Quality control method for total polysaccharide in production process of fermented cordyceps sinensis powder by near-infrared analysis
阅读说明：本技术 近红外分析发酵虫草菌粉生产过程总多糖的质量控制方法 (Quality control method for total polysaccharide in production process of fermented cordyceps sinensis powder by near-infrared analysis ) 是由 陈丽华 朱卫丰 管咏梅 金晨 吴璐 史畑女 于 2019-10-21 设计创作，主要内容包括：本发明提供了一种近红外分析发酵虫草菌粉生产过程总多糖的质量控制方法,步骤如下：步骤S1,采用传统的方法检测总多糖标准含量；步骤S2,测定所述发酵虫草菌粉原始样品的平均光谱值为发酵虫草菌粉原始光谱；步骤S3,采用TQ Analyst软件分析所述发酵虫草菌粉原始光谱,将步骤S1与步骤S2结合得到定量分析模型；步骤S4,对发酵虫草菌粉待测样品进行近红外光谱扫描得到近红外扫描图谱；步骤S5,将近红外扫描图谱输入TQ Analyst软件进行分析,利用步骤S3得到的所述定量分析模型计算获得所述发酵虫草菌粉待测样品的总多糖含量。与相关技术相比,本发明提供的近红外分析发酵虫草菌粉生产过程总多糖的质量控制方法,快速、操作简单且不破坏样品。(The invention provides a quality control method for analyzing total polysaccharide in a production process of fermented cordyceps sinensis powder by near infrared, which comprises the following steps: step S1, detecting the standard content of total polysaccharide by a traditional method; step S2, determining the average spectral value of the original sample of the fermented cordyceps sinensis powder as the original spectrum of the fermented cordyceps sinensis powder; step S3, analyzing the original spectrum of the fermented cordyceps sinensis powder by adopting TQ Analyst software, and combining the step S1 with the step S2 to obtain a quantitative analysis model; step S4, performing near infrared spectrum scanning on a sample to be detected of the fermented cordyceps sinensis powder to obtain a near infrared scanning map; and S5, inputting the near-infrared scanning map into TQ analysis software for analysis, and calculating by using the quantitative analysis model obtained in the step S3 to obtain the total polysaccharide content of the sample to be detected of the fermented cordyceps sinensis powder. Compared with the related technology, the quality control method for analyzing the total polysaccharide in the production process of the fermented cordyceps sinensis powder by near infrared provided by the invention is rapid, simple to operate and does not damage samples.)
1. A quality control method for analyzing total polysaccharide in the production process of fermented cordyceps sinensis powder by near infrared is characterized by comprising the following steps:
step S1, detecting the standard content of total polysaccharide in the production process of the fermented cordyceps sinensis powder by adopting a traditional method;
step S2, providing a plurality of operation unit original samples of fermented cordyceps sinensis powder, respectively obtaining a spectral value of each original sample of fermented cordyceps sinensis powder, and taking an average spectral value of each original sample of fermented cordyceps sinensis powder as an original spectrum of fermented cordyceps sinensis powder;
step S3, analyzing the original spectrum of the fermented cordyceps sinensis powder by adopting TQ Analyst software, correlating the standard content of total polysaccharide in the production process of the fermented cordyceps sinensis powder obtained in the step S1 with the original spectrum of the fermented cordyceps sinensis powder obtained in the step S2, and obtaining a quantitative analysis model correlating the standard content of total polysaccharide in the production process of the fermented cordyceps sinensis powder with the original spectrum of the fermented cordyceps sinensis powder;
step S4, providing a sample to be detected of fermented cordyceps sinensis powder, and performing near infrared spectrum scanning on the sample to be detected of fermented cordyceps sinensis powder to obtain a near infrared scanning map of the sample to be detected of fermented cordyceps sinensis powder;
and S5, inputting the obtained near-infrared scanning spectrum into TQ analysis software for analysis, and calculating by using the quantitative analysis model obtained in the step S3 to obtain the total polysaccharide content of the sample to be detected of the fermented cordyceps sinensis powder.
2. The quality control method for the total polysaccharide in the production process of the fermented cordyceps sinensis powder according to claim 1, wherein the standard content of the total polysaccharide in the whole production process of the fermented cordyceps sinensis powder is determined by a phenol-sulfuric acid method in the step S1.
3. The quality control method for the near-infrared analysis of the total polysaccharides in the production process of the fermented cordyceps sinensis powder according to claim 2, wherein the step S1 comprises the following substeps:
step S11, extracting polysaccharide, precisely weighing 2g of Cordyceps powder, placing into a round bottom flask, adding 30ml of double distilled water, heating and refluxing at 100 deg.C for 2 times, each time for 1 hr, filtering while hot, mixing filtrates, and heating at 4000 r.min-1Centrifuging for 15min to remove precipitate, concentrating the supernatant according to a volume ratio of 1:5, adding 3 times of anhydrous ethanol into the concentrated supernatant, performing alcohol precipitation in a refrigerator at 4 deg.C for 12 hr, and subjecting the polysaccharide solution to alcohol precipitation at 4000r min-1Centrifuging for 15min, collecting precipitate, dissolving the precipitate in 15ml double distilled water, adding equal volume Sevage reagent, extracting for 3 times, collecting supernatant 8000r min-1Centrifuging for 15min, collecting supernatant, adding 3 times volume of 95% ethanol, 8000r min-1Centrifuging for 15min, collecting precipitate, dissolving in appropriate amount of double distilled water, and freeze drying to obtain fermented Cordyceps powder polysaccharide extract;
step S12, preparing a test sample solution, precisely weighing 2mg of the fermented cordyceps sinensis powder polysaccharide extract, placing the extract in a 2ml volumetric flask, adding double distilled water to dissolve the extract and fixing the volume to a scale mark to obtain the fermented cordyceps sinensis powder solution, precisely weighing 1ml of the fermented cordyceps sinensis powder solution, placing the solution in a 25ml volumetric flask, adding double distilled water to dissolve the solution and diluting the solution to the scale mark to obtain the test sample solution;
step S13, scanning at full wavelength, precisely measuring 2ml of glucose solution and 2ml of sample solution into a 25ml test tube with a plug, adding 0.7ml of 4% phenol solution, slowly adding 5ml of concentrated sulfuric acid, placing in a boiling water bath for 20min, taking out, placing at room temperature, taking 2ml of water as a blank for color development, taking the blank as a reference, and scanning the sample between 200 and 800;
step S14, establishing a glucose standard curve, precisely weighing 5mg of glucose, placing the glucose in a 10ml volumetric flask, adding and dissolving the glucose mother liquor, setting the glucose mother liquor to a scale mark to obtain a glucose mother liquor, precisely absorbing 0.4ml, 0.45ml, 0.6ml, 0.7ml, 0.8ml and 1.4ml of the glucose mother liquor into the 10ml volumetric flask, respectively adding double distilled water to dilute the glucose mother liquor to the scale mark to obtain glucose reference solutions with different concentrations, precisely transferring 2ml to 25ml of the glucose reference solutions with serial concentrations into a glass test tube with a plug, measuring absorbance at a position of 489nm wavelength after color development under the condition of the step S13, and making a working curve according to the corresponding concentration of the absorbance;
and step S15, after the sample solution prepared in the step S12 is developed under the condition of the step S13, measuring absorbance at the wavelength of 489nm, and substituting the absorbance into the working curve to calculate the standard content of the total polysaccharide in the production process of the fermented cordyceps sinensis powder.
4. The quality control method for the total polysaccharide in the production process of the fermented cordyceps sinensis powder by the near-infrared analysis according to claim 3, wherein the step S1 further comprises the step S16: arranging the standard contents of total polysaccharides in the production processes of the fermented cordyceps sinensis powder in different batches and different processes obtained in the step S15 in descending order, and selecting the correction set and the verification set according to the proportion of 5:1 under the condition of ensuring that the contents of the correction set comprise the contents of the verification set.
5. The method for quality control of total polysaccharides in the near-infrared analysis fermented cordyceps sinensis powder production process according to claim 4, wherein in step S3, the quantitative analysis model is verified by using the verification set obtained in step S16 as external data, the true value of the polysaccharide content measured by the phenol-sulfuric acid method in the verification set is compared with the predicted value of the quantitative analysis model, and the model error rate is calculated to verify the accuracy of the quantitative analysis model.
6. The quality control method for the near-infrared analysis of the total polysaccharides in the production process of the fermented cordyceps sinensis powder according to claim 1, wherein in the step S2, an integrating sphere mode is adopted to collect the spectrum of an original sample of the fermented cordyceps sinensis powder, and the collection process is as follows: wave number range is 4000-12500cm-1Scanning 64 times with a resolution of 8cm-1Air signal was collected as background, and the background was automatically subtracted during the experiment at 25 ℃ with a humidity of 40% and the spectrum was displayed as log 1/R.
7. The method for quality control of total polysaccharides in the near-infrared analysis of fermented cordyceps sinensis powder production process according to claim 1, wherein in step S3, the determination of the quantitative analysis model comprises the following steps: and establishing a partial least squares regression quantitative analysis model, comparing and analyzing results of the multivariate scattering correction combined with the original spectrum, the first derivative, the second derivative and the Savitzky-Golay smoothing spectrum, and screening out the optimal quantitative analysis model by taking the mean square error of the correction set, the mean square error of the verification set, the correlation coefficient of the correction set and the correlation coefficient of the verification set as indexes.
8. The method for quality control of total polysaccharides in the process of producing fermented Cordyceps sinensis powder by near-infrared analysis according to claim 1, wherein in step S3, the wave number range of the quantitative analysis model is 10526.3-8333.33cm-1、9903.9-6521.88cm-1Or 6667.11-4545.45cm-1。
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of product production process detection, in particular to a quality control method for analyzing total polysaccharide in a fermented cordyceps sinensis powder production process by near infrared.
[ background of the invention ]
The fermented Cordyceps powder is prepared by liquid submerged fermentation and processing of medicinal strains, and has effects of nourishing lung yin and invigorating kidney yang. Researches prove that the chemical components of the fermented cordyceps sinensis powder product are similar to those of cordyceps sinensis, and the fermented cordyceps sinensis powder product mainly contains nucleosides, sterols, polysaccharides, amino acids and other main components and can be used as a sustainable substitute of the cordyceps sinensis. The polysaccharide is one of active ingredients, and has the effects of protecting liver, reducing blood pressure, promoting immunity, resisting hyperglycemia, hyperlipidemia, resisting oxidation, resisting anoxia, resisting tumor, resisting hepatic fibrosis, promoting reverse cholesterol transport and the like, but only adenosine and ergosterol exist under the quality standard of a Jinshuibao capsule product of fermented cordyceps sinensis powder, and the polysaccharide is not listed in the Jinshuibao capsule product, so the quality control of the polysaccharide becomes a difficult problem.
Meanwhile, the chemical content measurement method of polysaccharide mainly comprises PMP derivatization-high performance liquid chromatography, phenol-sulfuric acid method, anthrone-sulfuric acid method and the like, and the chemical measurement method has complicated pretreatment steps, uses more organic reagents and damages samples, and cannot meet the requirements of modern rapid analysis and high-efficiency quality control.
Therefore, aiming at the defects that the polysaccharide detection method in the prior art is complicated in steps, easily damages samples and cannot meet the requirements of rapid analysis and high-efficiency quality control, a new quality control method for the total polysaccharide in the whole process of producing the fermented cordyceps sinensis powder, which can monitor the content of the polysaccharide at any time and can feed back and adjust the fermentation production process, is needed to solve the problems.
[ summary of the invention ]
The invention aims to solve the technical problems that the polysaccharide detection method in the prior art is complicated in steps, easy to damage samples and incapable of meeting the requirements of rapid analysis and efficient quality control, and provides a total polysaccharide quality control method in the whole process of producing fermented cordyceps sinensis powder, which can monitor the content of polysaccharide at any time and can feed back and adjust the fermentation production process.
A quality control method for analyzing total polysaccharide in the production process of fermented cordyceps sinensis powder by near infrared comprises the following steps:
step S1, detecting the standard content of total polysaccharide in the production process of the fermented cordyceps sinensis powder by adopting a traditional method;
step S2, providing a plurality of operation unit original samples of fermented cordyceps sinensis powder, respectively obtaining a spectral value of each original sample of fermented cordyceps sinensis powder, and taking an average spectral value of each original sample of fermented cordyceps sinensis powder as an original spectrum of fermented cordyceps sinensis powder;
step S3, analyzing the original spectrum of the fermented cordyceps sinensis powder by adopting TQ Analyst software, correlating the standard content of total polysaccharide in the production process of the fermented cordyceps sinensis powder obtained in the step S1 with the original spectrum of the fermented cordyceps sinensis powder obtained in the step S2, and obtaining a quantitative analysis model correlating the standard content of total polysaccharide in the production process of the fermented cordyceps sinensis powder with the original spectrum of the fermented cordyceps sinensis powder;
step S4, providing a sample to be detected of fermented cordyceps sinensis powder, and performing near infrared spectrum scanning on the sample to be detected of fermented cordyceps sinensis powder to obtain a near infrared scanning map of the sample to be detected of fermented cordyceps sinensis powder;
and S5, inputting the obtained near-infrared scanning spectrum into TQ analysis software for analysis, and calculating by using the quantitative analysis model obtained in the step S3 to obtain the total polysaccharide content of the sample to be detected of the fermented cordyceps sinensis powder.
Preferably, in the step S1, the standard content of total polysaccharide in the whole production process of the fermented cordyceps sinensis powder is determined by adopting a phenol-sulfuric acid method.
Preferably, the step S1 includes the following sub-steps:
step S11, extracting polysaccharide, precisely weighing 2g Cordyceps powder, placing into a round bottom flask, adding 30ml double distilled water, heating and refluxing at 100 deg.C for 2 times, each time for 1 hr, filtering while hot, mixing, filteringLiquid, 4000 r.min-1Centrifuging for 15min to remove precipitate, concentrating the supernatant according to a volume ratio of 1:5, adding 3 times of anhydrous ethanol into the concentrated supernatant, performing alcohol precipitation in a refrigerator at 4 deg.C for 12 hr, and subjecting the polysaccharide solution to alcohol precipitation at 4000r min-1Centrifuging for 15min, collecting precipitate, dissolving the precipitate in 15ml double distilled water, adding equal volume Sevage reagent, extracting for 3 times, collecting supernatant 8000r min-1Centrifuging for 15min, collecting supernatant, adding 3 times volume of 95% ethanol, 8000r min-1Centrifuging for 15min, collecting precipitate, dissolving in appropriate amount of double distilled water, and freeze drying to obtain fermented Cordyceps powder polysaccharide extract;
step S12, preparing a test sample solution, precisely weighing 2mg of the fermented cordyceps sinensis powder polysaccharide extract, placing the extract in a 2ml volumetric flask, adding double distilled water to dissolve the extract and fixing the volume to a scale mark to obtain the fermented cordyceps sinensis powder solution, precisely weighing 1ml of the fermented cordyceps sinensis powder solution, placing the solution in a 25ml volumetric flask, adding double distilled water to dissolve the solution and diluting the solution to the scale mark to obtain the test sample solution;
step S13, scanning at full wavelength, precisely measuring 2ml of glucose solution and 2ml of sample solution into a 25ml test tube with a plug, adding 0.7ml of 4% phenol solution, slowly adding 5ml of concentrated sulfuric acid, placing in a boiling water bath for 20min, taking out, placing at room temperature, taking 2ml of water as a blank for color development, taking the blank as a reference, and scanning the sample between 200 and 800;
step S14, establishing a glucose standard curve, precisely weighing 5mg of glucose, placing the glucose in a 10ml volumetric flask, adding and dissolving the glucose mother liquor, setting the glucose mother liquor to a scale mark to obtain a glucose mother liquor, precisely absorbing 0.4ml, 0.45ml, 0.6ml, 0.7ml, 0.8ml and 1.4ml of the glucose mother liquor into the 10ml volumetric flask, respectively adding double distilled water to dilute the glucose mother liquor to the scale mark to obtain glucose reference solutions with different concentrations, precisely transferring 2ml to 25ml of the glucose reference solutions with serial concentrations into a glass test tube with a plug, measuring absorbance at a position of 489nm wavelength after color development under the condition of the step S13, and making a working curve according to the corresponding concentration of the absorbance;
and step S15, after the sample solution prepared in the step S12 is developed under the condition of the step S13, measuring absorbance at the wavelength of 489nm, and substituting the absorbance into the working curve to calculate the standard content of the total polysaccharide in the production process of the fermented cordyceps sinensis powder.
Preferably, the step S1 further includes the step S16: arranging the standard contents of total polysaccharides in the production processes of the fermented cordyceps sinensis powder in different batches and different processes obtained in the step S15 in descending order, and selecting the correction set and the verification set according to the proportion of 5:1 under the condition of ensuring that the contents of the correction set comprise the contents of the verification set.
Preferably, in step S3, the quantitative analysis model is verified by using the verification set obtained in step S16 as external data, the true value of the polysaccharide content measured by the phenol-sulfuric acid method in the verification set is compared with the predicted value of the quantitative analysis model, a model error rate is calculated, and the accuracy of the quantitative analysis model is verified.
Preferably, in step S2, the spectrum of the original sample of the fermented cordyceps sinensis powder is collected in an integrating sphere mode, and the collection process is as follows: wave number range is 4000-12500cm-1Scanning 64 times with a resolution of 8cm-1Air signal was collected as background, and the background was automatically subtracted during the experiment at 25 ℃ with a humidity of 40% and the spectrum was displayed as log 1/R.
Preferably, in step S3, the determining of the quantitative analysis model includes the following steps: and establishing a partial least squares regression quantitative analysis model, comparing and analyzing results of the multivariate scattering correction combined with the original spectrum, the first derivative, the second derivative and the Savitzky-Golay smoothing spectrum, and screening out the optimal quantitative analysis model by taking the mean square error of the correction set, the mean square error of the verification set, the correlation coefficient of the correction set and the correlation coefficient of the verification set as indexes.
Preferably, in step S3, the wave number range of the quantitative analysis model is 10526.3-8333.33cm-1、9903.9-6521.88cm-1Or 6667.11-4545.45cm-1。
Compared with the related technology, the quality control method for analyzing the total polysaccharide in the production process of the fermented cordyceps sinensis powder by near infrared adopts the near infrared spectrum as one of the process analysis technologies, has the characteristics of rapidness, no damage and low cost, and meets the modern quality control requirement; meanwhile, a simpler phenol-sulfuric acid method is adopted to determine the standard content of the total polysaccharide in the whole production process of the fermented cordyceps sinensis powder, and the quality of the total polysaccharide is controlled from the source based on each operation unit (strain culture, strain passage, strain fermentation, strain filtration, strain drying, strain crushing and strain mixing) of the fermented cordyceps sinensis powder production, so that the product quality in the production process of the fermented cordyceps sinensis powder is stable and controllable; in addition, the fermentation conditions have great influence on the activity of the polysaccharide, so that the content of the polysaccharide is monitored at any time, the fermentation production process is very necessary to be fed back and regulated, the near infrared spectrum has the characteristics of accuracy and quickness, and a total polysaccharide quantitative analysis model in the whole process chain is established by combining the near infrared spectrum with a partial least squares regression method, so that a preliminary basis is provided for producing the fermented cordyceps sinensis powder with the maximized polysaccharide activity.
[ description of the drawings ]
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without inventive efforts, wherein:
FIG. 1 is a schematic flow chart of a quality control method for analyzing total polysaccharides in a production process of fermented Cordyceps sinensis bacteria powder by near infrared;
FIG. 2 is a glucose standard work curve diagram obtained in step 17 of the quality control method for analyzing total polysaccharides in the production process of fermented Cordyceps sinensis bacteria powder according to the present invention;
FIG. 3 is a graph showing the average content of polysaccharide extracts from fermented Cordyceps sinensis bacteria powder in different batches and in the whole process in step 18 of the quality control method for analyzing total polysaccharides in the production process of fermented Cordyceps sinensis bacteria powder by near infrared analysis according to the present invention;
FIG. 4 is an original spectrum of fermented Cordyceps sinensis bacteria powder according to the quality control method for analyzing total polysaccharides in the production process of fermented Cordyceps sinensis bacteria powder provided by the present invention;
FIG. 5 is a scattergram of correlation values between actual values and calculated values of a quantitative model of total polysaccharides in fermented Cordyceps sinensis powder according to the quality control method for analyzing total polysaccharides in the production process of fermented Cordyceps sinensis powder provided by the present invention.
[ detailed description ] embodiments
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a quality control method for analyzing total polysaccharides in a production process of fermented cordyceps sinensis powder by using near infrared, which specifically comprises the following steps:
step S1, detecting the standard content of total polysaccharide in the production process of the fermented cordyceps sinensis powder by adopting a traditional method;
the conventional method can be a phenol-sulfuric acid method, a PMP-high performance liquid chromatography method, an anthrone-sulfuric acid method and the like, and in the embodiment, the phenol-sulfuric acid method is adopted to determine the standard content of the total polysaccharide in the whole production process of the fermented cordyceps sinensis powder.
Specifically, the step S1 includes the following sub-steps:
step S11, extracting polysaccharide, precisely weighing 2g of Cordyceps powder, placing into a round bottom flask, adding 30ml of double distilled water, heating and refluxing at 100 deg.C for 2 times, each time for 1 hr, filtering while hot, mixing filtrates, and heating at 4000 r.min-1Centrifuging for 15min to remove precipitate, concentrating the supernatant according to a volume ratio of 1:5, adding 3 times of anhydrous ethanol into the concentrated supernatant, performing alcohol precipitation in a refrigerator at 4 deg.C for 12 hr, and subjecting the polysaccharide solution to alcohol precipitation at 4000r min-1Centrifuging for 15min, collecting precipitate, dissolving the precipitate in 15ml double distilled water, adding equal volume Sevage reagent, extracting for 3 times, collecting supernatant 8000r min-1Centrifuging for 15min, collecting supernatant, adding 3 times volume of 95% ethanol, 8000r min-1Centrifuging for 15min, collecting precipitate, dissolving in appropriate amount of double distilled water, and freeze drying to obtain fermented Cordyceps powder polysaccharide extract;
wherein the ratio of the trichloromethane to the n-butanol in the Sevage reagent is 4: 1.
Step S12, preparing a test sample solution, precisely weighing 2mg of the fermented cordyceps sinensis powder polysaccharide extract, placing the extract in a 2ml volumetric flask, adding double distilled water to dissolve the extract and fixing the volume to a scale mark to obtain the fermented cordyceps sinensis powder solution, precisely weighing 1ml of the fermented cordyceps sinensis powder solution, placing the solution in a 25ml volumetric flask, adding double distilled water to dissolve the solution and diluting the solution to the scale mark to obtain the test sample solution;
step S13, scanning at full wavelength, precisely measuring 2ml of glucose solution and 2ml of sample solution into a 25ml test tube with a plug, adding 0.7ml of 4% phenol solution, slowly adding 5ml of concentrated sulfuric acid, placing in a boiling water bath for 20min, taking out, placing at room temperature, taking 2ml of water as a blank for color development, taking the blank as a reference, and scanning the sample between 200 and 800;
step S14, please refer to fig. 2, the establishment of the glucose standard curve, precisely weighing 5mg of glucose, placing the glucose into a 10ml volumetric flask, adding the glucose mother liquor which is dissolved and set to the scale mark to obtain a glucose mother liquor, precisely sucking the glucose mother liquor of 0.4ml, 0.45ml, 0.6ml, 0.7ml, 0.8ml and 1.4ml into the 10ml volumetric flask, respectively adding double distilled water to dilute the glucose mother liquor to the scale mark to obtain glucose reference solutions with different concentrations, precisely transferring 2ml to 25ml of the glucose reference solutions with a series of concentrations into a glass test tube with a plug, after developing color under the condition of step S13, measuring absorbance at the wavelength of 489nm, and making a working curve with the corresponding concentration of the absorbance;
step S15, referring to fig. 3, after the sample solution prepared in step S12 is developed under the condition of step S13, measuring absorbance at the wavelength of 489nm, and substituting the absorbance into the working curve to calculate the standard content of total polysaccharide in the production process of the fermented cordyceps sinensis powder;
and S16, arranging the standard contents of total polysaccharides in the production process of the fermented cordyceps sinensis powder obtained in the step S15 in different batches and different processes in a descending order, and selecting the correction set and the verification set according to a ratio of 5:1 under the condition of ensuring that the contents of the correction set comprise the contents of the verification set.
Step S2, referring to fig. 4, providing a plurality of operating unit original samples of fermented cordyceps sinensis powder, respectively obtaining a spectral value of each original sample of fermented cordyceps sinensis powder, and taking an average spectral value of each original sample of fermented cordyceps sinensis powder as an original spectrum of fermented cordyceps sinensis powder;
specifically, in step S2, the spectrum of the original sample of the fermented cordyceps sinensis powder is collected in an integrating sphere mode, and the collection process is as follows: wave number range is 4000-12500cm-1Scanning 64 times with a resolution of 8cm-1Air signal was collected as background, and the background was automatically subtracted during the experiment at 25 ℃ with a humidity of 40% and the spectrum was displayed as log 1/R.
Step S3, analyzing the original spectrum of the fermented cordyceps sinensis powder by adopting TQ Analyst software, correlating the standard content of total polysaccharide in the production process of the fermented cordyceps sinensis powder obtained in the step S1 with the original spectrum of the fermented cordyceps sinensis powder obtained in the step S2, and obtaining a quantitative analysis model correlating the standard content of total polysaccharide in the production process of the fermented cordyceps sinensis powder with the original spectrum of the fermented cordyceps sinensis powder;
preferably, the wave number range of the quantitative analysis model is 10526.3-8333.33cm-1、9903.9-6521.88cm-1Or 6667.11-4545.45cm-1。
Specifically, referring to fig. 5, after the quantitative analysis model is obtained, the verification set obtained in step S16 is used as external data to verify the quantitative analysis model, the true value of the polysaccharide content measured by the phenol-sulfuric acid method in the verification set is compared with the predicted value of the quantitative analysis model, the error rate of the model is calculated, and the accuracy of the quantitative analysis model is verified. The result is shown in table 1, and the error rate is 0.0018% -0.0498% as can be seen from table 1, the error between the predicted value and the true value of the obtained model is small, and the accuracy is high.
TABLE 1 comparison of the predicted value and the actual value of PLSR quantitative analysis model for total polysaccharides of fermented Cordyceps powder
Specifically, the determination process of the quantitative analysis model is as follows: establishing a Partial Least Squares Regression (PLSR) quantitative analysis model, and screening an optimal quantitative analysis model by combining results Of an original spectrum, a first derivative, a second derivative and a Savitzky-Golay (S-G) smoothing spectrum with a Correction set Mean Square error Of Prediction (RMSEC), a verification set Mean Square error Of Prediction (RMSEP) and a Correction set correlation coefficient (Rc) and a verification set correlation coefficient (Rp) as indexes by comparing and analyzing results Of a Multivariate Scatter Correction (MSC) and a Savitzky-Golay smoothing spectrum. Wherein, the performance index results of different pretreatment models are shown in Table 2.
TABLE 2 Performance index for different pretreatment modes
Step S4, providing a sample to be detected of fermented cordyceps sinensis powder, and performing near infrared spectrum scanning on the sample to be detected of fermented cordyceps sinensis powder to obtain a near infrared scanning map of the sample to be detected of fermented cordyceps sinensis powder;
and S5, inputting the obtained near-infrared scanning spectrum into TQ analysis software for analysis, and calculating by using the quantitative analysis model obtained in the step S3 to obtain the total polysaccharide content of the sample to be detected of the fermented cordyceps sinensis powder.
The fermented cordyceps sinensis powder used in the invention is fermented cordyceps sinensis powder (Cs-4) produced by Jiangxi national drug Limited liability company.
Compared with the related technology, the quality control method for analyzing the total polysaccharide in the production process of the fermented cordyceps sinensis powder by near infrared adopts the near infrared spectrum as one of the process analysis technologies, has the characteristics of rapidness, no damage and low cost, and meets the modern quality control requirement; meanwhile, a simpler phenol-sulfuric acid method is adopted to determine the standard content of the total polysaccharide in the whole production process of the fermented cordyceps sinensis powder, and the quality of the total polysaccharide is controlled from the source based on each operation unit (strain culture, strain passage, strain fermentation, strain filtration, strain drying, strain crushing and strain mixing) of the fermented cordyceps sinensis powder production, so that the product quality in the production process of the fermented cordyceps sinensis powder is stable and controllable; in addition, the fermentation conditions have great influence on the activity of the polysaccharide, so that the content of the polysaccharide is monitored at any time, the fermentation production process is very necessary to be fed back and adjusted, the near infrared spectrum has the characteristics of accuracy and quickness, and a total polysaccharide quantitative analysis model in the whole process chain is established by combining the near infrared spectrum with a partial least squares regression method, so that a preliminary basis is provided for producing the fermented cordyceps sinensis powder with the maximized polysaccharide activity.
While the foregoing is directed to embodiments of the present invention, it will be understood by those skilled in the art that various changes may be made without departing from the spirit and scope of the invention.