• Title/Summary/Keyword: CV performance

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Development and Validation of Analytical Method for Nitroxoline in Chicken Using HPLC-PDA (HPLC-PDA를 이용한 닭고기 중 Nitroxoline 분석법 개발)

  • Cho, Yoon-Jae;Chae, Young-Sik;Kim, Jae-Eun;Kim, Jae-Young;Kang, Ilhyun;Lee, Sang-Mok;Do, Jung-Ah;Oh, Jae-Ho;Chang, Moon-Ik;Hong, Jin-Hwan
    • Korean Journal of Environmental Agriculture
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    • v.32 no.1
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    • pp.70-77
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    • 2013
  • BACKGROUND: Nitroxoline is an antibiotic agent. It is used for the treatment of the second bacterial infection by the colibacillosis, salmonellosis and viral disease of the poultry. When the nitroxoline is indiscreetly used, the problem about the abuse of the antibiotics can occur. Therefore, this study presented the residue analytical method of nitroxoline in food for the safety management of animal farming products. METHODS AND RESULTS: A simple, sensitive and specific method for nitroxoline in chicken muscle by high performance liquid chromatograph with PDA was developed. Sample extraction with acetonitrile, purification with SPE cartridge (MCX) were applied, then quantitation by HPLC with C18 column under the gradient condition with 0.1 % tetrabutylammonium hydroxide-phosphoric acid and methanol was performed. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.999, analysed from 0.02 to 0.5 mg/L concentration. Limit of quantitation in chicken muscle showed 0.02 mg/kg, and average recoveries ranged from 72.9 to 88.1 % in chicken muscle. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 12 % in 0.02 and 0.04 mg/kg. CONCLUSION(S): Newly developed method for nitroxoline in chicken muscle was applicable to food inspection with the acceptable level of sensitivity, repeatability and reproducibility.

Modeling and Validation of Population Dynamics of the American Serpentine Leafminer (Liriomyza trifolii) Using Leaf Surface Temperatures of Greenhouses Cherry Tomatoes (방울토마토에서 잎 표면온도를 적용한 아메리카잎굴파리(Liriomyza trifolii) 개체군 밀도변동 모형작성 및 평가)

  • Park, Jung-Joon;Mo, Hyoung-Ho;Lee, Doo-Hyung;Shin, Key-Il;Cho, Ki-Jong
    • Korean journal of applied entomology
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    • v.51 no.3
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    • pp.235-243
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    • 2012
  • Population dynamics of the American serpentine leafminer, Liriomyza trifolii (Burgess), were observed and modeled in order to compare the effects of air and tomato leaf temperatures inside a greenhouse using DYMEX model builder and simulator (pre-programed module based simulation programs developed by CSIRO, Australia). The DYMEX model simulator consisted of a series of modules with the parameters of temperature dependent development and oviposition models of L. trifolii were incorporated from pre-published data. Leaf surface temperatures of cherry tomato leaves (cv. 'Koko') were monitored according to three tomato plant positions (top, > 1.8 m above the ground level; middle, 0.9 - 1.2 m; bottom, 0.3 - 0.5 m) using an infrared temperature gun. Air temperature was monitored at the same three positions using a self-contained temperature logger. Data sets for the observed air temperature and average leaf surface temperatures were collected (top and bottom surfaces), and incorporated into the DYMEX simulator in order to compare the effects of air and leaf surface temperature on the population dynamics of L. trifolii. The initial population consisted of 50 eggs, which were laid by five female L. trifolii in early June. The number of L. trifolii larvae was counted by visual inspection of the tomato plants in order to verify the performance of DYMEX simulation. The egg, pupa, and adult stage of L. trifolii could not be counted due to its infeasible of visual inspection. A significant positive correlation between the observed and the predicted numbers of larvae was found when the leaf surface temperatures were incorporated into the DYMEX simulation (r = 0.97, p < 0.01), but no significant positive correlation was observed with air temperatures(r = 0.40, p = 0.18). This study demonstrated that the population dynamics of L. trifolii was affected greatly by the leaf temperatures, though to little discernible degree by the air temperatures, and thus the leaf surface temperature should be for a consideration in the management of L. trifolii within cherry tomato greenhouses.

Development of a Method for Analyzing the Nicotine Content in Synthetic Flavoring Substances as Unauthorized E-cigarette Liquid by Using HPLC (전자담배 액상 충진제와 유사한 합성착향료 중 니코틴의 HPLC 분석법 개발)

  • Kim, Jae-Young;Lee, Sang-Mok;Chang, Moon-Ik;Cho, Yoon-Jae;Lee, Han-Jin;Chae, Young-Sik;Rhee, Gyu-Sik
    • Korean Journal of Food Science and Technology
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    • v.45 no.6
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    • pp.693-699
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    • 2013
  • A simple, sensitive, and specific method for quantifying the nicotine content of synthetic favoring substances (SFS) was developed using high performance liquid chromatography (HPLC) with a photo-diode array detector (PDA). Nicotine was extracted from SFS samples by using an acid-base liquid-liquid extraction method with dichloromethane and distilled water. The nicotine content was quantified by HPLC/PDA (261.9 nm) with a $C_{18}$ column under a gradient of 10% acetonitrile with 20 mM ammonium formate (ammonia solution adjusted to pH 8.7) to 100% acetonitrile. The calibration curve, analyzed from concentration standards between 0.1 to 2 mg/L, presented linearity with a correlation coefficient ($r^2$)>0.9999. The limit of quantitation (LOQ) of nicotine in SFS was 0.4 mg/kg, and the average recoveries ranged from 76.4% to 96.3%. The repeatability of measurements, expressed as the coefficient of variation (CV%), ranged from 1.74 to 5.12%. This newly developed method for nicotine quantification in SFS can be considered an analytical method with an acceptable level of sensitivity and repeatability.

Performance Test of the Iterative Method and Newly Developed True X Method (PET 검사에서 Iterative 재구성 방법과 True X 재구성 방법에 따른 영상의 균일성 및 대조도 비교 평가)

  • Choi, Jae-Min;NamKung, Chang-Kyeong;Park, Seung-Yong;Nam, Ki-Pyo;Lim, Ki-Cheon
    • The Korean Journal of Nuclear Medicine Technology
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    • v.13 no.1
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    • pp.20-24
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    • 2009
  • Objective: In this study, the differences between two reconstruction methods were analyzed by comparing image uniformity and contrast according to Iteration and Subset, which were altered through the Iterative method and True X method, used in Siemens' PET/CT studies. Methods: The Phantom images were obtained by exposure for two minutes per one bed. To determine the image uniformity, the Coefficient of variance was used. Also, in order to compare the contrast value, we measured and analyzed the ratio of the SUV mean of Phantom image's hot spheres and the background. Results: Under the same reconstruction conditions (Iteration and Subset) of CV, the Iterative method was higher than the True X method. In the comparison of the SUV mean ratio of the background and hot sphere, the True X method had a closer rate than the Iterative method. Conclusion: The newly developed True X reconstruction method is better than the previously used Iterative method in terms of uniformity and contrast. However, the date for this study was only obtained using the Phantom device. In order to obtain more accurate and useful information from the experiment, further research should be conducted. Also, it is necessary to find the appropriate standards for Iteration and Subset for further experimentation.

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Single Laboratory Validation and Uncertainty Estimation of a HPLC Analysis Method for Deoxynivalenol in Noodles (면류에서 HPLC를 이용한 데옥시니발레놀 분석법의 검증과 불확도 산정)

  • Ee, Ok-Hyun;Chang, Hyun-Joo;Kang, Young-Woon;Kim, Mee-Hye;Chun, Hyang-Sook
    • Journal of Food Hygiene and Safety
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    • v.26 no.2
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    • pp.142-149
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    • 2011
  • An isocratic high performance liquid chromatography (HPLC) method for routine analysis of deoxynivalenol in noodles was validated and estimated the measurement uncertainty. Noodles (dried noodle and ramyeon) were analyzed by HPLC-ultraviolet detection using immunoaffinity column for clean-up. The limits of detection (LOD) and quantification (LOQ) were 7.5 ${\mu}g$/kg and 18.8 ${\mu}g$/kg, respectively. The calibration curve showed a good linearity, with correlation coefficients $r^2$ of 0.9999 in the concentration range from 20 to 500 ${\mu}g$/kg. Recoveries and Repeatabilities expressed as coefficients of variation (CV) spiked with 200 and 500 ${\mu}g$/kg were $82{\pm}2.7%$ and $87{\pm}1.3%$% in dried noodle, and $97{\pm}1.6%$ and $91{\pm}12.0%$ in ramyeon, respectively. The uncertainty sources in measurement process were identified as sample weight, final volume, and sample concentration in extraction volume as well as components such as standard stock solution, working standard solution, 5 standard solutions, calibration curve, matrix, and instrument. Deoxynivalenol concentration and expanded uncertainty in two matrixes spiked with 200 ${\mu}g$/kg and 500 ${\mu}g$/kg were estimated to be $163.8{\pm}52.1$ and $435.2{\pm}91.6\;{\mu}g$/kg for dried noodle, and $194.3{\pm}33.0$ and $453.2{\pm}91.1\;{\mu}g$/kg for ramyeon using a coverage factor of two which gives a level of statistical confidence with approximately 95%. The most influential component among uncertainty sources was the recovery of matrix, followed by calibration curve.

Development and Preliminary Test of a Prototype Program to Recommend Nitrogen Topdressing Rate Using Color Digital Camera Image Analysis at Panicle Initiation Stage of Rice (디지털 카메라 칼라영상 분석을 이용한 벼 질소 수비량 추천 원시 프로그램의 개발과 예비 적용성 검토)

  • Chi, Jeong-Hyun;Lee, Jae-Hong;Choi, Byoung-Rourl;Han, Sang-Wook;Kim, Soon-Jae;Park, Kyeong-Yeol;Lee, Kyu-Jong;Lee, Byun-Woo
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.55 no.4
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    • pp.312-318
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    • 2010
  • This study was carried out to develop and test a prototype program that recommends the nitrogen topdressing rate using the color digital camera image taken from rice field at panicle initiation stage (PIS). This program comprises four models to estimate shoot N content (PNup) by color digital image analysis, shoot N accumulation from PIS to maturity (PHNup), yield, and protein content of rice. The models were formulated using data set from N rate experiments in 2008. PNup was found to be estimated by non-linear regression model using canopy cover and normalized green values calculated from color digital image analysis as predictor variables. PHNup could be predicted by quadratic regression model from PNup and N fertilization rate at panicle initiation stage with $R^2$ of 0.923. Yield and protein content of rice could also be predicted by quadratic regression models using PNup and PHNup as predictor variables with $R^2$ of 0.859 and 0.804, respectively. The performance of the program integrating the above models to recommend N topdressing rate at PIS was field-tested in 2009. N topdressing rate prescribed for the target protein content of 6.0% by the program were lower by about 30% compared to the fixed rate of 30% that is recommended conventionally as the split application rate of N fertilizer at PIS, while rice yield in the plots top-dressed with the prescribed N rate were not different from those of the plots top-dressed with the fixed N rates of 30% and showed a little lower or similar protein content of rice as well. And coefficients of variation in rice yield and quality parameters were reduced substantially by the prescribed N topdressing. These results indicate that the N rate recommendation using the analysis of color digital camera image is promising to be applied for precise management of N fertilization. However, for the universal and practical application the component models of the program are needed to be improved so as to be applicable to the diverse edaphic and climatic condition.

Determination and Survey of Fluoroquinolones Residue in Chicken Muscle by HPLC with Fluorescence Detector (액체크로마토그래피-형광검출기를 이용한 닭고기 중 플루오로퀴놀론계 항균물질 정량분석 및 잔류조사)

  • 박은정;임지흔;이성모
    • Journal of Food Hygiene and Safety
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    • v.19 no.1
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    • pp.12-18
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    • 2004
  • Ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin in chicken muscle were seperated by liquid extraction and determined with high performance liquid chromatography (HPLC) with fluorescence detector. Analysis was carried out using following conditions; Cl8 column (250${\times}$4.6 mm i.d. 5 ${\mu}{\textrm}{m}$ particle size), mobile phase composed of D.W. (containing 0.4% triethylamine and phospholic acid): methanol : acetonitrile (800:100:100, v/v/v), isocratic pump at a flow rate of 1.0 $m\ell$/min and 50 ${mu}ell$ of injection volume, fluorescence detector with EX278 nm/EM.456 nm. The calibration curves of four fluoroquinolones showed linearity (${\gamma}$$^2$$\geq$0.999) at concenration range of 0.025-0.6 $\mu\textrm{g}$/ml. The recoveries in fortified chicken muscle represented more than 80% with low coefficient of variation (〈10%) for concentration range of four fluoroquinolones. The detection limits for ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin were 23.5, 3.4, 3.0 and 2.5 ng/g in chicken muscle, respectively. We also monitored fluoroquinolones residue in muscle of chickens (broiler 1:227, Korean native chicken 219, laying chicken 77) using EEC-4-plate screening and HPLC conformation methods. Ten(broiler 5, Korean native chicken 5) out of the fifteen samples which were positively detected by EEC-plate screening method from 1,523 chicken meat were confirmed with ciprofloxacin and enrofloxacin by HPLC. The ranges of residual concentration were 0-0.12 ppm for ciprofloxacin and 0.01-6.79 ppm for enrofloxacin. In conclusion, our method could be applied effectively to determine four fluoroquinolones residues in chicken meat, and further survey for fluoroquinolones residue in chicken meat are needed for more effective control of fluoroquinolones used in livestock.

Effect of Terephthalaldehyde to Facilitate Electron Transfer in Heme-mimic Catalyst and Its Use in Membraneless Hydrogen Peroxide Fuel Cell (테레프탈알데하이드의 전자전달 강화효과에 따른 헴 단백질 모방 촉매의 성능 향상 및 이를 이용한 비분리막형 과산화수소 연료전지)

  • Jeon, Sieun;An, Heeyeon;Chung, Yongjin
    • Korean Chemical Engineering Research
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    • v.60 no.4
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    • pp.588-593
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    • 2022
  • Terephthalaldehyde (TPA) is introduced as a cross liker to enhance electron transfer of hemin-based cathodic catalyst consisting of polyethyleneimine (PEI), carbon nanotube (CNT) for hydrogen peroxide reduction reaction (HPRR). In the cyclic voltammetry (CV) test with 10 mM H2O2 in phosphate buffer solution (pH 7.4), the current density for HPRR of the suggested catalyst (CNT/PEI/hemin/PEI/TPA) shows 0.2813 mA cm-2 (at 0.2 V vs. Ag/AgCl), which is 2.43 and 1.87 times of non-cross-linked (CNT/PEI/hemin/PEI) and conventional cross liker (glutaraldehyde, GA) used catalyst (CNT/PEI/hemin/PEI/GA), respectively. In the case of onset potential for HPRR, that of CNT/PEI/hemin/PEI/TPA is observed at 0.544 V, while those of CNT/PEI/hemin/PEI and CNT/PEI/hemin/PEI/GA are 0.511 and 0.471 V, respectively. These results indicate that TPA plays a role in facilitating electron transfer between the electrodes and substrates due to the π-conjugated cross-linking bonds, whereas conventional GA cross-linker increases the overpotential by interrupting electron and mass transfer. Electrochemical impedance spectroscopy (EIS) results also display the same tendency. The charge transfer resistance (Rct) of CNT/PEI/hemin/PEI/TPA decreases about 6.2% from that of CNT/PEI/hemin/PEI, while CNT/PEI/hemin/PEI/GA shows the highest Rct. The polarization curve using each catalyst also supports the superiority of TPA cross liker. The maximum power density of CNT/PEI/hemin/PEI/TPA (36.34±1.41 μWcm-2) is significantly higher than those of CNT/PEI/hemin/PEI (27.87±0.95 μWcm-2) and CNT/PEI/hemin/PEI/GA (25.57±1.32 μWcm-2), demonstrating again that the cathode using TPA has the best performance in HPRR.

A Monitoring of Aflatoxins in Commercial Herbs for Food and Medicine (식·약공용 농산물의 아플라톡신 오염 실태 조사)

  • Kim, Sung-dan;Kim, Ae-kyung;Lee, Hyun-kyung;Lee, Sae-ram;Lee, Hee-jin;Ryu, Hoe-jin;Lee, Jung-mi;Yu, In-sil;Jung, Kweon
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.267-274
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    • 2017
  • This paper deals with the natural occurrence of total aflatoxins ($B_1$, $B_2$, $G_1$, and $G_2$) in commercial herbs for food and medicine. To monitor aflatoxins in commercial herbs for food and medicine not included in the specifications of Food Code, a total of 62 samples of 6 different herbs (Bombycis Corpus, Glycyrrhizae Radix et Rhizoma, Menthae Herba, Nelumbinis Semen, Polygalae Radix, Zizyphi Semen) were collected from Yangnyeong market in Seoul, Korea. The samples were treated by the immunoaffinity column clean-up method and quantified by high performance liquid chromatography (HPLC) with on-line post column photochemical derivatization (PHRED) and fluorescence detection (FLD). The analytical method for aflatoxins was validated by accuracy, precision and detection limits. The method showed recovery values in the 86.9~114.0% range and the values of percent coefficient of variaton (CV%) in the 0.9~9.8% range. The limits of detection (LOD) and quantitation (LOQ) in herb were ranged from 0.020 to $0.363{\mu}g/kg$ and from 0.059 to $1.101{\mu}g/kg$, respectively. Of 62 samples analyzed, 6 semens (the original form of 2 Nelumbinis Semen and 2 Zizyphi Semen, the powder of 1 Nelumbinis Semen and 1 Zizyphi Semen) were aflatoxin positive. Aflatoxins $B_1$ or $B_2$ were detected in all positive samples, and the presence of aflatoxins $G_1$ and $G_2$ were not detected. The amount of total aflatoxins ($B_1$, $B_2$, $G_1$, and $G_2$) in the powder and original form of Nelumbinis Semen and Zizyphi Semen were observed around $ND{\sim}21.8{\mu}g/kg$, which is not regulated presently in Korea. The 56 samples presented levels below the limits of detection and quantitation.