• Near Infrared Analysis
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• 제1권2호
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• pp.29-33
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• 2000

The identification step of raw drug materials is an indispensible procedure in the GMP manufacturing process within the pharmaceutical industry. However, wet chemistry methods for identification of drug materials, used by the various Pharmacopeia are time-consuming and expensive steps. In this paper, near-infrared spectroscopy (NIRS) has been developed for identifying eleven drug substances including calcium pantothenate, cefaclor, cefoperazone, cephradine, dextromethorphan, ehtambutol, nicotinamide, pyrozinamide, tramadol, vitamin C, and vitamin E. Also the aim of ths work is to consturct a new algorithm for calibration model using soft independence modeling of class analogy (SIMCA) with Malinowskis Indicator Function (IND), which is used for finding the number of principal components of each class of the SIMACA model. The use of NIR technique with pattern recognition to qualify raw materials can make it possible to monitor process in real time as well as to control all procedures in the pharmaceutical industry. As the result, the samples identified of 183 different batches from 11 different compounds were separated clearly by SIMCA with 2nd derivative spectra in the NIR region of 1100∼2400 nm.

• 한국근적외분광분석학회:학술대회논문집
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• 한국근적외분광분석학회 2001년도 NIR-2001
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• pp.3105-3105
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• 2001

Ingests and fecal contamination on a poultry carcass is a food safety hazard due to potential microbiological contamination. A visible/near-infrared (NIR) spectrometer was used to discriminate among pure ingesta and fecal material, breast skin contaminated with ingesta or fecal material and uncontaminated breast skin. Birds were fed isocaloric diets formulated with either maize, mile, or wheat and soybean meal for protein requirements. Following completion of the feeding period (14 days), the birds were humanely processed and eviscerated to obtain ingests from the crop or proventriculus and feces from the duodenum, ceca, and colon portion of the digestive tract. Pure feces and ingesta, breast skin, and contaminated breast skin were scanned from 400 to 2500 nm and analyzed from 400 to 900 nm. Principal component analysis (PCA) of reflectance spectra was used to discriminate between contaminates and uncontaminated breast skin. Results indicate that visible (400 to 760 nm) and NIR 760-900 nm spectra can detect contaminates. From PCA analysis, key wavelengths were identified for discrimination of uncontaminated skin from contaminates based the evaluation of loadings weights.

• 한국근적외분광분석학회:학술대회논문집
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• 한국근적외분광분석학회 2001년도 NIR-2001
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• pp.1021-1021
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• 2001

Sample presentation, which means how to set samples to an NIR instrument, is very important in Near Infrared (NIR) Spectroscopy. When sample presentation is not suitable for the samples that you use, very good spectra can not be obtained even if you use a sophisticated NIR instrument. In my presentation, various NIR sample presentations for agricultural products such as intact fruits, single grains, vegetable juice and the others will be explained. In case of peaches with thin peel, the fiber optics of Interactance can be used. However, the fiber optics are not suitable for oranges with relatively thick peel. In this case, transmittance method is useful. As for a small sample such as single grains, a specially designed cell is needed. The cell in transmittance mode has been developed and then applied to single kernels of rice and soybean. In this case we also used the fiber optics. As regards liquid type of sample, a cuvette cell made of quartz in transmittance mode is popular. However, it is time-consuming to wash and dry it. In order to compensate this disadvantage the sample presentation using normal test tubes as sample cells have been developed and applied to milk, rumen juice and urine of a milking cow. An individual test tube can be used for each sample if you use the calibration equation with sample cell compensation. The test tube cell has also been applied to spinach juice for determination of undesirable constituents. It is concluded that sample presentation is most important for NIR Spectroscopy.

• 한국근적외분광분석학회:학술대회논문집
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• 한국근적외분광분석학회 2001년도 NIR-2001
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• pp.2102-2102
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• 2001

Near infrared, diffuse reflectance spectroscopy has shown significant potential for in vitro and in vivo assessment of metabolic status. However, the complexity of living samples can lead to ambiguous results. This presentation will focus on methods that provide controls for scattering and absorption estimation in tissue. For robust estimations, normalization procedures will be shown which can greatly improve interpretability of results. Normalization based on time, location and spectral property will be shown with data from models, tissue phantoms and in vivo measurements. In particular, interpretation of NIR spectra associated with major respiratory constituents will be examined. Measurement of constituents such as hemoglobin, myoglobin, tissue edema, and lactate will be shown. Results suggest that NIR may provide a valuable tool for physiological monitoring in critical care research and practice.

• 한국근적외분광분석학회:학술대회논문집
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• 한국근적외분광분석학회 2001년도 NIR-2001
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• pp.1529-1529
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• 2001

The watercore in apple is very important factor in storage and sorting of fruit. Most consumers tend to prefer the apple included watercore in immediately after harvest, however the watercore causes fruit flesh to brown during storage and lose the worth after all. But it is practically impossible to judge to the naked eye whether an apple has watercore or not. Therefore, the rapid, accurate and non-destructive analysis method for discrimination of watercore should be settled without delay. In this study we attempted the discrimination and quantitative analysis of watercore in apple fruit using near-infrared transmittance spectroscopy ‘Fuji’ apple fruits produced in Kyungpook of Korea was used in this experiment. The watercore content in apple was evaluated by graphic treatment of culled slice sections(10 mm). NIR transmittance spectra were collected over the 500 to 1000 nm spectral region with a spectrometer (Sentronic Co., Germany). The calibration models were carried out by partial least squares (PLS) analysis between NIR spectra data of apples and chemical data of watercore content. The spectra were different in absorbance between apple included watercore and not included one. Apple included watercore had higher absorption band than sample not included one at 732 and 820 nm. The calibration model seems to be accurate to predict the watercore content in apple fruit, the correlation coefficient (R) and root mean square error of prediction (RMSEP) were 0.99 and 0.93%, respectively. This result indicates that the PLSR calibration model by using NIR transmittance spectroscopy could be used for discrimination of watercore in apple fruit.

• 한국근적외분광분석학회:학술대회논문집
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• 한국근적외분광분석학회 2001년도 NIR-2001
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• pp.1072-1072
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• 2001

The purpose of this research is to evaluate rapid determination of phosphorus in soils using NIR spectroscopy. The soil samples from the fields subject to different crops and land-use in Kyeongbook province, Korea were used to make the calibration and validation of the calibration set estimating phosphorus in soil. The NIR reflectance was scanned at 2nm intervals from 1100 to 2500nm with an InfraAlyzer 500 (Bran+Luebbe Co.). Various regression analyses were used to evaluate a NIRS method for determination of phosphorus in the soil. NIR absorption approach requires many soil samples to obtain optimal prediction. Applicability of NIR spectra technique may allow for the analysis of available soil phosphorus rapidly as well as total component within a few seconds.

• 한국근적외분광분석학회:학술대회논문집
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• 한국근적외분광분석학회 2001년도 NIR-2001
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• pp.1171-1171
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• 2001

Quantitative analysis is an important requirement in exploration, mining and processing of minerals. There is an increasing need for the use of quantitative mineralogical data to assist with bore hole logging, deposit delineation, grade control, feed to processing plants and monitoring of solid process residues. Quantitative analysis using X-Ray Powder Diffraction (XRD) requires fine grinding and the addition of a reference material, or the application of Rietveld analysis to XRD patterns to provide accurate analysis of the suite of minerals present. Whilst accurate quantitative data can be obtained in this manner, the method is time consuming and limited to the laboratory. Mid infrared when combined with multivariant analysis has also been used for quantitative analysis. However, factors such as the absorption coefficients and refractive index of the minerals requires special sample preparation and dilution in a dispersive medium, such as KBr to minimize distortion of spectral features. In contrast, the lower intensity of the overtones and combinations of the fundamental vibrations in the near infrared allow direct measurement of virtually any solid without special sample preparation or dilution. Thus Near Infrared Spectroscopy (NIR) has found application for quantitative on-line/in line analysis and control in a range of processing applications which include, moisture control in clay and textile processing, fermentation processes, wheat analysis, gasoline analysis and chemicals and polymers. It is developing rapidly in the mineral exploration industry and has been underpinned by the development of portable NIR spectrometers and spectral libraries of a wide range of minerals. For example, iron ores have been identified and characterized in terms of the individual mineral components using field spectrometers. Data acquisition time of NIR field instruments is of the order of seconds and sample preparation is minimal. Consequently these types of spectrometers have great potential for in-line or on-line application in the minerals industry. To demonstrate the applicability of NIR field spectroscopy for quantitative analysis of minerals, a specific example on the quantification of lateritic bauxites will be presented. It has been shown that the application of Partial Least Squares regression analysis (PLS) to the NIR spectra can be used to quantify chemistry and mineralogy in a range of lateritic bauxites. Important, issues such as sampling, precision, repeatability, and replication which influence the results will be discussed.

• Bulletin of the Korean Chemical Society
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• 제25권5호
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• pp.647-651
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• 2004

Partial Least Squares (PLS) calibration performance has been systematically investigated by changing spectral resolutions of near-infrared (NIR) spectra. For this purpose, synthetic samples simulating naphtha were prepared to examine the calibration performance in complex chemical matrix. These samples were composed of $C_6-C_9$ normal paraffin, iso-paraffin, naphthene, and aromatic hydrocarbons. NIR spectra with four different resolutions of 4, 8, 16, and 32$cm^{-1}$ were collected and then PLS regression was performed. For PLS calibration, five different group compositions (such as total paraffin content) and six different pure components (such as benzene concentration) were selected. The overall results showed that at least 8$cm^{-1}$ resolution was required to resolve the complex chemical matrix such as naphtha. It was found that the influence of resolution on the PLS calibration was varied by the spectral features of a component.

• 한국근적외분광분석학회:학술대회논문집
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• 한국근적외분광분석학회 2001년도 NIR-2001
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• pp.1614-1614
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• 2001

The sweetness (。Bix) of fruit is the main quality factor contributing to the fruit taste. The brix of the apple fruit can be measured non-destructively by near infrared (NIR) spectroscopy, allowing the sweetness grading of individual apple fruit. However, the fruit quality is influenced by various factors such as growing location, producing year, variety and harvest time etc., accordingly the robust NIR calibration is required. In this experimental results are presented the influence of two variations such as growing location and producing year of apple fruit in establishing of calibrations for sweetness, and developed a stable and highly accurate calibration. Apple fruit (Fuji) was collected every year from 1995 to 1997 in 3 different growing locations (Andong, Youngchun and Chungsong) of Kyungpook in Korea. NIR reflectance spectra of apple fruit were scanned in wavelength range of 1100∼2500nm using an InfraAlyzer 500C (Bran+Luebbe) with halogen lamp and PbS detector. The multiple linear regression and stepwise was carried out between the NIR raw spectra and the brix measured by refractometer to select the best regression equations. The calibration models by each growing district were well predicted to dependent sample set, but poorly predicted to independent sample set. Combined calibration model using data of three growing districts predicted reasonable well to a population set drawn from all growing districts(SEP = 0.69%, Bias=-0.075). The calibration models by each harvest year were not transferable across harvest year, however a combined calibration model using data of three harvest years was sufficiently robust to predict each sample sets(SEP = 0.53%, Bias = 0.004).

• 한국근적외분광분석학회:학술대회논문집
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• 한국근적외분광분석학회 2001년도 NIR-2001
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• pp.4112-4112
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• 2001

The feasibility of NIR spectroscopy as a quick and nondestructive method for quality control of uniformity of coating thickness of pharmaceutical tablets was investigated. Near infrared spectra of a set of pharmaceutical tablets with varying coating thickness were measured with a diffuse reflectance fiber optic probe connected to a Broker IFS 28/N FT-NIR spectrometer. The challenging issues encountered in this study included: 1. The similarity of the formulation of the core and coating materials, 2. The lack of sufficient calibration samples and 3. The non-linear relationship between the NIR spectral intensity and coating: thickness. A peak at 7184 $cm^{-1}$ was identified that differed for the coating material and the core material when M spectra were collected at 2 $cm^{-1}$ resolution (0.4 nm at 7184 $cm^{-1}$). The study showed that the coating thickness can be analyzed by polynomial fitting of the peak area of the selected peak, while least squares calibration of the same data failed due to the lack of availability of sufficient calibration samples. Samples of coal powder and solid pieces of coal were analyzed by FT-NIR diffuse reflectance spectroscopy with the goal of predicting their ash content, percentage of volatile components, and energy content. The measurements were performed on a Broker Vector 22N spectrometer with a fiber optic probe. A partial least squares model was constructed for each of the parameters of interest for solid and powdered sample forms separately. Calibration models varied in size from 4 to 10 PLS ranks. Correlation coefficients for these models ranged from 86.6 to 95.0%, with root-mean-square errors of cross validation comparable to the corresponding reference measurement methods. The use of FT-NIR diffuse reflectance measurement techniques was found to be a significant improvement over existing measurement methodologies in terms of speed and ease of use, while maintaining the desired accuracy for all parameters and sample forms.(Figure Omitted).