• Title/Summary/Keyword: Spiking

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Effects of Electrical Stimulation on Physicochemical and Rheological Properties of Plaice, Paralichthys olivaceus Muscle at Early Period after Death (전기자극이 넙치육의 사후조기의 물리화학적 및 물성적 변화에 미치는 영향)

  • LEE Nam-Geoul;YANG Mu-Hae;CHO Young-Je
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.28 no.1
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    • pp.23-30
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    • 1995
  • This study was undertaken to clarify the effects of electrical stimulation on physicochemical and rheological properties of the plaice (Paralichthys olivaceus) muscle at early period after death. The plaices were electrically stimulated in seawater bath (110V/60Hz) for 15sec., 35sec., and 60sec. and killed instantly with spiking at the head. Killed samples were stored at $5^{\circ}C$, and the changes in rigor index, ATP breakdown, lactate accumulation, and breaking strength of muscle through storage were investigated. Electrical stimulation effectively accelerated rigor-mortis, lactate accumulation , and ATP breakdown. As the time of electrical stimulation was lengthened, the onset of rigor-mortis of all samples were accelerated Just after killing, and the amount of lactate was rapidly increased, But, significant differences were not observed in variance of rigor-mortis and lactate concentration. Electrically stimulated plaices showed decreasing in ATP to $4.58{\mu}mole/g$ for 15sec., $4.13{\mu}mole/g$ for 35sec., and $2.39{\mu}mole/g$ for 60sec. samples as compared with $5.5{\mu}mole/g$ of unstimulated samples. As the time of electrical stimulation was lengthened, ATP in samples were decomposed more rapidly. The rate constant of ATP breakdown were $0.244hr^{-1}$ for 15sec., $0.358hr^{-1}$ for 35sec., and $0.479hr^{-1}$ for 60sec.. The level of breaking strength in muscle of the plaice was $1050.30\pm50.23g$ immediately after killing. Values of breaking strength in samples electrically stimulated for 35sec. increased rapidly just after killing among all samples. However, the breaking strength was not increased through the whole storage time in samples stimulated for 60sec.. The value and time roaching to the maximum breaking strength for each samples stimulated electrically for 15, 35 and 60 second were $1264.43\pm35.76g$ and 2hr, $1357.68\pm22.50g$ and Ohr, and $1012.18\pm57.36g$ and Ohr. Breaking strength in all samples electrically stimulated decreased significantly (P<0.05) after reaching the maximum values.

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Validation of a Rapid Quantitative Method for the Residues of Nitrofuran Metabolites in Loach by Accelerated Solvent Extraction and HPLC Triple Quadrupole Mass Spectrometry

  • Ryu, Eun Chae;Han, Yun-jeong;Park, Seong-soo;Lim, Chul-joo;Choi, Sunok;Park, Se Chang
    • Journal of Food Hygiene and Safety
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    • v.31 no.2
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    • pp.85-93
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    • 2016
  • A rapid method using HPLC-MS/MS has been developed for quantitative determination of the metabolites of nitrofurans, namely 3-amino-2-oxazolidone (AOZ), 5-morpholinomethyl-3-amino-2-oxazolidinone (AMOZ), 1-ammino-hydantoin (AHD) and semicarbazide (SEM) in loach. The extraction procedure was founded on simultaneous acidic hydrolysis and derivatization using 2-nitrobenzaldehyde (2-NBA) for 1 hour at $50^{\circ}C$, followed by purification with liquid-liquid extraction. Recovery was evaluated by spiking standards into blank samples at three levels (0.5, 1.0 and $2.0{\mu}g/kg$), and the mean recovery was 75.1-108.1%. Precision values expressed as the relative standard deviation (%RSD) were ${\leq}8.7%$ and ${\leq}8.5%$ for intra-day and inter-day precision, respectively. Linearity was studied in the range of $0.2-20{\mu}g/Kg$ for NBAOZ, $0.8-20{\mu}g/Kg$ for NBAMOZ, $0.2-20{\mu}g/Kg$ for NBAHD, and $0.1-20{\mu}g/Kg$ for NBSEM, and the obtained coefficient correlations (r) were ${\geq}0.99$ for all compounds. Limits of detection (LODs) for the derivatized nitrofuran metabolites were established at $0.06{\mu}g/Kg$ for NBAOZ, $0.24{\mu}g/Kg$ for NBAMOZ, $0.06{\mu}g/Kg$ for NBAHD, and $0.03{\mu}g/Kg$ for NBSEM. Limits of quantification (LOQs) were established at $0.2{\mu}g/Kg$ for NBAOZ, $0.8{\mu}g/Kg$ for NBAMOZ, $0.2{\mu}g/Kg$ for NBAHD, and $0.1{\mu}g/Kg$ for NBSEM. This simplified rapid method for reducing the derivatization and hydrolysis times can be applied to the determination of nitro-furan residues in loach.

Analytical Method for MCPA Residue in Brown Rice and Rice Straw by HPLC/UVD (HPLC/UVD를 이용한 현미와 볏짚 중 MCPA의 잔류분석방법 확립)

  • Yoo, Ki-Yong;Kang, Dae-Won;Choi, Yong-Hwa;Han, Seong-Soo
    • Korean Journal of Weed Science
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    • v.30 no.4
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    • pp.361-370
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    • 2010
  • This study was carried out to establish the analytical method of MCPA residue in brown rice and rice straw by HPLC/UVD. When MCPA was extracted from sample under the pH 3.6 by adding acetone 200 mL and 1N-HCl 100 mL, the extraction efficiency was high by 87%. And purification efficiency was high by 83% when 5 mL of 1% methanol/acetonitrile was eluated by the florisil Sep-pak cartridge column. From spiking of $0.1{\mu}g\;mL^{-1}$ and $0.25{\mu}g\;mL^{-1}$ of MCPA to control sample, respectively, average recovery rate of MCPA in brown rice was 96.0% and 94.9% and that in rice straw was 92.5% and 88.2%, respectively. Precision of experiment was very high by relative standard deviation of 1.5% to 5.7%. In brown rice and rice straw treated with bentazone+MCPA (11+1.2%) of 30 kg and 60 kg per ha at 30 days after rice transplanting, respectively, maximum residue limit was under $0.05{\mu}g\;mL^{-1}$ of the recommended rate of Korean Food and Drug Administration. From the above results, the analytical procedure of MCPA in plants such as hydrolysis, saponification and derivatization were ommited, and retention time was faster and recovery rate was higher than the existed results of HPLC/UVD. Therefore, these results were greatly improved and seemed to be usefully applied for residue analysis of MCPA in plants.

Fate of Heavy Metals in Activated Sludge: Sorption of Heavy Metal ions by Nocardia amarae

  • Kim, Dong-wook
    • Proceedings of the Korean Environmental Sciences Society Conference
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    • 1998.10a
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    • pp.2-4
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    • 1998
  • Proliferation of Nocardia amarae cells in activated sludge has often been associated with the generation of nuisance foams. Despite intense research activities in recent years to examine the causes and control of Nocardia foaming in activated sludge, the foaming continued to persist throughout the activated sludge treatment plants in United States. In addition to causing various operational problems to treatment processes, the presence of Nocardia may have secondary effects on the fate of heavy metals that are not well known. For example, for treatment plants facing more stringent metal removal requirements, potential metal removal by Nocardia cells in foaming activated sludge would be a welcome secondary effect. In contrast, with new viosolid disposal regulations in place (Code o( Federal Regulation No. 503), higher concentration of metals in biosolids from foaming activated sludge could create management problems. The goal of this research was to investigate the metal sorption property of Nocardia amarae cells grown in batch reactors and in chemostat reactors. Specific surface area and metal sorption characteristics of N. amarae cells harvested at various growth stages were compared. Three metals examined in this study were copper, cadmium and nickel. Nocardia amarae strain (SRWTP isolate) used in this study was obtained from the University of California at Berkeley. The pure culture was grown in 4L batch reactor containing mineral salt medium with sodium acetate as the sole carbon source. In order to quantify the sorption of heavy metal ions to N amarae cell surfaces, cells from the batch reactor were harvested, washed, and suspended in 30mL centrifuge tubes. Metal sorption studies were conducted at pH 7.0 and ionlc strength of 10-2M. The sorption Isotherm showed that the cells harvested from the stationary and endogenous growth phase exhibited significantly higher metal sorption capacity than the cells from the exponential phase. The sequence of preferential uptake of metals by N. amarae cells was Cu>Cd>Ni. The specific surFace area of Nocardia cells was determined by a dye adsorption method. N.amarae cells growing at ewponential phase had significantly less specific surface area than that of stationary phase, indicating that the lower metal sorption capacity of Nocardia cells growing at exponential phase may be due to the lower specific surface area. The growth conditions of Nocardia cells in continuous culture affect their cell surface properties, thereby governing the adsorption capacity of heavy metal. The comparison of dye sorption isotherms for Nocardia cells growing at various growth rates revealed that the cell surface area increased with increasing sludge age, indicating that the cell surface area is highly dependent on the steady-state growth rate. The highest specific surface area of 199m21g was obtained from N.amarae cell harvested at 0.33 day-1 of growth rate. This result suggests that growth condition not only alters the structure of Nocardia cell wall but also affects the surface area, thus yielding more binding sites of metal removal. After reaching the steady-state condition at dilution rate, metal adsorption isotherms were used to determine the equilibrium distributions of metals between aqueous and Nocardia cell surfaces. The metal sorption capacity of Nocardia biomass harvested from 0.33 day-1 of growth rate was significantly higher than that of cells harvested from 0.5- and 1-day-1 operation, indicatng that N.amarae cells with a lower growth rate have higher sorpion capacity. This result was in close agreement with the trend observed from the batch study. To evaluate the effect of Nocardia cells on the metal binding capacity of activated sludge, specific surface area and metal sorption capacity of the mixture of Nocardia pure cultures and activated sludge biomass were determined by a series of batch experiments. The higher levels of Nocardia cells in the Nocardia-activated sludge samples resulted in the higher specific surface area, explaining the higher metal sorption sites by the mixed luquor samples containing greater amounts on Nocardia cells. The effect of Nocardia cells on the metal sorption capacity of activated sludge was evaluated by spiking an activated sludge sample with various amounts of pre culture Nocardia cells. The results of the Langmuir isotherm model fitted to the metal sorption by various mixtures of Nocardia and activated sludge indicated that the mixture containing higher Nocardia levels had higher metal adsorption capacity than the mixture containing lower Nocardia levels. At Nocardia levels above 100mg/g VSS, the metal sorption capacity of activate sludge increased proportionally with the amount of Noeardia cells present in the mixed liquor, indicating that the presence of Nocardia may increase the viosorption capacity of activated sludge.

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Analysis of Four Pesticides, Isoproturon, Phenmedipham, Pyridate and Nitenpyram Residues by High-Performance Liquid Chromatography with Diode-Array Detector (HPLC를 이용한 Isoproturon, Phenmedipham, Pyridate 및 Nitenpyram 4종 성분의 잔류농약 분석법 개발)

  • Yang, Sung-Yong;Koo, Yun-Chang;Wang, Zeng;Heo, Kyeong;Kim, Hyeong-Kook;An, Eun-Mi;Shin, Han-Seung;Lee, Jin-Won;Lee, Kwang-Won
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.39 no.8
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    • pp.1165-1170
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    • 2010
  • A method for the determination of four pesticide compounds, urea (isoproturon), bis-carbamate (phenmedipham), thiocarbamate (pyridate) and vinyllidenediamine (nitenpyram) were examined and analyzed by HPLC with C-18 column ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size). Mobile phase consisted of deionized water, acetonitrile and 50 mM $KH_2PO_4$ (pH 2.5). Isoproturon and phenmedipham analytical condition was isocratic elution of the column with 50% solvent A (acetonitrile) and 50% solvent B (deionized water); pyridate was 85% solvent A (acetonitrile) and 15% solvent B (deionized water) at a flow rate of 1 mL/min; and nitenpyram analytical condition was 90% solvent A (50 mM $KH_2PO_4$, pH 2.5) and 10% solvent B (acetonitrile) at a flow rate of 1 mL/min. In results, retention times were 6.12, 8.63, 9.40 and 12.76 min for isoproturon, phenmedipham, pyridate and nitenpyram, respectively. All injection volumes were $10\;{\mu}L$ and the limit of quantitation was 0.05 mg/kg for four pesticide compounds, respectively. Recovery rate test was performed with three farm products, rice, apple and soybean. Four pesticide compounds were spiked at concentrations of 0.05, 0.1 and 0.5 mg/kg. The recovery rates were ranged from 70.18% to 118.08% and the standard deviations of all experiments were within 10%.

Modified QuEChERS Multi-Residue Analysis Method for 61 pesticides in Fruits using with HPLC and GC-ECD/NPD (HPLC 및 GC-ECD/NPD를 이용한 과일 중 61종 농약의 QuEChERS 전처리 다성분 분석법 개발)

  • Lee, Ju-Young;Hong, Su-Myeong;Kim, Taek-Kyum;Min, Zaw Win;Kim, Yang-Hyeon;Song, Kyung-Ae;Kwon, Hye-Yong;Lee, Hee-Dong;Im, Geon-Jae;Kim, Doo-Ho;Kim, Jang-Eok
    • The Korean Journal of Pesticide Science
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    • v.16 no.3
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    • pp.242-256
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    • 2012
  • QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method has been a lot of research for pesticide analysis, because it is very simple and fast. However, this method requires high sensitivity instrument such as LC-MS/MS because of the use of small sample volume and many impurities compared to the conventional method. So, QuEChERS method needs to be modified for using with HPLC and GC-ECD/NPD. The aim of this work was to study the application of the QuEChERS method as well as its modification for the extraction and preconcentration of 5 groups of 61 pesticides from 4 fruits prior to their determination by HPLC-PDA, GC-ECD/NPD, and LC-MS/MS. The method was validated using spiking levels at 0.1 mg/kg (or 0.01 mg/kg) in apple, grapes, pear and persimmon. The average recovery by QuEChERS AOAC Official 2007. 01 version using the LC-MS/MS varied from 71.1127.4% for 61 pesticides. The average recovery rates using modified QuEChERS varied from 70.9~126% for 61 pesticides by HPLC-PDA and GC-ECD/NPD. The results satisfied the criteria of multiple pesticide residue analysis, setting 70~130% for recovery rates and below 30% for CV.

Determination of Aflatoxins in Nuts, Their Products and Dried Fruits Using Rapid Resolution Liquid Chromatography Coupled with Tandem Mass Spectrometry (RRLC-MS/MS를 이용한 견과류 및 그 가공품과 건조과실류의 아플라톡신 분석)

  • Choi, Su-Jeong;Park, Ju-Sung;Jung, So-Young;Son, Yeo-Joon;Lyi, Yun-Jeong;Kim, Mi-Sun;Park, So-Hyun;Lee, Sang-Me;Chae, Young-Zoo
    • Korean Journal of Food Science and Technology
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    • v.43 no.6
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    • pp.702-710
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    • 2011
  • The occurrence of aflatoxins $B_1$, $B_2$, $G_1$ and $G_2$ in nuts, their products and dried fruits was investigated. Samples were collected from local markets in Seoul and analyzed by rapid resolution liquid chromatography coupled with tandem mass spectrometry using an immunoaffinity column. The chromatography method was validated for assay of aflatoxins using linearity, accuracy, precision and limit of detection and quantification. The linearity in the concentration ranged from 0.10 to $20{\mu}g/kg$ with $R^2$ > 0.9999. Sample recoveries ranged from 71.1 to 97.2% with relative standard deviations below 4.5% for spiking levels from 1 to $10{\mu}g/kg$. The limits of detection ranged between 0.02 and $0.05{\mu}g/kg$ and the limits of quantification ranged between 0.05 and $0.10{\mu}g/kg$. The levels of aflatoxin $B_1$, $B_2$, $G_1$ and $G_2$ in nuts, their products and dried fruits were $B_1$ 0.10 to $9.94{\mu}g/kg$, $B_2$ 0.08 to $1.54{\mu}g/kg$, $G_1$ 0.04 to $3.21{\mu}g/kg$ and $G_2$ 0.06 to $0.14{\mu}g/kg$.

Modeling on the Sorption Kinetics of Lead and Cadmium onto Natural Sediments (퇴적물에서의 납과 카드뮴의 흡착 동력학 모델링)

  • Kwak, Mun-Yong;Ko, Seok-Oh;Park, Jae-Woo;Jeong, Yeon-Gu;Shin, Won-Sik
    • Korean Journal of Ecology and Environment
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    • v.39 no.4 s.118
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    • pp.450-461
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    • 2006
  • In this study, sorption kinetics of lead (Pb) and cadmium (Cd) onto coastal sediments were investigated at pH 5.5 using laboratory batch adsorbers. Four different models: one-site mass transfer model (OSMTM), pseudo-first-order kinetic model (PFOKM) ,pseudo-second-order kinetic model (PSOKM) and two compartment first-order kinetic model (TCFOKM) were used to analyze the sorption kinetics. As expected from the number of model parameters involved, the three-parameter TCFOKM was better than the two-parameter OSMTM, PFOKM and PSOKM in describing sorption kinetics of Pb and Cd onto sediments. Most sorption of Pb and Cd was rapidly completed within the first three hours, followed by slow sorption in the subsequent period of sorption. All models predicted that the sorbed amount at the apparent sorption ($q_{e,s}$) equilibria increased as the CEC and surface area of the sediments increased, regardless of initial spiking concentration ($C_0$) and heavy metal and the sediment type. The sorption rate constant ($k_s,\;hr^{-1}$) in OSMTM also increased as the CEC and BET surface area increased. The rate constant of pseudo-first-order sorption ($k_{p1,s},\;hr^{-1}$) in PFOKM were not correlated with sediment characteristics. The results of PSOKM analysis showed that the rate constant of pseudo-second-order sorption ($k_{p2,s},\;g\;mmol^{-1}\;hr^{-1}$) and the initial sorption rate ($v_{o,s},\;mg\;g^{-1}\;hr^{-1}$) were not correlated with sediment characteristics. The fast sorption fraction ($f_{1,s}$) in TCFOKM increased as CEC and BET surface increased regardless of initial aqueous phase concentrations. The sorption rate constant of fast fraction ($k_{1,s}=10^{0.1}-10^{1.0}\;hr^{-1}$) was much greater than that of slow sorption fraction ($k_{2,s}=10^{-2}-10^{-4}\;hr^{-1}$) respectively.

Development of Analytical Method for Kasugamycin in Agricultural Products using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Kasugamycin 시험법 개발)

  • Lee, Han Sol;Do, Jung-Ah;Park, Ji-Su;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.235-241
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    • 2019
  • An analytical method was developed for the determination of an antibiotic fungicide, kasugamycin, in agricultural products (hulled rice, potato, soybean, mandarin and green pepper) using liquid chromatographytandem mass spectrometry (LC-MS/MS). Samples were extracted with methanol adjusted to pH 13 using 1 N sodium hydroxide, and purified with a HLB (hydrophilic lipophilic balance) cartridge. Linearity of a matrix-matched calibration curve using seven concentration levels, from 0.001 to 0.1 mg/kg, was excellent with a correlation coefficient ($R^2$) of more than 0.9998. The limits of detection (LOD) and quantification (LOQ) of instrument were 0.0005 and $0.001{\mu}g/mL$, respectively, and the LOQ of analytical method calculated as 0.01 mg/kg. The average recoveries at three spiking levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) were in the range of 71.2~95.4% with relative standard deviation of less than 12.1%. The developed method was simple and all optimized results was satisfied with the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. The present study could be served as a reference for the establishment of maximum residue limits (MRL) of kasugamycin and be used as basic data for safety management relative to kasugamycin residues in imported and domestic agricultural products.