• Korean Journal of Food Science and Technology
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• v.36 no.5
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• pp.701-710
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• 2004

Uncertainty was quantified to evaluate calcium determination result in infant formula with AAS (Atomic Absorption Spectrometry) and ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry). Uncertainty sources in measurand, such as sample weight, final volume of sample, sample dilution and the instrumental result were identified and used as parameters for combined standard uncertainty based on the GUM (Guide to the expression of uncertainty in measurement) and Draft EURACHEM/CITAC Guide. Uncertainty components of each sources in measurand were identified as resolution, reproducibility and stability of chemical balance, standard material purity, standard material molecular weight, standard solution concentration, standard solution dilution factor, sample dilution factor, calibration curve, recovery, instrumental precision, reproducibility, and stability, Each uncertainty components were evaluated by uncertainty types and included to calculate combined uncertainty. The kinds of uncertainty sources and components in the analytical method by AAS and ICP-AES were same except sample dilution factor for AAS. The analytical results and combined standard uncertainties of calcium content were estimated within the certification range $(367{\pm}20\;mg/100g)$ of CRM (Certified Reference Material) and were not significantly different between method by AAS followed by ashing and method by ICP-AES followed by acid digestion as $359.52{\pm}23.61\;mg/100g\;and\;354.75{\pm}16.16\;mg/100g$, respectively. Identifying uncertainty sources related with precision, repeatability, stability, and maintaining proper instrumental conditions as well as personal proficiency was needed to reduce analytical error.

• Journal of the Korea Institute of Information and Communication Engineering
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• v.10 no.7
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• pp.1319-1325
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• 2006

Urine analysis is basic test in clinical medicine using visual examination by expert nurse. Recently, this test is measured by automatic urine analysis system. But, this system has different results by each instrument. So, a new classification algorithm is required for accurate classify and urine color collection. In this paper, a intelligent color classifier of urine analysis system was designed using neural network algorithm. The input parameters are three stimulus(RGB) after preprocessing using normalization. The fuzzy inference and neural network ware constructed for classify class according to 9 urine test items and $3{\sim}7$ classes. The experiment material to be used a standard sample of medicine. The possibility to adapt classifier designed for urine analysis system was verified as classifying measured standard samples and observing classified result. Of many test items, experimental results showed a satisfactory agreement with test results of reference system.

• Food Science of Animal Resources
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• v.35 no.4
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• pp.466-472
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• 2015

A rapid and simple analytical method, using liquid chromatography tandem mass spectrometry (LC-MS/MS), was developed to detect myo-inositol (MI) in infant formulas. For protein removal: acid hydrolysis and lipid removal through organic solvent extraction. The operating conditions for instrumental analysis were determined based on previously reported analogous methods that used LC-MS/MS. Quantitative analysis was used for the detection limit test, infant formula recovery test, and standard reference material (SRM) 1849a to verify the validity of our LC-MS/MS analytical method, which was developed to quantify MI. For validation, the results of our method were compared with the results of quantitative analyses of certified values. The test results showed that the limit of detection was 0.05 mg/L, the limit of quantitation was 0.17 mg/L, and the method detection limit was 17 mg/kg. The recovery test exhibited a recovery between 98.07-98.43% and a relative standard deviation between 1.93-2.74%. Therefore, the result values were good. Additionally, SRM 1849a was measured to have an MI content of 401.84 mg/kg and recovery of 98.25%, which is comparable to the median certified value of 409 mg/kg. From the aforementioned results, we judged that the instrumental analysis conditions and preparation method used in this study were valid. The rapid analytical method developed herein could be implemented in many laboratories that seek to save time and labor.

• Journal of Environmental Science International
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• v.14 no.12
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• pp.1129-1139
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• 2005

A series of experiments was conducted to identify the potential of five phytoplankton species as standard test species for marine ecotoxicological tests. The candidate phytoplankton species are Skeletonema costatum, Heterosigma akashiwo, Prorocentrum micans, Isochrysis galbana, and Tetraselmis suecica. Salinity tolerance and sensitivity on potassium dichromate as a reference material were identified. Toxicity of eleven ocean dumped sewage sludges and four red tide expellent extracts were estimated by the inhibition of population growth rates (PGR) of marine diatom S. costatum, While most species revealed relatively weak tolerance on salinity, T. suecica demonstrated the highest salinity tolerance ranged from $5\~35$ psu and the others $15\~35$ psu. H. akashiwo revealed the highest sensitivity as 72h $IC_{50}$=0.76mg/L and T. suecica the lowest as 72h $IC_{50}$=8.89mg/L on potassium dichromate. Sludge extracts from industrial waste, domestic sewage and livestock farm waste sludge showed high toxicity as 72h $IC_{50}$<$2\%$ and lowest toxicity from filtration bed sludge as 72h $IC_{50}$=$30.50\%$ NOEC (No Observed Effective Concentration) of sludge extract ranged from <$0.4\%$ to $1.6\%$ and this indicated high phytotoxicity of ocean dumped sewage sludge. The test sensitivity of phytoplankton PGR inhibition was much higher than those of marine rotifer Brachionus plicatilis mortality test and bioluminescent inhibition test by marine bacteria Vibrio fischeri, and comparable with the sea urchin (Strongylocentrotus intermedius) fertilization test. As a result the phytotoxicity test using phytoplankton PGR inhibition ($IC_{50}$) must be a useful tool for marine phyto-toxicological evaluation of ocean dumped materials.

• Environmental Analysis Health and Toxicology
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• v.29
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• pp.18.1-18.9
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• 2014

Objectives The purpose of this study was to determine a separation method for each arsenic metabolite in urine by using a high performance liquid chromatography (HPLC)-inductively coupled plasma-mass spectrometer (ICP-MS). Methods Separation of the arsenic metabolites was conducted in urine by using a polymeric anion-exchange (Hamilton PRP X-100, $4.6mm{\times}150mm$, $5{\mu}m$) column on Agilent Technologies 1260 Infinity LC system coupled to Agilent Technologies 7700 series ICP/MS equipment using argon as the plasma gas. Results All five important arsenic metabolites in urine were separated within 16 minutes in the order of arsenobetaine, arsenite, dimethylarsinate, monomethylarsonate and arsenate with detection limits ranging from 0.15 to $0.27{\mu}g/L$ ($40{\mu}L$ injection). We used G-EQUAS No. 52, the German external quality assessment scheme and standard reference material 2669, National Institute of Standard and Technology, to validate our analyses. Conclusions The method for separation of arsenic metabolites in urine was established by using HPLC-ICP-MS. This method contributes to the evaluation of arsenic exposure, health effect assessment and other bio-monitoring studies for arsenic exposure in South Korea.

• Asian Journal of Atmospheric Environment
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• v.11 no.4
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• pp.283-299
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• 2017

An analytical method using high-performance liquid chromatography (HPLC) with fluorescence (FL) detection was developed for simultaneously analyzing 10 polycyclic aromatic hydrocarbons (PAHs) and 18 nitro-derivatives of PAHs (NPAHs). The two-dimensional HPLC system consists of an on-line clean-up and reduction for NPAHs in the 1st dimension, and separation of the PAHs and the reduced NPAHs and their FL detection in the 2nd dimension after column-switching. To identify an ideal clean-up column for removing sample matrix that may interfere with detection of the analytes, the characteristics of 8 reversed-phase columns were evaluated. The nitrophenylethyl (NPE)-bonded silica column was selected because of its shorter elution band and larger retention factors of the analytes due to strong dipole-dipole interactions. The amino-substituted PAHs (reduced NPAHs), PAHs and deuterated internal standards were separated on polymeric octadecyl-bonded silica (ODS) columns and by dual-channel detection within 120 min including clean-up and reduction steps. The limits of detection were 0.1-9.2 pg per injection for PAHs and 0.1-140 pg per injection for NPAHs. For validation, the method was applied to analyze crude extracts of fine particulate matter ($PM_{2.5}$) samples and achieved good analytical precision and accuracy. Moreover, the standard reference material (SRM1649b, urban dust) was analyzed by this method and the observed concentrations of PAHs and NPAHs were similar to those in previous reports. Thus, the method developed here-in has the potential to become a standard HPLC-based method, especially for NPAHs.

• Analytical Science and Technology
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• v.15 no.5
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• pp.433-438
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• 2002

Trace elements in two air filters (V-50, P-50) artificially loaded with urban dust provided from IAEA were determined non-destructively using instrumental neutron activation analysis. Standard reference material (Urban Particulate Matter, SRM 1648) of National Institute of Standard and Technology was used for analytical quality control. About 20 elements in both of loaded filter samples were determined. To evaluate inter-laboratory comparison and proficiency test, analytical data were statistically treated with the results which collected from 49 laboratories, 40 countries participated in this study using neutron activation analysis, particle induced X-ray emission, inductively coupled plasma mass spectroscopy, etc,. From the results of statistical treatment, Z-scores are within ${\pm}2$. Furthermore, accuracy and precision of obtained analytical values are passed according to the criteria of the proficiency test. Consequently, it was proved that analytical quality for air dust samples being performed has been controlled properly.

• Analytical Science and Technology
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• v.23 no.6
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• pp.518-523
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• 2010

In this paper, the study of analysis of uranium isotopes in environmental samples with a kinetic phosphorescence analyzer (KPA) was described. After leaching uranium fraction from soil and glass material with microwave acid digestion technology, uranium isotopes were purified with UTEVA column, and then measured using KPA. Linearity and repeatability tests for measurement of uranium isotopes were carried out in the uranium standard solution with KPA. The reliability for analytical method of uranium with KPA was validated by its application to uranium standard solution, ground water, IAEA and NIST reference samples.

• The Korea Journal of Herbology
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• v.23 no.3
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• pp.27-32
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• 2008

Objectives : In this paper, we describe that $^1H-NMR$ spectroscopy may be superior to the conventional HPLC for the quantitative analysis of hesperidin from Citrus unshiu. Methods : $^1H-NMR$ spectra (400 MHz) were recorded in $DMSO-d_6$ using a Varian UNITY Inova AS 400 FT NMR spectrometer. One hundred milligram of powdered Citrus unshiu was weighed out and mixed with 1 ml of $DMSO-d_6$ with sonication for 30 min (room temperature). The extracts were filtrated through a 0.45 ${\mu}m$ PVDF filter and 0.5 ml of filtrated extract used for quantitative $^1H-NMR$ measurement (added 1 mg of dimethyl terephthalate as internal standard). The quantity of hesperidin was calculated by the ratio of the intensity of the compound to the known amount of internal standard. For HPLC analysis, the half gram of plant material was extracted with 60 ml of MeOH for 2 hours. The extracts were made 100 ml volume and analyzed by a Waters HPLC system using a YMC ODS column. The total flow rate was 1.0 ml/min with a sample volume 10 ${\mu}l$ and UV detection at 280nm. Results : The contents of hesperidin in Citrus unshiu was determined $5.33{\pm}0.06$% in the quantitative $^1H-NMR$ method and $5.15{\pm}0.12%$ in HPLC method. Using the quantitative $^1H-NMR$ the contents of hesperidin can be determined in much shorter time than the conventional HPLC measurements. Conclusions : From those results, the advantages of quantitative $^1H-NMR$ analysis are that can be analyzed to identify and quantify, and no reference compounds required for calibration curve. Besides, it allows rapid and simple quantification for hesperidin with an analysis time for only 10 min without any pre-purification steps.

• Journal of the Korean Chemical Society
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• v.34 no.1
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• pp.63-68
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• 1990

The chemical ingredients such as $SiO_2,\;Al_2O_3,\;MgO,\;Fe_2O_3,\;CaO$ and $TiO_2$in silica minerals were determined by X-ray fluorescence spectrometry using a matrix correction method. The synthesized standards mixed with reagent grade oxides and the sample were diluted by fusing with 16 times $Li_2B_4O_7$. The matrix effects correlated among the ingredients were corrected by the empirical coefficient method based on the Lucas-Tooth and Pyne model. The analytical results showed relatively good agreement between the different sets of coefficients but were improved with increasing the number of standard. The accuracy of this method was also examined with the standard reference material of NIST.