wild jujube kernel oil and preparation of a sample solution for testing: sucking 50 mu L of wild jujube kernel oil of each batch of samples, adding 150 mu L of trimethylchlorosilane derivatization reagent, putting the mixture into a constant-temperature oscillation metal bath for derivatization for 1.5h, and then passing through a 0.22 mu m filter membrane to obtain a sample solution to be tested;
thirdly, determining the characteristic spectrum of the wild jujube kernel oil by gas chromatography-mass spectrometry: the gas chromatography test conditions were: a GC-MS combined instrument, an HP-5MS capillary column with the thickness of 30m multiplied by 0.25mm multiplied by 0.25 mu m, high-purity nitrogen as carrier gas, the flow rate of 1.0mL/min, the split ratio of 20:1, the sample injection amount of 0.5 mu L, the initial temperature of 150 ℃, the initial temperature of 1min, the initial temperature of 215 ℃ at the rate of 5 ℃/min, the initial temperature of 18min, the initial temperature of 240 ℃ at the rate of 5 ℃/min, the initial temperature of 6min, and the initial temperature of 270 ℃ at the rate of 10 ℃/min for 13 min;
mass spectrum conditions: EI ionization is 70eV, the ion source temperature is 200 ℃, the interface temperature is 250 ℃, and the scanning range is 50-500 m/z;
fourthly, qualitative identification of chemical components: according to the gas chromatography-mass spectrometry spectrogram of the wild jujube kernel oil, the compounds are matched by using Masshunter data analysis software in combination with NIST14 standard mass spectrograms and relative retention indexes, and the compounds with the matching degree of more than 90% can be used as identification results.
In the second step, the temperature of the constant-temperature oscillation metal bath is 90 ℃, and the rotating speed is 300 r/min.
A method for constructing a characteristic spectrum of wild jujube kernel oil by gas chromatography-mass spectrometry is used for quality detection of wild jujube kernel oil. The invention has the following beneficial effects:
the invention adopts a gas chromatography-mass spectrometry technology combined with a traditional Chinese medicine chromatogram characteristic spectrum similarity evaluation system to establish a convenient, effective and integral quality control method for the wild jujube kernel oil. The pretreatment of the research adopts a direct derivatization method to process samples, is simple and time-saving, identifies 27 components in total, and can embody the characteristics of saturated fatty acid and unsaturated fatty acid in wild jujube kernel oil and wild jujube kernel oil components. The research has important significance for ensuring the quality of the wild jujube seed oil in the traditional Chinese medicine and health food raw materials and intermediate products of preparations and developing new traditional Chinese medicines of wild jujube seed series.
Compared with the prior art, the method has the following advantages and effects: 1. the sample pretreatment is simple; 2. matching the compounds by using Masshunter data analysis software in combination with NIST14 standard mass spectrograms and relative retention indexes, and identifying 27 components in total; 3. the 9 characteristic peaks of the characteristic spectrum of the wild jujube kernel oil established in the research are structurally identified, and the relative peak area accounts for more than 90% of the total peak area, so that the quality of the wild jujube kernel oil can be more accurately evaluated.
Drawings
FIG. 1 is a chromatogram of total ion current of spine date seed oil;
FIG. 2 is a chromatogram of total ion current of the semen Ziziphi Spinosae oil;
FIG. 3 is a characteristic spectrum and a comparison characteristic spectrum of wild jujube kernel oil;
FIG. 4 is a graph showing the relative content of characteristic components of spine date seed oil;
FIG. 5 is a PCA analysis chart of spine date seed oil and spine date seed oil;
FIG. 6 is a graph of relative content analysis of spine date seed oil and spine date seed oil.
Detailed Description
Example 1
Establishing a wild jujube kernel oil characteristic map, comprising the following steps:
and (3) collecting a sample in the step (1). The method comprises the following specific steps: the spina date seeds used for the experiment are purchased from the Anguo medicinal material market in Hebei and Shanxi province and Dongdao medicinal material Co Ltd. The semen Ziziphi Spinosae is identified as dry mature seed of Ziziphus jujuba Mill.Var.spinose (Bunge) Hu ex H.F.Chou; the semen Ziziphi Spinosae is dry mature seed of Ziziphus mauritiana Lam. of Rhamnaceae. 13 batches of spina date seed samples are collected and stored in the modern research center of traditional Chinese medicine of Shanxi university.
And (2) extracting the wild jujube kernel oil. The method comprises the following specific steps: precisely weighing 2g of each batch of samples, placing the samples in Soxhlet extraction, adding 90mL of petroleum ether (60-90 ℃), heating and refluxing for 4 hours, and recovering the petroleum ether to obtain the wild jujube seed oil and the management jujube seed oil.
And (3) derivatization and preparation of a test solution. The method comprises the following specific steps: sucking 50 μ L of oil of each batch of samples, adding 150 μ L of TMCS (trimethylchlorosilane) derivatization reagent, placing in a constant-temperature oscillation metal bath (model: Mixing Block MB-102) at 90 deg.C and 300r for derivatization for 1.5h, and filtering with 0.22 μm filter membrane to obtain the test solution.
And (4) performing gas chromatography-mass spectrometry analysis. The method comprises the following specific steps:
instruments and reagents: GC-MS (Agilent 5977B gas chromatograph, G4513A autosampler, quadrupole mass analyzer); HP-5MS capillary column (30 m.times.0.25 mm. times.0.25 μm), TMCS (trimethylchlorosilane) derivatization reagent 150 μ L, constant temperature shaking metal bath (model: Mixing Block MB-102).
Gas chromatography conditions: HP-5MS capillary column (30m × 0.25mm × 0.25 μm), high purity nitrogen as carrier gas, flow rate of 1.0mL/min, split ratio of 20:1, sample injection amount of 0.5 μ L, inlet temperature of transmission line temperature, temperature programming: the starting temperature was 150 ℃ for 1min, then ramped up to 215 ℃ at 5 ℃/min for 18min, then ramped up to 240 ℃ at 5 ℃/min for 6min, then ramped up to 270 ℃ at 10 ℃/min for 13 min.
Mass spectrum conditions: EI ionization is 70eV, ion source temperature is 200 ℃, interface temperature is 250 ℃, and scanning range m/z is 50-500.
And (5) qualitatively identifying chemical components. The method comprises the following specific steps: according to the method of the step (2-4), obtaining a gas chromatography-mass spectrometry spectrum of the wild jujube kernel oil (see figure 1). Compounds were matched using Masshunter data analysis software in combination with NIST14 standard mass spectra and relative retention indices, and compounds with a degree of match greater than 95% were used as identification results. And (3) searching and checking a NIST14 LIBRARY standard mass spectrum atlas by a mass spectrum computer data system for each peak in the total ion flow graph, wherein the compound with the matching degree of more than 95 percent can be used as an identification result. A total of 27 components were identified, see table 1.
TABLE 1 chemical composition identified in spine date seed and spine date seed oil
And (6) verifying a characteristic spectrum methodology. The method comprises the following specific steps:
a. precision test
Weighing 2g of S1 sample, preparing a sample solution according to the sample pretreatment method in the step (2) and the step (3), continuously feeding samples for 6 times according to the chromatographic mass spectrometry condition in the step (4), and collecting a map. The similarity evaluation software of the chromatographic characteristic spectrum of the traditional Chinese medicine is adopted for processing, the similarity is more than 0.99, and the precision of the instrument is good.
b. Repeatability test
Weighing 2g and 6 parts of S1 sample, preparing a sample solution according to the sample pretreatment method in the step (2) and the step (3), injecting sample according to the chromatographic mass spectrometry condition in the step (4), and collecting a map. The similarity evaluation software of the chromatographic characteristic spectrum of the traditional Chinese medicine is adopted for processing, the similarity is more than 0.99, and the repeatability of the preparation method is good.
The establishment of the characteristic map and the calibration of the characteristic peak in the step (7) are as follows:
a. and (3) calibrating the characteristic peaks, selecting 9 common chromatographic peaks with larger peak areas (accounting for more than 90% of the total peak area) as characteristic peaks of the characteristic spectrum according to the identification result of the chemical components in the step (5), wherein the characteristic peaks are sequentially arranged according to the peak emergence order, namely palmitic acid C16:1, linoleic acid C18:3, oleic acid C18:2, stearic acid C18:1, arachidonic acid C20:1, campesterol C28:5, behenic acid C22:1, squalene C30:6, beta-sitosterol C29:5 and gamma-tocopherol C28: 5.
b. The reference substance of the selected characteristic spectrum of the reference substance (S) is usually selected from index components which are easy to obtain, stable in property and high in content, and is mainly used for determining technical parameters of the characteristic spectrum. Oleic acid has the highest response value and the largest peak area in the wild jujube kernel oil chromatogram, accounts for 24 percent of the total peak area, and is monounsaturated fatty acid. The response value of the palmitic acid in the wild jujube kernel oil chromatogram is second, the peak area accounts for 15% of the total peak area, the palmitic acid is saturated fatty acid, the palmitic acid is stable in property, is better separated from adjacent fatty acid peaks, is not crossed, meets the requirements of characteristic spectrum stability and repeatability investigation, and is comprehensively analyzed.
c. And (3) establishing a characteristic spectrum, exporting 13 batches of wild jujube kernel oil gas chromatography-mass spectrum data obtained in the step (5) into TXT files, and respectively introducing the TXT files into software of version 2.0 of a Chinese medicine chromatography characteristic spectrum similarity evaluation system for processing to obtain 13 batches of wild jujube kernel oil characteristic spectra and comparison characteristic spectra thereof. As shown in fig. 2, S1 is a control feature map, which is generated by multi-point correction and full spectrum peak matching. Statistics of the relative retention times of the 9 characteristic peaks in 13 batches of spina date seeds with respect to the reference peak (R) are shown in Table 2.
TABLE 213 statistics of the relative retention times of 9 characteristic peaks in wild jujube seed batches
Example 2
The method is used for evaluating the uniformity of the wild jujube kernel oil and measuring the relative content.
The characteristic spectrum can represent the correlation between the complex components of the substances and the quality of the complex components, wherein the similarity evaluation plays an important role, the wild jujube kernel oil similarity evaluation method adopted by the invention is software of 2.0 version of a Chinese medicinal chromatographic characteristic spectrum similarity evaluation system recommended by the State pharmacopoeia Committee, the similarity of the characteristic spectrums of 13 batches of wild jujube kernel oil is calculated by taking a contrast characteristic spectrum as a standard, and the calculation result is shown in a table 3. As can be seen from the table, the similarity of the 13 batches of wild jujube kernel oil samples is 0.996-1, and the wild jujube kernel oil samples have high similarity, which indicates that the uniformity of the wild jujube kernel oil samples of different batches is better. The relative contents of the 9 characteristic components are calculated by using a peak area normalization method, and the three components with higher contents are sequentially oleic acid, linoleic acid and palmitic acid, and account for more than 70% of the total content of the wild jujube kernel oil, as shown in a figure (4).
Example 3
Distinguishing wild jujube kernel oil from natural jujube kernel oil
The samples were collected as follows: the experimental jujube kernel is purchased from the Annational medicinal material market in Hebei province, and is identified as dry mature seeds of Ziziphus mauritiana Lam. The 7-reason jujube kernel samples are collected and stored in the modern research center of traditional Chinese medicine of Shanxi university.
And (3) constructing a 7-batch jujube kernel oil characteristic map (shown in figure 2) according to the steps (2-6) in the example 1. 13 batches of wild jujube kernel oil and 7 batches of processed jujube kernel oil are taken as research objects, the areas of the spectral peaks in the characteristic spectrum of each sample form an original data matrix, and the main component analysis is carried out by SIMCA-P13.0, and the result is shown in figure 5. The cumulative variance contribution of the first two principal components PC1 (52%) and PC2 (25%) was 77%. As can be seen from FIG. 5, all the samples of spine date seeds are gathered together, and all the samples of spine date seed are gathered together, which shows that the spine date seed oil and the spine date seed oil can be accurately distinguished by the principal component analysis.
Example 4
Can be used for comparing the relative contents of different types of fatty acids in wild jujube kernel oil and natural jujube kernel oil
Based on the wild jujube kernel oil and wild jujube kernel oil feature maps constructed in examples 1 and 3, the peak area normalization method is used to calculate the relative content of 9 feature components in each sample. Wherein palmitic acid, stearic acid and behenic acid are saturated fatty acids, oleic acid and arachidonic acid are monounsaturated fatty acids, and linoleic acid, squalene, sitosterol and tocopherol are polyunsaturated fatty acids, and as can be seen from fig. 6, the jujube kernel has higher content of saturated fatty acids and monounsaturated fatty acids, most of the polyunsaturated fatty acids are higher in the wild jujube kernel, and the sitosterol is higher in the wild jujube kernel.
TABLE 3 characteristic components of characteristic map of wild jujube kernel oil
Table 413 batch jujuba seed oil sample similarity calculation results
Claims (2)
1. A method for constructing a characteristic spectrum of wild jujube kernel oil by gas chromatography-mass spectrometry is characterized by comprising the following steps: the method comprises the following steps:
firstly, extracting wild jujube kernel oil: respectively taking 2g of each batch of samples, placing the samples in Soxhlet extraction, adding 90mL of petroleum ether, heating and refluxing for 4h at the temperature of 60-90 ℃, and recovering the petroleum ether to obtain the wild jujube kernel oil;
secondly, derivatization of the wild jujube kernel oil and preparation of a sample solution for testing: sucking 50 mu L of wild jujube kernel oil of each batch of samples, adding 150 mu L of trimethylchlorosilane derivatization reagent, putting the mixture into a constant-temperature oscillation metal bath for derivatization for 1.5h, and then passing through a 0.22 mu m filter membrane to obtain a sample solution to be tested; the temperature of the constant-temperature oscillating metal bath is 90 ℃, and the rotating speed is 300 r/min;
thirdly, determining the characteristic spectrum of the wild jujube kernel oil by gas chromatography-mass spectrometry: the gas chromatography test conditions were: a GC-MS combined instrument, an HP-5MS capillary column with the thickness of 30m multiplied by 0.25mm multiplied by 0.25 mu m, high-purity nitrogen as carrier gas, the flow rate of 1.0mL/min, the split ratio of 20:1, the sample injection amount of 0.5 mu L, the initial temperature of 150 ℃, the initial temperature of 1min, the initial temperature of 215 ℃ at the rate of 5 ℃/min, the initial temperature of 18min, the initial temperature of 240 ℃ at the rate of 5 ℃/min, the initial temperature of 6min, and the initial temperature of 270 ℃ at the rate of 10 ℃/min for 13 min;
mass spectrum conditions: EI ionization is 70eV, the ion source temperature is 200 ℃, the interface temperature is 250 ℃, and the scanning range is 50-500 m/z;
fourthly, qualitative identification of chemical components: according to a gas chromatography-mass spectrometry spectrogram of the wild jujube kernel oil, matching the compounds by using Masshunter data analysis software in combination with a NIST14 standard mass spectrogram and a relative retention index, wherein the compounds with the matching degree of more than 90% can be used as an identification result;
fifthly, establishing a characteristic spectrum and calibrating a characteristic peak:
(1) calibration of characteristic peaks: selecting 9 common chromatographic peaks with peak areas accounting for more than 90% of the total peak area as characteristic spectrum characteristic peaks, wherein the characteristic peaks are sequentially arranged into palmitic acid, linoleic acid, oleic acid, stearic acid, arachidonic acid, docosanoic acid, squalene, beta-sitosterol and gamma-tocopherol according to the peak appearance sequence;
(2) selection of reference (S): selecting palmitic acid as a reference substance (S);
(3) establishing a characteristic spectrum: exporting the obtained gas chromatography-mass spectrometry spectrogram data of the wild jujube kernel oil into a TXT file, respectively introducing the TXT file into a software version 2.0 of a Chinese medicine chromatogram characteristic spectrogram similarity evaluation system to be processed to obtain a wild jujube kernel oil characteristic spectrogram, taking the spectrogram of a sample S1 as a reference spectrogram, and generating a wild jujube kernel oil comparison characteristic spectrogram R through multipoint correction and full spectrum peak matching;
(4) analyzing a characteristic spectrum: and calculating the similarity of the characteristic maps of the wild jujube kernel oil by taking the contrast characteristic map as a standard, wherein the similarity is 0.996-1, and the similarity is very high, which indicates that the uniformity of the wild jujube kernel oil of different batches is better.
2. A method for constructing a characteristic spectrum of the wild jujube kernel oil by gas chromatography-mass spectrometry according to claim 1, which is used for the quality detection of the wild jujube kernel oil.
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