Tridemorph is a systemic morpholine fungicide for crops. The objective of this study was to develop reliable and sensitive analytical method for determination of tridemorph residues in tea samples for ensuring the food safety. Tridemorph residues in samples were extracted with acetonitrile after hydration, partitioned with saline water, and then purified using an aminopropyl ($NH_2$) SPE cartridge. The purified samples were detected and quantified using LC-ESI-MS/MS. The linear detection limits for tridemorph ranged from 0.02 to $1.0mgL^{-1}$ with a correlation coefficient of 0.9999. The method was validated using tea samples spiked with tridemorph at different concentration levels (0.02 and $0.05{\mu}gmL^{-1}$). The average recovery ranged between 75.0 and 84.7% with relative standard deviations less than 10%. The LOD and LOQ were 0.01 and $0.02mgL^{-1}$, respectively. The developed method was applied successfully to the identification of tridemorph in real tea samples obtained from different sources, and tridemorph was not detected in any of the samples. The results show that the developed analytical method is accurate and suitable for tridemorph determination in tea samples.
HA Jai Yi;PARK Jun-Hyo;KIM Myoung Sug;CHUNG Joon-Ki;JEONG Hyun Do
Korean Journal of Fisheries and Aquatic Sciences
/
v.32
no.4
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pp.420-426
/
1999
We examined the immune response in flounder, Paralichthys olivaceus, with immunization of formalin killed Edwardsiella tarda as an antigen. The ELISPOT-assay (enzyme-linked immunospot assay) was optimized technically and applied to count the number of total and specific antibody secreting cells (TASC and SASC) in lymphocytes of different lymphatic organs. Incubation of lymphocytes on 96 well plate for more than 2.5hrs came out enough time in ELISPOT-assay for counting the antibody secreting cells in the anterior kidney and spleen. However, too much of plate-coated antigen or rabbit anti-flounder immunoglobulin for SASC or TASC counting, respectively, was appeared to decrease the sensitivity of the assay system. Specificity of the system was also confirmed by the absence of TASC in lymphocytes treated with cycloheximide to prevent protein synthesis. The peak numbers of SASC appeared at wk 3 post immunization after that there was a sharp decrease and reached to almost zero at wk 7. In the spleen and kidney, the timing and numbers of SASC on peak response were concurrent without preferential organ distribution. The specific antibody level in the sera increased rapidly between wk 2 and 3 after immunization, i.e. like the specific cellular response found with ELISPOT-assay on that period, However, the remained high level of specific serum antibody from wk 5 after immunization until the end of experiment was clearly distinguishable from the kinetics of SASC response decreased sharply.
A study was carried out on the elelctrochemical characteristics of chemically modified electrodes (CMEs) by cyclic voltammetry. Fabrication of CMEs was made by coating with mixed valence (mv) inorganic-metal polymeric films on the glassy carbon electrode surface by potential cycling. Anodic oxidation behavior of methanol and L-ascorbic acid was studied by using CMEs working electrode. Deposition of films such as mv ruthenium oxo/ruthenium cyanide film (mv Ru-O/CN-Ru), mv ruthenium oxo/ferrocyanide film (mv Ru-O/$Fe(CN)_6$), and mv ruthenium oxo/ruthenium cyanide/Rhodium film (mv Ru-O/CN-Ru/Rh) was obtained to coat by scan rate of 50 mV/sec within the specified potential range (-0.5V ~ +1.2V). Film thickness was controlled by the repeat of the potential cycling. Anodic oxidation behavior of methanol was as follow. Calibration graph by using mv Ru-O/CN-Ru film showed linearly from 10 mM to 80 mM MeOH with slope factor of $-7.552{\mu}A/cm^2$. Although slope factor by using mv Ru-O/$Fe(CN)_6$ film was $-5.13{\mu}A/cm^2$, yet linear range of calibration graph could be extended from 10 mM to 100 mM MeOH. Anodic oxidation behavior of L-ascorbic acid was studied by mv Ru-O/CN-Ru film on the glassy carbon electrode and the glassy carbon electrode with Rh film, Glassy carbon electrode modified with Ru polymeric film was showed better sensitivity than the Rh-glassy carbon modified electrode (mv Ru-O/CN-Ru/Rh). Calibration graph was linear from 0.1 mM to 5 mM L-ascorbic acid by using glassy carbon electrode modified with Ru polymeric film. Solpe factor and relative coefficient are $-84.78{\mu}A/mM$ and 0.998, respectively.
Six commerical rice varieties were cultivated and harvested at different locations in 1987 and 1988 to clarify the degree of locational variations. of several characteristics related to rice grain quality using the rice samples harvested from 8 to 20 locations for a variety each year. Locational variations of percent brown rice, percent milled rice, 1000-grain weight and amylose content were small, but whole grain rate, alkali digestibility, gel consistency, percent white-center and white-belly grain, degree of chalkiness and degree of translucency showed larger variations between locations. The degree of locational variation of sensory evaluation score for eating quality of cooked rice were varied from small to large along with rice variety used and year cultivated. Texture palatability index and stickiness of cooked rice among rheogram characteristics showed larger locational variations, but cohesiveness and springiness showed smaller variations between locations. Set back, break down and maximum viscosity showed larger locational variations among amylogram characteristics of rice flour. Special attention was given to a cultivated location, Anseong, because rice samples harvested at Anseong showed lower percent white-center and white-belly grain, and low set back and high break down in Chucheongbyeo, lower percent white-center and white-belly grain, higher texture palatability index and viscousness/hardness ratio, and low set back and high break down in Dongjinbyeo, higher texture palatability index, and low set back and high break down in Yongmunbyeo, lower percent white-center and white-belly grain in Sangpungbyeo, and low set back and high break down in Samkangbyeo. No other locations in this study produced rice samples showing wide acceptable quality-related characteristics except Anseong.
Kim, Hee-Yun;Jang, Young-Mi;Joo, Hyun-Jin;Jung, Young-Hyun;Lee, Myoung-Sook;Park, Jong-Seok;Lee, Kwang-Ho;Lee, Hwa-Mi
Korean Journal of Food Science and Technology
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v.39
no.4
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pp.372-379
/
2007
A high-performance liquid chromatography-electrospray ionization (HPLC-ESI) tandem MS was developed for the rapid and simultaneous determination of forbidden medicines in dietary supplements. Thirteen medicinal components such as PDE-5 inhibitors and their analogues, and the newly identified dimethylsildenafil and xanthoanthrafil, were included in this study. After tentative standardization of molecular ions in both polarities using thirteen references on the mass spectrometer, with ESI-continuous infusion via the syringe pump method, the relative intensity of the ions present in the resulting spectra was quantitatively compared. From the results, the ion mode was selected depending on each reference's characteristics. A HPLC method coupled with the ESI mode was developed considering the matrix effect and interference depending on the type of sample. The validation test of the developed method was followed by carrying out precision, accuracy, recovery, sensitivity and linearity, etc. The method showed sufficiently high sensitivity, reproducibility, and specificity, and produced 4 times faster results when compared with the existing HPLC/UV method for the determination of forbidden compounds in dietary supplements.
Liquid ionization chamber is filled with liquid equivalent material unlike air filled ionization chamber. The high density material allow very small-volume chamber to be constructed that still have a sufficiently high sensitivity. However liquid ionization chamber should be considered for both initial recombination and general recombination. We, therefore, studied using the Co-60 beam as the continuous beam and the microLion chamber (PTW) for comparing the ion collection efficiency by Greening theory, two-dose rate method and our experiment method. The measurements were carried out using Theratron 780 as the cobalt machine and water phantom and 0.6 cc Farmer type ionization chamber was used with microLion chamber in same condition for measuring the charge of microLion chamber according to the dose rates. Dose rate was in 0.125~0.746 Gy/min and voltages applied to the microLion chamber were +400, +600 and +800 V. As the result, the collection efficiency by three method was generally less than 1%. In particular, our experimental collection efficiency was in good agreement within 0.3% with Greening theory except the lowest two dose rates. The collection efficiency by two-dose rate method also agreed with Greening theory generally less than 1%, but the difference was about 4% when the difference of two dose rates were lower. The ion recombination correction factors by Greening theory, two-dose rate method and our experiment were 1.0233, 1.0239 and 1.0316, respectively, in SSD 80 cm, depth 5 cm recommended by TRS-398 protocol. Therefore we confirmed that the loss by ion recombination was about 3% in this condition. We think that our experiment method for ion recombination correction will be useful tool for radiation dosimetry in continuous beam.
A study for the assessment of natural environmental radiation exposure at a flat and open field of about $10,000m^2$ in area in CNU Daeduk campus has been carried out by means of gamma-ray scintillation spectrometry and thermoluminescence dosimetry for one year period of time from October 1984. The detectors used were 3'${\phi}{\times}$3' NaI(T1) and two different types of LiF TLD, namely, chip sealed in plastic sheet which tightly pressed on two open holes of a metal plate and Teflon disk. Three 24-hour cycles of in-situ spectrometry, and two 3-month and one 1-month cycles of field TL dosimetry were performed. All the spectra measured were converted into exposure rate by means of G(E) opertaion, and therefrom exposure rate due to terrestrial component of environmental radiation was figured out. Exposure rate determined by the spectrometry was, on average, $(10.54{\pm}2.96){\mu}R/hr$, and the rates of $(12.0{\pm}3.4){\mu}R/hr$ and $(11.0{\pm}3.6){\mu}R/hr$ were obtained from chip and disk TLD, respectively. Fluctuations in diurnal variation of the exposure rate measured by the spectrometry were noticeable sometime even in a single cycle of 24 hours. It is concluded that appropriately combined use of TLD with iu-sitn gamma-ray spectrometry system can give more accurate and precise measure of environmental radiation exposure, and further study for more adequate and sensitive TLD for environmental dosimetry, including improvement and elevation of accuracy in data assessment through inter-laboratory or international intercomparison is necessary.
This study was carried out to evaluate the performance of sampling and analytical methodology used for the measurement of toxic volatile organic compounds (VOCs) in the ambient air. VOCs were determined by the adsorbent tube sampling and automatic thermal desorption coupled with GC/MSD analysis. Target analytes were 33 compounds including major aromatic compounds such as BTEX, and halogenated compounds. The methodology was investigated with a wide range of different adsorbents which are commercially available and have been frequently adopted for the VOC measurement. A total of 10 adsorbents were tested in this study: 6 carbon-based adsorbents such as Carbotrap, Carbopack B, Carbosieve S-III, Carboxen 1000, Carbotrap C, Activated Charcoal; and 4 polymer-based adsorbents including Tenax, Porapak Q, Chromosorb 102, and Chromosorb 106. The sampling performance was evaluated with respect to the sampling capacity of VOCs with single-adsorbent and multiple-adsorbents methods for standard samples and field samples. As a result, the best adsorbents for single-adsorbent method in the sampling of toxic organic compounds (including benzene, toluene, xylenes etc.) appeared to be Carbotrap, Carbopack B and Tenax TA. On the other hand, Chromosorb 102, Chromosorb 106 and Porapak Q were found to be unsuitable adsorbents for VOC measurement based on thermal desorption method. Multi-adsorbent packings were evaluated with 4 carbon-based adsorbents, which classified by 3 combination sets of double adsorbents and 2 combination sets of triple adsorbents. The results indicated that the most suitable combination for toixc VOC measurements is Carbotrap C with Carbotrap. Multi-sorbents tubes packed with a strong adsorbent such as Carbosieve S-III or Carboxen 1000 were found to be relatively unsuitable for several compounds, not only owing to the effect of migration of adsorbed compounds from weaker adsorbent to stronger adsorbent, but to hydrophobic nature of the adsorbents. Therefore, it should be addressed that selection of a proper adsorbent (or combination of multi sorbents) is extremely important to obtain reliable data for the concentrations of toxic VOCs in indoor and outdoor environments.
Purpose : Because of the rapid physical decay of the short half-lived radionuclide, counting of event for image is very limited. In this reason, long scan duration is applied for more accurate quantitative analysis in the relatively low sensitive examination. The aim of this study was to evaluate the difference according to scan duration and investigate the resonable scan duration using the radionuclide of 11C and 18F in PET scan. Materials and Methods : 1994-NEMA Phantom was filled with 11C of $30.08{\pm}4.22MBq$ and 18F of $40.08{\pm}8.29MBq$ diluted with distilled water. Dynamic images were acquired 20frames/1minute and static image was acquired for 20minutes with 11C. And dynamic images were acquired 20frames/2.5minutes and static image was acquired for 50minutes with 18F. All of data were applied with same reconstruction method and time decay correction. Region of interest (ROI) was set on the image, maximum radioactivity concentration (maxRC, kBq/mL) was compared. We compared maxRC with acquired dynamic image which was summed one bye one to increase the total scan duration. Results : maxRC over time of 11C was $3.85{\pm}0.45{\sim}5.15{\pm}0.50kBq/mL$ in dynamic image, and static image was $2.15{\pm}0.26kBq/mL$. In case of 18F, the maxRC was $9.09{\pm}0.42{\sim}9.48{\pm}0.31kBq/mL$ in dynamic image and $7.24{\pm}0.14kBq/mL$ in static. In summed image of 11C, as total scan duration was increased to 5, 10, 15, 20minutes, the maxRC were $2.47{\pm}0.4$, $2.22{\pm}0.37$, $2.08{\pm}0.42$, $1.95{\pm}0.55kBq/mL$ respectively. In case of 18F, the total scan duration was increased to 12.5, 25, 37.5, and 50minutes, the maxRC were $7.89{\pm}0.27$, $7.61{\pm}0.23$, $7.36{\pm}0.21$, $7.31{\pm}0.23kBq/mL$. Conclusion : As elapsed time was increased after completion of injection, the maxRC was increased by 33% and 4% in dynamic study of 11C and 18F respectively. Also the total scan duration was increased, the maxRC was reduced by 50% and 20% in summed image of 11C and 18F respectively. The percentage difference of each result is more larger in study using relatively shorter half-lived radionuclide. It appears that the accuracy of decay correction declined not only increment of scan duration but also increment of elapsed time from a starting point of acquisition. In study using 18F, there was no big difference so it's not necessary to consider error of quantitative evaluation according to elapsed time. It's recommended to apply additional decay correction method considering decay correction the error concerning elapsed time or to set the scan duration of static image less than 5minutes corresponding 25% of half life in study using shorter half-lived radionuclide as 11C.
The endeavors enhancing the grain quality of high-yielding japonica rice were steadily continued during 1980s-1990s along with the self-sufficiency of rice production and the increasing demands of high-quality rices. During this time, considerably great progress and success was obtained in development of high-quality japonica cultivars and quality evaluation techniques including the elucidation of interrelationship between the physicochemical properties of rice grain and the physical or palatability components of cooked rice. In 1990s, some high-quality japonica rice cultivars and special rices adaptable for food processing such as large kernel, chalky endosperm, aromatic and colored rices were developed and its objective preference and utility was also examined by a palatability meter, rapid-visco analyzer and texture analyzer, Recently, new special rices such as extremely low-amylose dull or opaque non-glutinous endosperm mutants were developed. Also, a high-lysine rice variety was developed for higher nutritional utility. The water uptake rate and the maximum water absorption ratio showed significantly negative correlations with the K/Mg ratio and alkali digestion value(ADV) of milled rice. The rice materials showing the higher amount of hot water absorption exhibited the larger volume expansion of cooked rice. The harder rices with lower moisture content revealed the higher rate of water uptake at twenty minutes after soaking and the higher ratio of maximum water uptake under the room temperature condition. These water uptake characteristics were not associated with the protein and amylose contents of milled rice and the palatability of cooked rice. The water/rice ratio (in w/w basis) for optimum cooking was averaged to 1.52 in dry milled rices (12% wet basis) with varietal range from 1.45 to 1.61 and the expansion ratio of milled rice after proper boiling was average to 2.63(in v/v basis). The major physicochemical components of rice grain associated with the palatability of cooked rice were examined using japonica rice materials showing narrow varietal variation in grain size and shape, alkali digestibility, gel consistency, amylose and protein contents, but considerable difference in appearance and texture of cooked rice. The glossiness or gross palatability score of cooked rice were closely associated with the peak, hot paste and consistency viscosities of viscosities with year difference. The high-quality rice variety "IIpumbyeo" showed less portion of amylose on the outer layer of milled rice grain and less and slower change in iodine blue value of extracted paste during twenty minutes of boiling. This highly palatable rice also exhibited very fine net structure in outer layer and fine-spongy and well-swollen shape of gelatinized starch granules in inner layer and core of cooked rice kernel compared with the poor palatable rice through image of scanning electronic microscope. Gross sensory score of cooked rice could be estimated by multiple linear regression formula, deduced from relationship between rice quality components mentioned above and eating quality of cooked rice, with high probability of determination. The $\alpha$-amylose-iodine method was adopted for checking the varietal difference in retrogradation of cooked rice. The rice cultivars revealing the relatively slow retrogradation in aged cooked rice were IIpumbyeo, Chucheongyeo, Sasanishiki, Jinbubyeo and Koshihikari. A Tonsil-type rice, Taebaegbyeo, and a japonica cultivar, Seomjinbyeo, showed the relatively fast deterioration of cooked rice. Generally, the better rice cultivars in eating quality of cooked rice showed less retrogradation and much sponginess in cooled cooked rice. Also, the rice varieties exhibiting less retrogradation in cooled cooked rice revealed higher hot viscosity and lower cool viscosity of rice flour in amylogram. The sponginess of cooled cooked rice was closely associated with magnesium content and volume expansion of cooked rice. The hardness-changed ratio of cooked rice by cooling was negatively correlated with solids amount extracted during boiling and volume expansion of cooked rice. The major physicochemical properties of rice grain closely related to the palatability of cooked rice may be directly or indirectly associated with the retrogradation characteristics of cooked rice. The softer gel consistency and lower amylose content in milled rice revealed the higher ratio of popped rice and larger bulk density of popping. The stronger hardness of rice grain showed relatively higher ratio of popping and the more chalky or less translucent rice exhibited the lower ratio of intact popped brown rice. The potassium and magnesium contents of milled rice were negatively associated with gross score of noodle making mixed with wheat flour in half and the better rice for noodle making revealed relatively less amount of solid extraction during boiling. The more volume expansion of batters for making brown rice bread resulted the better loaf formation and more springiness in rice breed. The higher protein rices produced relatively the more moist white rice bread. The springiness of rice bread was also significantly correlated with high amylose content and hard gel consistency. The completely chalky and large grain rices showed better suitability far fermentation and brewing. The glutinous rice were classified into nine different varietal groups based on various physicochemical and structural characteristics of endosperm. There was some close associations among these grain properties and large varietal difference in suitability to various traditional food processing. Our breeding efforts on improvement of rice quality for high palatability and processing utility or value-adding products in the future should focus on not only continuous enhancement of marketing and eating qualities but also the diversification in morphological, physicochemical and nutritional characteristics of rice grain suitable for processing various value-added rice foods.ice foods.
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