Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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2001.06a
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pp.4111-4111
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2001
When a drug is prepared in a tablet, the active component represents only a small portion of the dosage form. The other components of the formulation include materials to assist in the dissolution, antioxidants, coloring agents and bulk fillers. The tablets are tested using approved testing methods usually involving separation and subsequent quantification of the active component. Tablets may also be tested by near-Infrared Reflectance spectrometry (NIRS). In the present study, based on NIRS and multivariate calibration methods, a novel and precise method is developed for direct determination of ascorbic acid in vitamin C tablet. Two different tablet formulations were powdered in three different sizes, 63-125 ${\mu}{\textrm}{m}$, and examined. Spectral region of 4750-4950 $cm^{-1}$ / was used and optimized for quantitative operations. Partial least squares (PLS) and multiple linear regression (MLR) methods were performed for this spectral region. The results of optimized PLS and MLR methods showed that reproducibility increase with decreasing grain size and standard error of calibration (SEP) of less than 1% w/w of ascorbic acid and a correlation coefficient of 0.998 can be achieved. The PLS method showed better results than MLR. Seven overdose and underdose samples (prepared in the laboratory to match marketed products) were tested by proposed and iodometric standard methods. A correlation between NIRS predicted ascorbic acid values and iodomet.ic values was calculated ($R^2$=0.9950). Finally, the direct analysis of individual intact tablets in their unit-dose packages (Blistering in aluminum and PVC foils) obtained from market were also carried out and a correlation coefficient of 0.9989 and SEP of 0.931% w/w of ascorbic acid were achieved.
Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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2001.06a
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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).
Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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2001.06a
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pp.1157-1157
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2001
Yeast, Kurtzurnanomyces sp. I-11, produces biosurfactant, mannosyl erythritol lipid (MEL), from soya oil. The properties of biosurfactant MEL include low-toxicity and high biodegradability. MEL provides new possibilities for a wide range of industrial applications, especially food, cosmetic, pharmaceutical fields and chemicals for biotechnology. In the fermentation process, techniques of measuring and controlling substrates and products are important to obtain high productivity with optimum concentrations of substrate and product in the culture broth. The measurement system for the concentrations of soya oil and MEL in the fermentation process was developed using near-infrared spectroscopy (NIRS). Soya oil and MEL in the culture broth were extracted with ethyl acetate and NIR spectra was carried out between the second derivative NIR spectral data at 1312 and 2040 nm and MEL concentrations obtained using a thin-layer chromatography with a flame-ionization detector (TLC/FID) method. A calibration equation for soya oil was results of the validation of the calibration equation, good agreement was observed between the results of the TLD/FID method and those of the NIRS method for both constituents. NIR method was applied to the measurement of the concentrations of MEL and soya oil in the practical fermentation and good results were obtained. The study indicates that NIRS is a useful method for measurement of the substrate and product in the glycolipid fermentation.
Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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2001.06a
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pp.3112-3112
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2001
Near-Infrared Spectroscopy (NIRS) was investigated aiming at the identification of falsified drugs. The identification is based on comparison of the NIR spectrum of a sample with a typical spectra of an authentic drug using multivariate modelling and classification algorithms (PCA/SIMCA). Two spectrophotometers (Brimrose - Luminar 2000 and 2030), based on acoustic-optical filter (AOTF) technology, sharing the same controlling computer, software (Brimrose - Snap 2.03) and the data acquisition electronics, were employed. The Luminar 2000 scans the range 850 1800 nm and was employed for transmitance/absorbance measurements of liquids with a transflectance optical bundle probe with total optical path of 5 mm and a circular area of 0.5 $\textrm{cm}^2$. Model 2030 scans the rage 1100 2400 nm and was employed for reflectance measurement of solids drugs. 300 spectra, acquired in about 20 s, were averaged for each sample. Chemometric treatment of the spectral data, modelling and classification were performed by using the Unscrambler 7.5 software (CAMO Norway). This package provides the Principal Component Analysis (PCA) and SIMCA algorithms, used for modelling and classification, respectively. Initially, NIRS was evaluated for spectrum acquisition of various drugs, selected in order to accomplish the diversity of physico-chemical characteristics found among commercial products. Parameters which could affect the spectra of a given drug (especially if presented as solid tablets) were investigated and the results showed that the first derivative can minimize spectral changes associated with tablet geometry, physical differences in their faces and position in relation to the probe beam. The effect of ambient humidity and temperature were also investigated. The first factor needs to be controlled for model construction because the ambient humidity can cause spectral alterations that should cause the wrong classification of a real drug if the factor is not considered by the model.
Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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2001.06a
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pp.3111-3111
/
2001
The implementation of NIR and chemometrics in the Pharmaceutical industries is still in strong progress, both regarding qualitative and quantitative applications and beneficial results are seen. Looking at the development so far, NIR will change the pharmaceutical industry even more in the future. This presentation will address the experiences and progress achieved regarding the application and implementation of quantitative methods for determination of content uniformity and assay of tablets with less than 10% w/w of active, using Near Infrared transmittance spectroscopy in combination with PLS. Also qualitative methods for identification of the same tablets by Near Infrared reflectance spectroscopy will be discussed. Four commercial tablet strengths are formulated and produced from two different compositions by direct compression. Three different strengths are dose proportional, i.e. fixed concentration by varying in size. The aim was to replace the conventional primary methods for analysing content uniformity, assay and identification by NIR. Studies were performed on comparing transmittance versus reflectance spectroscopy for both applications on the dose proportional tablets. The model for determination of content uniformity and assay was developed to cover both coated and uncoated tablets, whereas the qualitative model was developed to identify coated tablets only. The impact of the tablet formulation, tablet size and coating, resulted in individual models far each composition The best calibration was achieved using diffuse reflectance for the identification purposes and diffuse transmittance for the quantitative determination of the active content within the tablets. As NIR in combination with other techniques opens up the possibility of total quality management within the production, the transfer of the above-mentioned models from a laboratory based approach to an at-line approach at H.Lundbeck will be addressed too.
Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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2001.06a
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pp.1248-1248
/
2001
Mastitis is a major problem for the global dairy industry and causes substantial economic losses from decreasing milk production and considerable compositional changes in milk, reducing milk quality. The potential of near infrared (NIR) spectroscopy in the region from 1100 to 2500nm and chemometric method for classification to detect milk from mastitic cows was investigated. A total of 189 milk samples from 7 Holstein cows were collected for 27 days, consecutively, and analyzed for somatic cells (SCC). Three of the cows were healthy, and the rest had mastitis periods during the experiment. NIR transflectance milk spectra were obtained by the InfraAlyzer 500 spectrophotometer in the spectral range from 1100 to 2500nm. All samples were divided into calibration set and test set. Class variable was assigned for each sample as follow: healthy (class 1) and mastitic (class 2), based on milk SCC content. The classification of the samples was performed using soft independent modeling of class analogy (SIMCA) and different spectral data pretreatment. Two concentration of SCC - 200 000 cells/ml and 300 000 cells/ml, respectively, were used as thresholds fer separation of healthy and mastitis cows. The best detection accuracy was found for models, obtained using 200 000 cells/ml as threshold and smoothed absorbance data - 98.41% from samples in the calibration set and 87.30% from the samples in the independent test set were correctly classified. SIMCA results for classes, based on 300 000 cells/ml threshold, showed a little lower accuracy of classification. The analysis of changes in the loading of first PC factor for group of healthy milk and group of mastitic milk showed, that separation between classes was indirect and based on influence of mastitis on the milk components. The accuracy of mastitis detection by SIMCA method, based on NIR spectra of milk would allow health screening of cows and differentiation between healthy and mastitic milk samples. Having SIMCA models, mastitis detection would be possible by using only DIR spectra of milk, without any other analyses.
Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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2001.06a
/
pp.4104-4104
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2001
Milk somatic cell count (SCC) is a recognized indicator of cow health and milk quality. The potential of near infrared (NIR) spectroscopy in the region from 1100 to 2500nm to measure SCC content of cow milk was investigated. A total of 196 milk samples from 7 Holstein cows were collected for 28 days, consecutively, and analyzed for fat, protein, lactose and SCC. Three of the cows were healthy, and the rest had mastitis periods during the experiment. NIR transflectance milk spectra were obtained by the InfraAlyzer 500 spectrophotometer in a wavelength range from 1100 to 2500 nm. The calibration for logSCC was performed using partial least square (PLS) regression and different spectral data pretreatment. The best accuracy of determination was found for equation, obtained using smoothed absorbance data and 10 PLS factors. The standard error of calibration was 0.361, calibration coefficient of multiple correlation 0.868, standard error of prediction for independent validation set of samples 0.382, correlation coefficient 0.854 and the variation coefficient 7.63%. The accuracy of logSCC determination by NIR spectroscopy would allow health screening of cows, and differentiation between healthy and mastitic milk samples. When the spectral information was studied it has been found that SCC determination by NIR milk spectra was indirect and based on the related changes in milk composition. In the case of mastitis, when the disease occurred, the most significant factors that simultaneously influenced milk spectra were alteration of milk proteins and changes in ionic concentration of milk.
Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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2001.06a
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pp.1528-1528
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2001
Ginseng cultivated in different country or growing condition has generally different components such as saponin and protein, and it relates to efficacy and action. Protein content assumes by nitrogen content in ginseng radix. Nitrogen content could be determined by chemical analysis such as kjeldahl or extraction methods. However, these methods require long analysis time and result environmental pollution and sample damage. In this work we investigated possibility of non-destructive determination of nitrogen content in ginseng radix using near-infrared spectroscopy. Ginseng radix, root of Panax ginseng C. A. Meyer, was studied. Total 120 samples were used in this study and it was consisted of 6 sample sets, 4, 5 and 6-year-old Korea ginseng and 7, 8 and 9-year-old China ginseng, respectively. Each sample set has 20 sample. Nigrogen content was measured by electronic analysis. NIR reflectance spectra were collected over the 1100 to 2500 nm spectral region with a InfraAlyzer 500C (Bran+Luebbe, Germany) equipped with a halogen lapmp and PbS detector and data were collected every 2 nm data point intervals. The calibration models were carried out by multiple linear regression (MLR) and partial least squares (PLS) analysis using IDAS and SESAME software. Result of electronic analysis, Korean ginseng were different mean value in nitrogen content of China ginseng. Ginseng tend to generally decrease the nitrogen content according as cultivation year is over 6 years. The MLR calibration model with 8 wavelengths using IDAS software accurately predicted nitrogen contents with correlation coefficient (R) and standard error of prediction of 0.985 and 0.855%, respectively. In case of SESAME software, the MLR calibration with 9 wavelength was selected the best calibration, R and SEP were 0.972 and 0.596%, respectively. The PLSR calibration model result in 0.969 of R and 0.630 of RMSEP. This study shows the NIR spectroscopy could be applied to determine the nitrogen content in ginseng radix with high accuracy.
Kim, Eun-Ok;Sohn, Mi-Ryeong;Kwon, Young-Kil;Lin, Gou-Lin;Cho, Rae-Kwang
Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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2001.06a
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pp.1529-1529
/
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.
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