CN114428061A - Method for predicting total polysaccharide content in fiddlehead based on ultraviolet-visible-near infrared spectrum - Google Patents
Method for predicting total polysaccharide content in fiddlehead based on ultraviolet-visible-near infrared spectrum Download PDFInfo
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Abstract
The invention discloses a method for predicting the content of total polysaccharide in fiddlehead based on an ultraviolet-visible-near infrared spectrum, which relates to the technical field of fiddlehead quality detection and comprises the following steps: (1) collecting an ultraviolet-visible-short wave near-infrared spectrogram of a fiddlehead powder sample for multiple times by using an ultraviolet-visible near-infrared spectrophotometer, wherein the measurement range of the ultraviolet-visible near-infrared spectrophotometer is 200-1100 nm; (2) preprocessing spectral data: preprocessing the spectral data by adopting a first derivative method; (3) screening wavelength variables; (4) and predicting the content of the total polysaccharide in the bracken. The invention has the beneficial effects that: the method comprises the steps of collecting ultraviolet-visible-short wave near infrared spectrum data of a bracken sample, introducing the collected data into a quantitative analysis model, and predicting the total polysaccharide content of the bracken sample. The method realizes rapid nondestructive detection of total polysaccharide content in herba Fimbristylis Dichotomae, and can be used for rapid detection of herba Fimbristylis Dichotomae quality evaluation.
Description
Technical Field
The invention relates to the technical field of bracken quality detection, in particular to a method for predicting the content of total polysaccharides in bracken based on an ultraviolet-visible-near infrared spectrum.
Background
Fiddlehead is a spore plant, also known as ottelia acuminata, ruyi vegetable, fist-shaped vegetable, etc. The fern can grow in mountain and forest fields, is less polluted, is delicious to eat and crisp in taste, can be used as a medicine for both rhizomes and whole grass of fern, has high medicinal value, and becomes a mountain and wild vegetable which is deeply loved by people in recent years.
The bracken is rich in nutrient components, flavonoid, polysaccharide, protein and the like, the content of the total polysaccharide is used as one of important indexes for evaluating the quality of the bracken and products thereof, but the research on the bracken polysaccharide is relatively less, and the research on the total polysaccharide component in the bracken has important significance for the deep development of bracken resources. The traditional method for determining the content of the total polysaccharide in the fiddlehead mainly adopts an anthrone-sulfuric acid colorimetric method (Hakuwaning, Chenlinlin, Sihuayang, and the like, fiddlehead polysaccharide ultrasonic-assisted extraction and pharmacological activity preliminary research [ J ] natural product research and development, 2019,031(006): 957-.
Ultraviolet-visible-short wave near infrared spectroscopy (UV-visible-short wave near infrared spectrum, UV-Vis-SWNIR-DRS) is used as a rapid and nondestructive analysis technology, has the characteristics of simplicity, rapidness, cost saving and the like, is applied to the aspects of soil and cancer in-situ diagnosis, traditional Chinese medicine identification and the like, and is only rarely researched and applied to the detection of chemical components in plant powder samples. And compared with the near infrared spectrum or the mid-infrared spectrum, the ultraviolet-visible-short wave near infrared spectrum can reflect the change of electrons in the sample by removing the vibration of molecules through the spectrum information, so that the spectrum data is richer. This technique is less studied in quantitative detection. The problems that the spectral information is complex, the correlation between the quantitative components and the spectral information is not strong, and the interference of wavelength variables on the accuracy of the model is not relevant are solved in the detection process.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for predicting the content of total polysaccharides in fiddlehead based on an ultraviolet-visible-near infrared spectrum.
The invention solves the technical problems through the following technical means:
a method for predicting the content of total polysaccharides in fiddlehead based on an ultraviolet-visible-near infrared spectrum comprises the following steps:
(1) collecting an ultraviolet-visible-short wave near-infrared spectrogram of a fiddlehead powder sample for multiple times by using an ultraviolet-visible near-infrared spectrophotometer, wherein the measurement range of the ultraviolet-visible near-infrared spectrophotometer is 200-1100 nm;
(2) preprocessing spectral data: preprocessing the spectral data by adopting a first derivative method;
(3) screening wavelength variables: screening 388-566 nm, 744-833 nm and 1011-1100 nm three wave bands to establish effective wavelengths of a PLS model;
(4) predicting the content of the total polysaccharide of the bracken: and (4) combining the wavelength variable in the step (3) with the total polysaccharide content of the bracken sample, establishing a quantitative model of the wavelength variable and the total polysaccharide content of the bracken sample by a partial least square method, and predicting the total polysaccharide content of the bracken according to the quantitative model.
Has the advantages that: the ultraviolet-visible-near infrared spectrum technology is applied to the rapid quantitative analysis research of the total polysaccharide components in the fiddlehead for the first time, and the method of multiple acquisition and spectrum pretreatment of the same sample is adopted, so that the influence of manual sampling errors and spectrum noise on an ultraviolet-visible-short wave near infrared spectrogram can be effectively reduced; the constructed quantitative model of the total polysaccharide content in the bracken can quickly predict the total polysaccharide content in the bracken sample.
The method has the advantages that the spectrum information is complex in the detection process, the correlation between the quantitative components and the spectrum information is not strong, and the interference of the wavelength variable on the accuracy of the model is avoided.
Preferably, the preparation method of the bracken powder sample comprises the following steps: picking fresh bracken samples, cleaning, removing impurities, cutting into sections, drying at 60 ℃, and collecting powder of 60-100 meshes.
Preferably, the bracken powder sample is stored under closed dry conditions.
Has the advantages that: the bracken powder samples are processed in a consistent mode, sample difference can be reduced, the bracken powder samples are dried to meet detection requirements, and the bracken powder samples are stored under a closed drying condition to ensure stability of the bracken samples.
Preferably, the bracken samples are collected from different production locations, at different time periods.
Has the advantages that: and the sample range is enlarged, so that the application range of the model is enlarged.
Preferably, the bracken powder sample has a total polysaccharide content ranging from 2.30% to 7.592%.
Preferably, the spectrum acquisition in the step (1) comprises the following steps:
(a) dividing the bracken powder sample into a correction set sample, a prediction set sample and a complete external verification sample according to the proportion of 4:2: 1;
(b) the method comprises the steps of placing a fiddlehead powder sample in a quartz single-reflection accessory sample pool equipped with an ultraviolet-visible-near infrared spectrometer, setting the measurement range of a Hitachi ultraviolet-visible near infrared spectrophotometer to be 200-1100 nm, setting the scanning frequency of the Hitachi ultraviolet-visible near infrared spectrophotometer to be 32 times, setting the resolution to be 4.0nm, and repeatedly collecting the same sample for 6 times to obtain original spectral data.
Preferably, the total polysaccharide content of the prediction set samples is verified using the established quantitative model, and the external verification is performed using a complete external verification sample.
Has the advantages that: the verification proves that the invention can provide a reliable method for the determination and research of the content of the total polysaccharide of the bracken.
Preferably, the spectrum preprocessing in the step (2) comprises the following steps: performing baseline correction and average spectrogram calculation on an ultraviolet-visible-short wave near-infrared spectrogram collected by the same fiddlehead powder sample to obtain an average spectrogram, eliminating the spectrogram caused by manual sampling errors, eliminating spectral noise caused by a detection environment by an average spectrum moving average 15-point smoothing method, and finally processing spectral data by a first derivative method.
Has the advantages that: 8 spectrum preprocessing methods are compared, a constant variable offset method, a maximum-minimum normalization method, a vector normalization method, a multivariate scattering correction method, a first derivative method, a second derivative method, a multivariate scattering correction plus first derivative method and a vector normalization plus first derivative method are eliminated to screen the preprocessing methods, and R of a PLS model correction set is compared2And correcting the set root mean square error RMSECV value to obtain the optimal spectrum preprocessing data processed by the first derivative method.
Preferably, the method for detecting the total polysaccharide content of the bracken sample in the step (4) comprises the following steps:
(a) weighing a bracken powder sample, and mixing the raw materials according to a material-liquid ratio of 1: 15, adding distilled water, carrying out condensation reflux extraction at 95 ℃, filtering and collecting filtrate, extracting filter residues, combining the extracting solutions and placing the combined extracting solutions in a volumetric flask for later use;
(b) using anthrone-sulfuric acid ratioColor method, measuring total polysaccharide content in herba Fimbristylis Dichotomae, measuring absorbance at 620nm wavelength with glucose as standard substance to obtain standard curve equation of glucose (Y is 50.029X-0.0035, R is20.999, wherein X is glucose concentration mg/mL and Y is absorbance A.
Preferably, the uv-vis-nir spectrophotometer is hitachi uv-vis-nir spectrophotometer UH 4150.
The invention has the advantages that: the ultraviolet-visible-near infrared spectrum technology is applied to the rapid quantitative analysis research of the total polysaccharide components in the fiddlehead for the first time, and the method of multiple acquisition and spectrum pretreatment of the same sample is adopted, so that the influence of manual sampling errors and spectrum noise on an ultraviolet-visible-short wave near infrared spectrogram can be effectively reduced; the constructed quantitative model of the total polysaccharide content in the bracken can quickly predict the total polysaccharide content in the bracken sample.
The method has the advantages that the spectrum information is complex in the detection process, the correlation between the quantitative components and the spectrum information is not strong, and the interference of the wavelength variable on the accuracy of the model is avoided.
The bracken powder samples are processed in a consistent mode, sample difference can be reduced, the bracken powder samples are dried to meet detection requirements, and the bracken powder samples are stored under a closed drying condition to ensure stability of the bracken samples.
The bracken samples are collected from different production places and different periods, so that the sample range can be enlarged, and the accuracy of the detection result is improved.
The verification proves that the invention can provide a reliable method for the determination and research of the content of the total polysaccharide of the bracken.
Drawings
FIG. 1 is a flow chart of a quantitative analysis method for the total polysaccharide content in fiddlehead based on UV-visible-shortwave near infrared spectroscopy combined with chemometrics analysis in an embodiment of the present invention;
FIG. 2 is a graph of the original UV-VISIBLE-SHORT-WAVE NIR spectra of several samples of bracken according to an embodiment of the present invention;
FIG. 3 is a graph of a first derivative method pre-treatment spectrum of several bracken samples according to an embodiment of the present invention;
FIG. 4 is a graph of the predicted effect of the quantitative analysis model of total polysaccharides in fiddlehead samples according to the embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
The Hitachi ultraviolet visible near infrared spectrophotometer (UH4150) is equipped with a sample cell with a quartz single reflection accessory.
Step one, collecting a fiddlehead sample. Collecting fiddlehead samples at different producing areas and different periods. The quantity of the bracken samples is enough, so that the adaptability of establishing the model is improved.
And step two, preparing a bracken powder sample. Dividing the collected fresh bracken samples into 14 groups, each group comprises 10 samples, sorting, cleaning, removing impurities, cutting into segments, drying at 60 ℃, crushing, sieving, collecting powder of 60-100 meshes, drying, sealing and storing for later use.
And step three, dividing 140 parts of the fiddlehead samples prepared in the step one into 80 parts of correction set samples, 40 parts of prediction set samples and 20 parts of complete external verification set samples, and acquiring the spectral data of each fiddlehead sample by using a Hitachi ultraviolet visible near-infrared spectrophotometer. Before the spectral data is collected, the Hitachi ultraviolet visible near-infrared spectrophotometer is started and preheated for 0.5h, and meanwhile, neutral alumina powder is used as a blank control to eliminate spectral noise caused by a detection environment when a sample is detected every time.
Step four, the process of spectrum collection is as follows: the fiddlehead powder sample is placed in a quartz single-reflection accessory sample pool equipped with an ultraviolet visible near-infrared spectrophotometer, the measurement range of the Hitachi ultraviolet visible near-infrared spectrophotometer is set to be 200-1100 nm, the scanning frequency of the Hitachi ultraviolet visible near-infrared spectrophotometer is set to be 32 times, the resolution ratio is set to be 4.0nm, and the same sample is repeatedly collected for 6 times to obtain original spectral data.
Step five, accurately weighing 2.0g of fiddlehead dry powder, and mixing the weighed materials according to a material-liquid ratio of 1: 15, adding 30mL of distilled water, carrying out condensation reflux extraction for 2 h/time at 95 ℃, filtering and collecting filtrate, extracting filter residues for 2 times, combining the extracting solutions and placing in a volumetric flask for later use. The content of total polysaccharide in the bracken is determined by adopting an anthrone-sulfuric acid colorimetric method. Measuring absorbance at 620nm wavelength with glucose as standard substance to obtain standard curve equation of glucose (Y is 50.029X-0.0035, R)20.999. (X is a glucose concentration mg/mL, and Y is an absorbance A).
Step six, spectrum pretreatment: and performing baseline correction and average spectrogram calculation on the original spectrogram of the ultraviolet-visible-short wave near infrared spectrum acquired 6 times by the same fiddlehead sample to obtain an average spectrum, and eliminating data difference caused by artificial sampling errors.
8 spectrum pretreatment methods were applied: and (3) screening a preprocessing method by combining a constant variable offset elimination method, a maximum-minimum normalization method, a vector normalization method, a multivariate scattering correction method, a first derivative method, a second derivative method, a multivariate scattering correction plus first derivative method, a vector normalization plus first derivative method and a Partial Least Squares (PLS).
By comparing R of the PLS model correction set2Cross-validating the root mean square error RMSECV value to obtain a higher R value by using a spectral preprocessing method of a first derivative method2The value 0.6618, the minimum RMSECV value was 0.765, and the UV-VISIBLE-SHORT-WAVE NIR spectra of the bracken samples pretreated by the first derivative method were obtained.
OPUS7 was used.5, optimizing a modeling wavelength and a PLS algorithm by software to construct a model, wherein the optimized wavelengths are 388-566 nm, 744-833 nm and 1011-1100 nm, and 3 wave bands are obtained to obtain higher R2Value 0.7430, minimum RMSECV value 0.667%.
Step seven, establishing a correction model of the content of the total polysaccharides in the fiddlehead: and establishing a quantitative model between the spectral characteristic variables and the total polysaccharide content of 80 correction set samples by a partial least square method. The correlation coefficient of the obtained model correction set is 0.9066, and the root mean square error is 0.421%.
Step eight, verifying a total polysaccharide content correction model in the fiddlehead: the total polysaccharide content in 40 samples of the predicted fiddlehead was verified using this quantitative model, and in addition, a complete external test was performed using 20 samples of fiddlehead. The correlation coefficient for the prediction set was 0.7834, the root mean square error was 0.639%, and in addition, complete external testing was performed using 20 samples of bracken with errors ranging from-1.33% to 1.125%. The method can provide a reliable method for the determination and research of the content of the total polysaccharide in the bracken.
Examples
The method for predicting the content of total polysaccharides in fiddlehead based on the ultraviolet-visible-near infrared spectrum specifically comprises the following steps:
1. collection of bracken samples
Collecting fiddlehead samples in different producing areas and different periods to enlarge the adaptive range of the model.
2. Preparation of bracken powder samples
Collecting 14 groups of fresh bracken samples, 10 samples of each group, picking, cleaning, removing impurities, cutting into sections, drying at 60 ℃, crushing, sieving, collecting powder between 60 meshes and 100 meshes, drying, sealing and storing for later use.
3. Acquisition of raw spectra
Before the sample is collected, the ultraviolet-visible near-infrared spectrophotometer at the day is started, the ultraviolet-visible near-infrared spectrophotometer is preheated for 0.5h, and neutral alumina powder is used as a blank control to eliminate spectral noise caused by a detection environment when the sample is detected every time. And (3) dividing 140 parts of fiddlehead samples obtained in the last step into 80 parts of correction set samples, 40 parts of prediction set samples and 20 parts of complete external verification sets, and collecting the ultraviolet-visible-short wave near infrared spectrogram of each fiddlehead sample by using a Hitachi ultraviolet-visible near infrared spectrophotometer (UH 4150). The method comprises the steps of setting the measurement range of the Hitachi ultraviolet visible near-infrared spectrophotometer to be 200-1100 nm, setting the scanning times of the Hitachi ultraviolet visible near-infrared spectrophotometer to be 32 times, setting the resolution to be 4.0nm, and repeatedly collecting the same sample for 6 times to obtain original spectral data, wherein the original spectral data are shown in figure 2.
4. Determination of total polysaccharide content in bracken sample
The content of total polysaccharide in the bracken is determined by using anthrone-sulfuric acid ratio method. Accurately weighing 2.0g of fiddlehead dry powder, and mixing the weighed materials according to a material-liquid ratio of 1: 15, adding 30mL of distilled water, carrying out condensation reflux extraction for 2 h/time at 95 ℃, filtering and collecting filtrate, extracting filter residues for 2 times, combining the extracting solutions and placing in a volumetric flask for later use. The content of total polysaccharide in the bracken is determined by adopting an anthrone-sulfuric acid colorimetric method. Measuring absorbance at 620nm wavelength with glucose as standard substance to obtain standard curve equation of glucose (Y is 50.029X-0.0035, R)20.999. (X is a glucose concentration mg/mL, and Y is an absorbance A).
5. Spectral preprocessing
And performing baseline correction and average spectrogram calculation on the original spectrogram of the ultraviolet-visible-short wave near infrared spectrum acquired 6 times by the same fiddlehead sample to obtain an average spectrum, and eliminating the spectrogram caused by artificial sampling errors.
8 spectral pretreatment methods were applied: and (3) screening a preprocessing method by combining a constant variable offset elimination method, a maximum-minimum normalization method, a vector normalization method, a multivariate scattering correction method, a first derivative method, a second derivative method, a multivariate scattering correction plus first derivative method, a vector normalization plus first derivative method and a partial least square algorithm.
By comparing R of PLS models2Cross-validating the root mean square error value RMSECV to obtain a higher R value by using a spectral preprocessing method of a first derivative method2The value 0.6618, the minimum RMSECV value was 0.765, and the UV-VIS-SHORT-WAVE NIR spectra of the bracken samples after spectral pretreatment by the first derivative method were obtained, as shown in FIG. 3.
Table 1 shows the results of the spectral pretreatment method
6. Wavelength variable optimization
The modeled wavelength was optimized using the OPUS7.5 software on the basis of the full wavelength data.
By using the optimized wavelengths of 388-566 nm, 744-833 nm and 1011-1100 nm and 3 wave bands, higher R is obtained2The value is 0.743, the minimum RMSECV value is 0.667%.
Table 2 shows the results of the 4 wavelength variable screening methods
7. Prediction of total polysaccharide content in bracken
Predicting the content of total polysaccharide in the bracken sample by adopting a quantitative model according to the ultraviolet-visible-short wave near infrared spectrum characteristic variable of the bracken sample; and establishing a quantitative model between the spectral characteristic variables and the total polysaccharide content of 80 correction set samples by a partial least square method, verifying the total polysaccharide content of 40 prediction set samples by using the quantitative model, and performing complete external inspection by using 20 samples.
The correlation coefficient of the obtained model correction set is 0.9066, the root mean square error is 0.421%, the correlation coefficient of the prediction set is 0.7834, the root mean square error is 0.639%, as shown in fig. 4, in addition, 20 parts of bracken samples are used for complete external inspection, and the error is-1.33% -1.125%. The constructed method can provide a reliable method for the determination and research of the content of the total polysaccharide in the bracken.
Table 3 is a complete external verification comparison analysis table
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for predicting the content of total polysaccharides in fiddlehead based on an ultraviolet-visible-near infrared spectrum is characterized by comprising the following steps: the method comprises the following steps:
(1) collecting an ultraviolet-visible-short wave near-infrared spectrogram of a fiddlehead powder sample for multiple times by using an ultraviolet-visible near-infrared spectrophotometer, wherein the measurement range of the ultraviolet-visible near-infrared spectrophotometer is 200-1100 nm;
(2) preprocessing spectral data: preprocessing the spectral data by adopting a first derivative method;
(3) screening wavelength variables: screening three wave bands of 388-566 nm, 744-833 nm and 1011-1100 nm to establish effective wavelengths of the PLS model;
(4) predicting the content of the total polysaccharide of the bracken: and (4) combining the wavelength variable in the step (3) with the total polysaccharide content of the bracken sample, establishing a quantitative model of the wavelength variable and the total polysaccharide content of the bracken sample by a partial least square method, and predicting the total polysaccharide content of the bracken according to the quantitative model.
2. The method for predicting the total polysaccharide content in fiddlehead based on uv-vis-nir spectroscopy of claim 1, wherein: the preparation method of the bracken powder sample comprises the following steps: picking fresh bracken samples, cleaning, removing impurities, cutting into sections, drying at 60 ℃, and collecting powder of 60-100 meshes.
3. The method for predicting the total polysaccharide content in fiddlehead based on uv-vis-nir spectroscopy of claim 1, wherein: the bracken powder samples were stored under closed dry conditions.
4. The method for predicting the total polysaccharide content in fiddlehead based on uv-vis-nir spectroscopy of claim 1, wherein: the bracken samples were collected from different production locations, at different times.
5. The method for predicting the total polysaccharide content in fiddlehead based on uv-vis-nir spectroscopy of claim 1, wherein: the total polysaccharide content of the bracken powder sample ranges from 2.30% to 7.592%.
6. The method for predicting the total polysaccharide content in fiddlehead based on uv-vis-nir spectroscopy of claim 1, wherein: the spectrum acquisition in the step (1) comprises the following steps:
(a) dividing the bracken powder sample into a correction set sample, a prediction set sample and a complete external verification sample according to the proportion of 4:2: 1;
(b) the method comprises the steps of placing a fiddlehead powder sample in a quartz single-reflection accessory sample pool equipped with an ultraviolet-visible-near infrared spectrometer, setting the measurement range of a Hitachi ultraviolet-visible near infrared spectrophotometer to be 200-1100 nm, setting the scanning frequency of the Hitachi ultraviolet-visible near infrared spectrophotometer to be 32 times, setting the resolution to be 4.0nm, and repeatedly collecting the same sample for 6 times to obtain original spectral data.
7. The method of claim 6 for predicting total polysaccharide content in bracken based on UV-visible-near infrared spectroscopy, wherein: and (3) verifying the total polysaccharide content of the prediction set sample by using the established quantitative model, and performing external verification by using a complete external verification sample.
8. The method for predicting the total polysaccharide content in fiddlehead based on uv-vis-nir spectroscopy of claim 1, wherein: the spectrum pretreatment in the step (2) comprises the following steps: performing baseline correction and average spectrogram calculation on an ultraviolet-visible-short wave near-infrared spectrogram collected by the same fiddlehead powder sample to obtain an average spectrogram, eliminating the spectrogram caused by manual sampling errors, eliminating spectral noise caused by a detection environment by an average spectrum moving average 15-point smoothing method, and finally processing spectral data by a first derivative method.
9. The method for predicting the total polysaccharide content in fiddlehead based on uv-vis-nir spectroscopy of claim 1, wherein: the method for detecting the total polysaccharide content of the bracken sample in the step (4) comprises the following steps:
(a) weighing a bracken powder sample, and mixing the raw materials according to a material-liquid ratio of 1: 15, adding distilled water, carrying out condensation reflux extraction at 95 ℃, filtering and collecting filtrate, extracting filter residues, combining the extracting solutions and placing the combined extracting solutions in a volumetric flask for later use;
(b) determining total polysaccharide content in herba Fimbristylis Dichotomae by anthrone-sulfuric acid colorimetric method, determining absorbance at 620nm wavelength with glucose as standard substance to obtain standard curve equation of glucose Y (50.029X-0.0035), R20.999, wherein X is glucose concentration mg/mL and Y is absorbance A.
10. The method for predicting the content of total polysaccharides in bracken based on UV-visible-near infrared spectrum according to claim 1, wherein: the ultraviolet visible near-infrared spectrophotometer is a Hitachi ultraviolet visible near-infrared spectrophotometer UH 4150.
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