CN109633060B - Construction method of fried perilla seed characteristic spectrum and application of fried perilla seed characteristic spectrum in frying process - Google Patents
Construction method of fried perilla seed characteristic spectrum and application of fried perilla seed characteristic spectrum in frying process Download PDFInfo
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Abstract
The invention discloses a construction method of a fried perilla seed characteristic spectrum and application thereof in a frying process. Based on the principal component analysis, the stir-frying process of the perilla seeds is optimized by combining the establishment method of the feature map of the stir-fried perilla seeds, and a basis is provided for the standardization of the stir-frying process.
Description
Technical Field
The invention belongs to the field of traditional Chinese medicines, and particularly relates to a construction method of a fried perilla seed characteristic spectrum and application thereof in a frying process.
Background
The perilla seeds are dry mature fruits of Perilla Perillastescens (L.) Britt. of Labiatae, the fruits are harvested in autumn, impurities are removed, and the fruits are dried in the sun, the perilla resources are widely distributed in China, such as Guangdong, Guangxi, Hubei, Yunnan, Guizhou, Sichuan, Taiwan, Zhejiang, Anhui, Fujian provinces, the perilla plants like warm climate and short sunshine, the adaptability is strong, and the perilla plants are planted in 21 provinces of northeast, northwest, southeast and southwest of China at present. It is warm in nature and pungent in taste, has the functions of depressing qi and resolving phlegm, relieving cough and asthma, and loosening the bowel to relieve constipation, and is mainly used for treating phlegm stagnation and adverse flow of qi, cough and asthma, intestinal dryness and constipation and the like clinically.
At present, the processing technology of perilla fruit is stir-frying, for example, under the item of perilla fruit decoction pieces of China pharmacopoeia 2015 edition, the stir-frying is carried out until the perilla fruit is completely fried until the perilla fruit is exploded by a stir-frying method, and the stir-frying of perilla fruit is carried out according to the traditional Chinese medicine decoction piece processing standard of Tianjin, namely, a pot is heated, the perilla fruit is placed in the pot, the surface pigment is fried to deepen color, and when the aroma escapes, the perilla fruit is taken out and cooled. The processing standard of the traditional Chinese medicine decoction pieces in Hunan province is that the clean perilla seeds are taken and fried by slow fire until the sound of explosion occurs, and then taken out and cooled. The processing standard of the Chinese medicinal decoction pieces in Shanghai city is that raw perilla seeds are taken and fried to have burst sound by a clear frying method. The empirical terms are difficult to control quantitatively, and the stir-frying process is not specified.
The invention optimizes the stir-frying process of the perilla seeds by establishing a determination method of the feature spectrum of the stir-fried perilla seeds, based on the main component analysis and combined with the feature spectrum method to research the stir-frying process of the perilla seeds, and provides a basis for the standardization of the stir-frying process.
Disclosure of Invention
The invention aims to provide a construction method of a fried perilla seed characteristic spectrum, which has good reproducibility, accuracy and reliability.
The invention is realized by the following technical scheme:
a construction method of a fried perilla seed characteristic spectrum comprises the following steps:
(a) preparation of mixed control solution: taking appropriate amount of caffeic acid, rosmarinic acid, and luteolin as reference substances, and adding methanol to obtain mixed reference substance solution containing caffeic acid 2 μ g, rosmarinic acid 40 μ g, and luteolin 5 μ g per mL;
(b) preparation of a test solution: respectively taking about 0.5g of fried perilla fruit drinking tablets, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of 80% methanol, weighing, ultrasonically treating for 15-45 minutes, cooling, complementing weight loss reduction amount with 80% methanol, shaking uniformly, filtering, and taking a subsequent filtrate to obtain the final product;
(c) chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile is taken as a mobile phase A, 0.1 percent formic acid solution is taken as a mobile phase B, and gradient elution is carried out according to the specification in the following table; sample introduction amount: 2 mu l of the solution; the column temperature is 30 ℃; the detection wavelength is 330 nm;
(d) establishing a fried perilla seed contrast characteristic spectrum: precisely absorbing 2 mul of the mixed reference solution and the test solution respectively, injecting into a high performance liquid chromatograph, measuring, establishing a fried perilla seed comparison characteristic spectrum by adopting a traditional Chinese medicine chromatogram fingerprint similarity evaluation system, determining that the fried perilla seed comparison characteristic spectrum has 9 characteristic peaks, namely a peak 1, a peak 2, a peak 3, a peak 4, a peak X1, a peak X2, a peak 5, a peak 6 and a peak 7, taking the peak 6 as a reference peak, and respectively setting the relative retention time of each characteristic peak as follows: 0.32, 0.43, 0.73, 0.88, 0.95, 0.96, 0.97, 1.0, 1.17, the relative retention time of which should be within ± 10% of the stated value.
The characteristic peak attribution is as follows: peak 2 is caffeic acid, Peak 6 is rosmarinic acid, Peak 7 is luteolin.
Further preferably, the preparation of the test solution: sieving parched fructus Perillae decoction pieces with a second sieve, collecting about 0.5g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml 80% methanol, weighing, ultrasonic treating for 30 min with ultrasonic power of 250W and ultrasonic frequency of 40KHz, cooling, supplementing with 80% methanol to reduce weight loss, shaking, filtering, and collecting the filtrate.
The invention also provides an application of the construction method of the fried perilla seed characteristic spectrum in the frying process, the area of the characteristic peak is subjected to principal component analysis according to the constructed fried perilla seed characteristic spectrum method, an index with a characteristic value of more than 1 is selected as a principal component, two principal components are extracted, and the index characteristic peaks for inspecting the frying process are selected as follows according to the influence on the principal components and the component difference before and after frying: the stir-frying process of the perilla seeds is determined by taking the content of the rosmarinic acid and a standardized value based on 4 index characteristic peak area/sample weighing amount as indexes, namely the peak X1, the peak X2, the rosmarinic acid and the luteolin.
Preferably, the content of rosmarinic acid in the stir-fried perilla seeds is not less than 0.20%. The content of the rosmarinic acid is determined according to the purple perilla item of Chinese pharmacopoeia 2015 edition. Agilent SB C18(4.6 mm. times.150 mm, 5 μm) was used as a column; methanol-0.1% formic acid solution (40: 60) is used as a mobile phase; the detection wavelength was 330 nm. The number of theoretical plates should not be less than 3000 calculated according to the peak of rosmarinic acid.
Preferably, the stir-frying process of the perilla seeds comprises the following steps: controlling the pot temperature at 190 ℃, the electric ceramic furnace power at 1000W, the processing time at 4 minutes and the stir-frying frequency at 60 times/minute.
Further preferably, the temperature of the material is controlled to be 155-160 ℃.
Compared with the prior art, the invention has the following beneficial effects:
the method establishes the characteristic spectrum of the fried perilla seeds aiming at the problems in the frying process of the perilla seeds, has good reproducibility, is accurate and reliable, optimizes the frying process of the perilla seeds by combining the determination method for establishing the characteristic spectrum of the fried perilla seeds based on the analysis of main components, and provides a basis for the standardization of the frying process.
Drawings
FIG. 1 is an overlay of feature spectra of 9 batches of parched fructus Perillae.
Detailed Description
The present invention is further illustrated by the following specific embodiments, which are not intended to limit the scope of the invention.
Example 1: method for constructing fried perilla seed characteristic spectrum
1. Instrument and reagent
Electric ceramic oven (Jiangsu Jiuyang, H22-X3), frying pan, Waters high performance liquid chromatograph (Waters, Waters e2695), Waters ultra performance liquid chromatograph (Watts, H-Class), Agilent SB C18 column (4.6mm × 150mm, 5 μm), Waters BEH C18 column (2.1mm × 100mm, 1.7 μm), Agilent SB C18 column (2.1mm × 100mm, 1.8 μm), YMC trap column (2.1mm × 100mm, 1.9 μm), ten-thousandth balance (Mettler-Torilogo, ME204E), millionth (Mettler-Torilogo, XP26), electric heating water boiler (Shanghai constant temperature water bath Co., HWS-28), digital control ultrasonic cleaner (Milne ultrasonic cleaner), Quik super pure water technology Q-Tech, Inc.
Caffeic acid (batch No. 110885-; rosmarinic acid (batch No. 110871) and 201706, purity: 90.5%, China institute for food and drug testing);
luteolin (batch No. 111520-201605, purity: 99.6%, China institute for food and drug testing).
2. Chromatographic conditions and preparation of test solutions
2.1 chromatographic conditions: a chromatographic column: agilent SB C18(2.1 mm. times.100 mm, 1.8 μm); sample introduction amount: 2 mu l of the solution; column temperature: 30 ℃; detection wavelength: 330 nm; acetonitrile was used as mobile phase a and 0.1% formic acid solution was used as mobile phase B, and gradient elution was performed as specified in table 1, flow rates: 0.3 ml/min.
TABLE 1 gradient elution Table
2.2 preparation of test solution: taking about 0.5g of fried perilla seed decoction pieces (screened by a second sieve), precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of 80% methanol, weighing, carrying out ultrasonic treatment (power of 250W and frequency of 40kHz) for 30 minutes, cooling, supplementing with 80% methanol to reduce weight loss, shaking up, filtering, and taking a subsequent filtrate to obtain the purple perilla seed decoction pieces.
3. Examination of preparation method of test solution
3.1 investigation of extraction solvent about 0.5g of stir-fried perilla seed decoction pieces (screened by a No. two sieve) are taken, precisely weighed, placed in a conical flask with a plug, precisely added with methanol, ethanol, 80% methanol, 50% methanol and diluted ethanol respectively as extraction solvents, weighed, ultrasonically treated for 30 minutes, cooled, supplemented with methanol, ethanol, 80% methanol, 50% methanol and diluted ethanol respectively, shaken uniformly, filtered, and a subsequent filtrate is taken, thus obtaining the purple perilla seed decoction pieces.
The experimental results are as follows: wherein 50% methanol and diluted ethanol have low extraction efficiency on luteolin, methanol and ethanol have low extraction efficiency on the first 6 th peak, and the whole extraction efficiency is higher by 80% methanol, so 80% methanol is selected as the extraction solvent.
3.2 the extraction time is considered to take 0.5g of fried perilla seed decoction pieces (screened by a No. two sieve), precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of 80% methanol, weighing, respectively carrying out ultrasonic treatment for 15 minutes, 30 minutes and 45 minutes, cooling, supplementing the weight loss by 80% methanol, shaking up, filtering, and taking the subsequent filtrate to obtain the traditional Chinese medicine composition.
The experimental results are as follows: by comparing the characteristic maps of different ultrasonic times, the extraction efficiency of chromatographic peaks in 15 minutes, 30 minutes and 45 minutes is found to be equivalent, and the ultrasonic time is selected to be 30 minutes in order to ensure the sufficient extraction.
3.3 the extraction method considers that 0.5g of stir-fried perilla seed decoction pieces (screened by a No. two sieve) are taken, precisely weighed, placed in a conical flask with a plug, precisely added with 25ml of 80 percent methanol, weighed, respectively ultrasonically treated for 30 minutes or heated and refluxed for 30 minutes, cooled, supplemented with 80 percent methanol to reduce the weight, shaken evenly and filtered, and the subsequent filtrate is taken, thus obtaining the perilla seed decoction pieces.
The experimental results are as follows: by comparing the characteristic maps of the ultrasonic extraction mode and the heating reflux extraction mode, the influence of the extraction mode on the characteristic maps can be found to be small, the extraction efficiency of the ultrasonic extraction mode and the heating reflux extraction mode is equivalent, and the ultrasonic extraction mode is selected as the extraction mode because the ultrasonic extraction mode is more convenient.
4. Determination of chromatographic conditions
4.1 the determination of the optimal absorption wavelength is carried out by comparing the integral body and the characteristic of 3 detection wavelength chromatograms at 254nm, 330nm and 360nm, the number and the response of chromatographic peaks are poorer at 254nm and 360nm than at 330nm, and finally the phenolic acid component and the flavonoid component are better absorbed when the detection wavelength is 330nm, so 330nm is selected as the detection wavelength.
4.2 investigation of Mobile phase four mobile phases acetonitrile-water, acetonitrile-0.1% formic acid, acetonitrile-0.2% formic acid, methanol-0.1% formic acid were selected for comparison in this experiment. The chromatographic peak separation degree of acetonitrile-water and methanol-0.1% formic acid system is poorer than that of acetonitrile-0.1% formic acid system, and the chromatographic peak separation degree of acetonitrile-0.1% formic acid and acetonitrile-0.2% formic acid are similar, and when acetonitrile-0.1% formic acid mobile phase is selected, the chromatographic peak separation degree is better, so that acetonitrile-0.1% formic acid solution is selected as the mobile phase.
5. Methodology investigation
5.1 specialization examination
Taking a proper amount of fried perilla seeds (screened by a No. two sieve), about 0.5g, precisely weighing, preparing a test solution, respectively taking a blank solvent, a reference solution and the test solution, and respectively injecting 2 mul of sample, wherein the result shows that the analysis method can correctly detect the identified characteristic peak without being interfered by an extraction solvent.
5.2 instrumental precision investigation
Sampling the fried perilla seed sample solution repeatedly for 6 times according to the chromatographic conditions, wherein the sampling volume is 2 mu l, the relative retention time and the relative peak area of other characteristic peaks are calculated by taking a rosmarinic acid peak as a reference peak, and the RSD of the relative retention time and the relative peak area of each chromatographic peak is less than 2 percent.
5.3 stability Studies
Taking a sample solution, respectively injecting samples at 0 hour, 2 hours, 4 hours, 8 hours and 12 hours according to the chromatographic conditions, wherein the sample injection volume is 2 mu l, and calculating the relative retention time and the relative peak area of other characteristic peaks by taking a rosmarinic acid peak as a reference peak, so that the relative retention time of each chromatographic peak within 12 hours is less than 1 percent, the RSD of the relative peak area is less than 5 percent, and the sample solution is basically stable within 12 hours.
5.4 repeatability test
About 0.5g of the same batch of samples are precisely weighed and are parallelly added with 6 parts to prepare a sample solution, and 2 mul of the sample solution is injected respectively. And (3) calculating the relative retention time and relative peak area of other characteristic peaks by taking the rosmarinic acid peak as a reference peak, wherein the relative retention time of each chromatographic peak is less than 1 percent and the RSD of the relative peak area is less than 5 percent, so that the method has good repeatability.
6. Durability test
6.1 investigation of different columns
A sample solution was taken and 2. mu.l of each of YMC Triart C18(2.1 mm. times.100 mm, 1.9 μm), Waters HSS T3(2.1 mm. times.100 mm, 1.8 μm) and Agilent SB C18(2.1 mm. times.100 mm, 1.8 μm) was injected into the column. The comparison of chromatographic peak performance parameters shows that chromatographic columns with different particle sizes are adopted, the chromatographic separation degree of each chromatographic peak can meet the analysis requirement, and the theoretical plate number is higher than Agilent SB C18, so the method can adopt the three ultra-performance liquid chromatographic columns.
6.2 investigation of different column temperatures
Taking the same sample solution, adopting the same chromatographic column and liquid chromatograph, setting the column temperature at 28 deg.C, 30 deg.C, 32 deg.C, and injecting 2 μ l sample respectively. And calculating the relative retention time and the relative peak area of other characteristic peaks by taking the rosmarinic acid peak as a reference peak. The result shows that the relative retention time of each chromatographic peak is less than 3 percent and the relative peak area RSD is less than 5 percent when the column temperature is different, and the result shows that the durability of the analysis method is good when the column temperature is different.
6.3 investigation of different flow rates
The sample solution is taken, the flow rates are respectively set to be 0.28ml/min, 0.30ml/min and 0.32ml/min, and 2 mul of sample is injected respectively. And calculating relative retention time and relative peak area by taking the rosmarinic acid peak as a reference peak. The result shows that the relative retention time RSD of each chromatographic peak at different flow rates is in the range of 0.16-3.80%, and the result shows that the analysis method has better durability at different flow rates. Small variations in flow rate can substantially meet system suitability requirements.
7. Establishment of fried perilla seed characteristic spectrum
The results of the relative retention time and the relative peak area obtained by measuring 9 batches of stir-fried perilla seed decoction pieces according to the method are shown in tables 2 and 3. After the peak 4, characteristic peaks X1 and X2 are obviously generated, a comparison spectrum is generated by adopting a traditional Chinese medicine chromatogram fingerprint similarity evaluation system, and a stir-fried perilla seed comparison characteristic spectrum is established, wherein as shown in figure 1, 9 characteristic peaks are determined, wherein the peak 1, the peak 2, the peak 3, the peak 4, the peak X1, the peak X2, the peak 5, the peak 6 and the peak 7 are determined, the peak 6 is taken as a reference peak, and the relative retention time of each characteristic peak is respectively as follows: 0.32, 0.43, 0.73, 0.88, 0.95, 0.96, 0.97, 1.0, 1.17, the relative retention time of which should be within ± 10% of the stated value. Wherein peak 2 is caffeic acid, peak 6 is rosmarinic acid, and peak 7 is luteolin.
TABLE 29 batch Perilla seed feature Spectroscopy results (relative Retention time)
TABLE 39 results of characteristic spectra (relative peak area) of stir-fried perilla seeds in batches
The result shows that the relative retention time RSD values of different test number samples are 0.02-0.74%, the deviation is small, the relative peak area RSD values are 4.68-128.07%, the fluctuation is large, the difference of sample characteristic maps among different processing technologies is large, and further conclusion is drawn that different processing technologies have certain influence on the chemical components of the perilla seeds.
Example 2: application of construction method of fried perilla seed characteristic spectrum in frying process
The areas of 9 characteristic peaks/the amounts of samples of 9 batches of stir-fried perilla seed decoction pieces were measured, and the results are shown in table 4.
TABLE 49 parched fructus Perillae characteristic chromatogram peak area/sample weighing
And (3) carrying out principal component analysis on the peak area of the characteristic peak of the fried perilla fruit by using SPSS20.0 software, selecting an index with a characteristic value greater than 1 as a principal component, and extracting two principal components as a result, wherein the cumulative contribution rate reaches 94.56%. The results are shown in Table 5. Wherein f8, i.e. rosmarinic acid, had a greater effect on principal component 1, and f9 luteolin had a greater effect on principal component 2, the results are shown in Table 6. Since the difference between the peak X1 and the peak X2 is large before and after processing, the processing technique of perilla seed is examined by using the peak X1, the peak X2, rosmarinic acid and luteolin as indexes. The index values of the processing technique finally obtained are shown in Table 7.
Total variance as explained in Table 5
The extraction method comprises the following steps: and (4) analyzing the main components.
TABLE 6 rotating component matrix a
The extraction method comprises the main components.
Rotation method-orthogonal rotation method with Kaiser normalization.
a. The rotation converged after 3 iterations.
Table 79 batches of different stir-fried perilla seed samples for each index value
The contents of 9 samples and the relative peak area data of each characteristic peak are normalized according to the formula Xij '═ Xij/Xijmax, wherein Xij' is the normalized value of the ith component j in the sample, Xij is the value of the ith component j in the sample, and Xijmax is the maximum value of the ith component j in the sample. According to literature research, the content of total flavonoids is increased compared with that of raw materials after stir-frying of perilla seeds, rosmarinic acid is easy to decompose due to heat, different weighting coefficients are given according to the primary and secondary positions in the processing technology selection, the values are weighted according to the normalized value Xij' and summed, and the comprehensive evaluation index Y is shown in Table 8, wherein the index Y is peak X1% + peak X2% + rosmarinic acid 35% + luteolin 40%.
TABLE 89 Standard index processing results for different batches of stir-fried Perilla frutescens fruit samples
And further substituting the Y value into an orthogonal test table, taking the electric ceramic furnace power W (A), the frying time min (B) and the frying frequency/min (C) as investigation factors, taking 3 levels of each factor, carrying out orthogonal design, and obtaining an analysis result of variance shown in a table 9 and a variance shown in a table 10.
TABLE 9 orthogonal test results Table
TABLE 10 ANOVA TABLE
F0.05(2,2)＝19.00F0.01(2,2)＝99.00
The visual analysis result shows that the influence of the three factors on the result is in the order of magnitude: the power of the electric ceramic furnace is greater than the turning frequency and the processing time is greater than the processing time. The result of the analysis of variance shows that the horizontal change of the influencing factor A has obvious influence on the experimental result of the processing technology, and the optimal processing technology A3B1C2 is comprehensively obtained, namely the pot temperature is controlled to be 190 ℃, the power of an electric ceramic furnace is controlled to be 1000W, the processing time is 4 minutes, and the stir-frying frequency is 60 times/minute.
Weighing three batches of perilla seeds in parallel, frying according to the frying process to obtain three batches of sample process verification, performing content measurement according to the perilla seed item of Chinese pharmacopoeia 2015 edition, and taking Agilent SB C18(4.6mm multiplied by 150mm, 5 mu m) as a chromatographic column; methanol-0.1% formic acid solution (40: 60) is used as a mobile phase; the detection wavelength was 330 nm. The number of theoretical plates should not be less than 3000 calculated according to the peak of rosmarinic acid. The results are shown in Table 11, and the relative retention times and relative peak areas of the profiles are shown in tables 12 and 13.
TABLE 11 determination of the assay results of the Stir-frying Process
TABLE 12 verification of the signature results of the Stirling Process (relative Retention time)
TABLE 13 verification of the signature results (relative peak area) of the Stirling Process
The result shows that the three-batch sample process verification shows that the determination mean value of the content of the rosmarinic acid is 0.325%, and the RSD value is 1.11%, which shows that the content of the three-batch samples has no obvious difference, the RSD value of the relative retention time of the three-batch samples is 0.00% -1.30%, which shows that the deviation of the relative retention time of each characteristic peak is small, but the RSD value of the relative peak area has large fluctuation and is possibly related to the small peak area. In a whole view, the reproducibility of the processing technology of the three batches of samples is better.
In addition, as can be seen from the results of the relative peak areas of test nos. 1 to 9 in tables 2 and 3, the relative peak areas of peak 1, peak 2 (caffeic acid), and peak 3 all showed a significantly decreasing trend, the relative peak areas of peak 4 and peak 5 changed smoothly, the relative peak areas of peaks X1 and X2 showed a significantly increasing gradient trend, and it is presumed that the peak area changes of both were related to temperature and there was a temperature inflection point. In view of the pot-out temperatures of the materials of test Nos. 1-9, the pot-out temperature of test No. 1 is 110 ℃, the pot-out temperatures of test Nos. 2-3 are 125-130 ℃, the pot-out temperatures of test Nos. 4-5 are 140-145 ℃, the pot-out temperature of test No. 6 is 157.2 ℃, the pot-out temperature of test No. 7 is 170 ℃, the pot-out temperature of test No. 6 is 185 ℃, the pot-out temperature of test No. 6 is 200 ℃, and the inflection point of the temperature is estimated to be possibly 155-160 ℃. Therefore, based on the analysis of main components, the study on the perilla seed frying process by combining a characteristic spectrum method discovers that the perilla seed frying process is reasonable when the temperature of the material is 155-160 ℃, and the characteristic spectrum of the perilla seed and the fried perilla seed can reflect the component difference of the perilla seed and the fried perilla seed, thereby explaining the rationality and the standardized explanation of 'frying when the perilla seed is needed'.
Claims (5)
1. The application of the construction method of the fried perilla seed characteristic spectrum in the frying process is characterized in that according to the constructed fried perilla seed characteristic spectrum method, the area of a characteristic peak is subjected to main component analysis, an index with a characteristic value greater than 1 is selected as a main component, two main components are extracted, and according to the influence on the main components and the component difference before and after frying, the characteristic peaks of the index for inspecting the frying process are selected as follows: the stir-frying process of the perilla seeds is determined by taking the content of the rosmarinic acid and a standardized value based on 4 index characteristic peak area/sample weighing amount as indexes, namely a peak X1, a peak X2, the rosmarinic acid and the luteolin;
the construction method of the fried perilla seed characteristic spectrum comprises the following steps:
(a) preparation of mixed control solution: taking appropriate amount of caffeic acid, rosmarinic acid, and luteolin as reference substances, and adding methanol to obtain mixed reference substance solution containing caffeic acid 2 μ g, rosmarinic acid 40 μ g, and luteolin 5 μ g per mL;
(b) preparation of a test solution: taking 0.5g of fried perilla seed decoction pieces, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of 60-80% methanol, weighing, heating and refluxing or ultrasonically treating for 15-45 minutes, cooling, supplementing with 60-80% methanol to reduce weight loss, shaking up, filtering, and taking a subsequent filtrate to obtain the final product;
(c) chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile is taken as a mobile phase A, 0.1 percent formic acid solution is taken as a mobile phase B, and gradient elution is carried out according to the specification in the following table; sample introduction amount: 2 mu l of the solution; the column temperature is 30 ℃; the detection wavelength is 330 nm; a chromatographic column: agilent SB C18, 2.1mm × 100mm, 1.8 μm;
(d) establishing a fried perilla seed contrast characteristic spectrum: respectively and precisely absorbing 2 mul of mixed reference substance solution and sample solution, injecting into a high performance liquid chromatograph, measuring, establishing a fried perilla seed control characteristic map by adopting a traditional Chinese medicine chromatogram fingerprint map similarity evaluation system, determining that the fried perilla seed control characteristic map has 9 characteristic peaks, namely a peak 1, a peak 2, a peak 3, a peak 4, a peak X1, a peak X2, a peak 5, a peak 6 and a peak 7, and taking the peak 6 as a reference peak, wherein the relative retention time of each characteristic peak is respectively: 0.32, 0.43, 0.73, 0.88, 0.95, 0.96, 0.97, 1.0, 1.17, the relative retention time of which should be within ± 10% of the specified value;
the characteristic peak attribution is as follows: peak 2 is caffeic acid, Peak 6 is rosmarinic acid, Peak 7 is luteolin.
2. The use of claim 1, wherein the preparation of the test solution: sieving parched fructus Perillae decoction pieces with a second sieve, weighing 0.5g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml 80% methanol, weighing, ultrasonic treating for 30 min with ultrasonic power of 250W and ultrasonic frequency of 40KHz, cooling, supplementing 80% methanol to reduce weight loss, shaking, filtering, and collecting the filtrate.
3. The use as claimed in claim 1, wherein the content of rosmarinic acid in the roasted perilla seed is not less than 0.20%.
4. The use of claim 1, wherein the stir-frying process of the perilla seeds comprises: controlling the pot temperature at 190 ℃, the electric ceramic furnace power at 1000W, the processing time at 4 minutes and the stir-frying frequency at 60 times/minute.
5. The use according to claim 4, wherein the temperature of the material is controlled to be in the range of 155 ℃ to 160 ℃.
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