• Title/Summary/Keyword: 최소검출한계

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Residual Change of Deltamethrin in Stream Water after Spaying for Pest Control of Stream Levee (하천둔치에 방역용 Deltamethrin 살포 시 하천수 중 잔류변화)

  • Han, Ye-Hun;Park, Jae-Hun;Lim, Jong-Sung;Lee, Yong-Ju;Lee, Sung-Kyu;Lee, Kyu-Seung
    • Korean Journal of Environmental Agriculture
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    • v.32 no.1
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    • pp.78-83
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    • 2013
  • BACKGROUND: This study was performed to investigate the change of deltamethrin residue after spraying for control of hygienic insects in bush of levee at Bansuk-dong stream (A) and Juk-dong ditch (B) in Yuseong, Daejeon. The drop concentrations and disappearance of deltamethrin residue in stream water were determined to evaluate the toxic effects of stream ecosystem. METHODS AND RESULTS: Water samples were collected at 7 points including 0, 5, 10, 20, 40, 70 and 100 m downstream from the deltamethrin spraying point. Water sample was partitioned into dichloromethane, and was determined with GC/${\mu}$-ECD. Limit of Quantitation of deltamethrin was 0.04 ${\mu}g/L$. Recoveries of deltamethrin at two fortification levels of 0.4 and 2.0 ${\mu}g/L$ were $91.57{\pm}3.13%$(n=3) and $94.40{\pm}4.59%$(n=3) in A stream, and $88.24{\pm}3.33%$(n=3) and $85.20{\pm}3.73%$(n=3) in B stream, respectively. Residue of A stream were from <0.04 ${\mu}g/L$ to 0.48 ${\mu}g/L$ and B stream were from 0.08 ${\mu}g/L$ to 14.95 ${\mu}g/L$ under practice application condition. And residues were from <0.04 ${\mu}g/L$ to 0.2 ${\mu}g/L$ in A stream treated deltamethrin with 1.0 mg level at the upper region. CONCLUSION(S): Practice application of deltamethrin for the pest control of waterside was not much shown toxic effect to ecosystem of stream.

Clinical Evaluation of a Rapid Diagnostic Test Kit for Canine Parvovirus and Coronavirus (개 파보바이러스와 코로나바이러스 진단을 위한 신속진단키트의 임상적 유용성)

  • Chaeyeong MIN;Won-Shik KIM;Chom-Kyu CHONG;Yong LIM
    • Korean Journal of Clinical Laboratory Science
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    • v.55 no.1
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    • pp.45-51
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    • 2023
  • Canine parvovirus type 2 (CPV-2) and canine coronavirus (CCoV) are major pathogens that can induce gastroenteritis in dogs. They are highly contagious and have a high morbidity rate. There are no specific treatments available for them to date. Therefore, rapid and accurate diagnosis becomes essential. The rapid diagnostic test (RDT) for animals can be used widely in the field because it is fast and easy to use for diagnosis. Thus, this study aimed to clinically evaluate and confirm the clinical utility of CPV-2/CCoV RDT. The parameters evaluated included the limit of detection (LoD), cross-reactivity, interference, sensitivity, specificity, negative likelihood ratio (NLR), and kappa value. The results revealed that the LoD values for CPV-2 and CCoV were 9.7×10 50% tissue culture infectious dose (TCID50)/mL and 2.5×102 TCID50/mL, respectively. There was no cross-reactivity with nine pathogens or interference by interfering materials. The RDT showed a sensitivity of 90.0%, a specificity of 100.0%, NLR of 0.1, and a kappa value of 0.90 for diagnosing both viruses. In conclusion, CPV-2/CCoV RDT is useful as a screening test because of its high sensitivity, specificity, kappa value, and low NLR.

Determination of mandipropamid residues in agricultural commodities using high-performance liquid chromatography with mass spectrometry (고성능액체크로마토그래피를 이용한 농산물 중 Mandipropamid의 잔류분석법 확립)

  • Kwon, Chan Hyeok;Chang, Moon Ik;Im, Moo Hyeog;Choi, Hoon;Jung, Da I;Lee, Su Chan;Yu, Jin Young;Lee, Young Deuk;Lee, Jong Ok;Hong, Moo Ki
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.518-525
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    • 2008
  • Mandipropamid is a new mandelamide-type fungicide to control foliar Oomycete pathogens in some vegetables. An analytical method was developed to determine mandipropamid residues in agricultural commodities using high-performance liquid chromatography (HPLC) and liquid chromatography/mass spectrometry (LC/MS). Mandipropamid was extracted with methanol from grape, tomato, green pepper, Chinese cabbage and potato samples. The extract was diluted with saturated sodium chloride solution and distilled water, and dichloromethane partition was followed to recover the mandipropamid from the aqueous phase. Florisil column chromatography was employed to further remove interfering co-extractives prior to HPLC analysis. Reverse-phased HPLC was successfully applied to determine mandipropamid in sample extracts with the detection at its ${\lambda}_{max}$ (223 nm). Overall recoveries of mandipropamid from fortified samples averaged $99.8{\pm}1.7$ (n=6), $89.3{\pm}5.3$ (n=6), $98.7{\pm}2.2$ (n=6), $99.7{\pm}6.8$ (n=6) and $91.1{\pm}3.1$ (n=6) for grape, tomato, green pepper, Chinese cabbage and potato, respectively. Limit of quantification of the method was 0.02~0.04 mg/kg for all samples. A LC/mass spectrometry with selected-ion monitoring was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to determine the terminal residue of mandipropamid in agricultural commodities.

Method comparison for analyzing formaldehyde in marker pen ink (마킹펜 잉크 내 폼알데하이드 분석법 비교)

  • Park, Kwang Seo;Kim, Yong Shin;Choe, Eun Kyung
    • Analytical Science and Technology
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    • v.33 no.3
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    • pp.115-124
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    • 2020
  • Marker pens belong to school things that are controlled by the regulation system called safety confirmation under special act on the safety of products for children with the formaldehyde criteria of 20 mg/kg. With nine marker pens available commercially, formaldehyde in marker pen ink was analyzed by present test standard where marking on a fabric swatch with a pen and extracting the swatch in water and derivatization with Nash reagent followed by UV/Vis spectrophotometeric measurement (Nash-UV/Vis method), giving not detected results or a false positive result in case of a colored water extract. However, the contents of formaldehyde in ink of nine marker pens were determinded to range between 3.2 ~ 93.2 mg/kg with three results above the safety criteria of 20 mg/kg by HPLC/DAD measurements on DNPH derivatives of formaldehyde (DNPH-HPLC/DAD method) in ink dissolved directly in water using an ultrasonic bath. Therefore, the DNPH-HPLC/DAD method with the extraction of ultrasonic dissolving ink in water is proposed as a proper method for analyzing formaldehyde in ink. The proposed method has advantages of lower detection limit and accuracy with colored extracts as well as a simple and fast extraction. The accuracy and precision of this method was estimated to be 90.1 ~ 105.4 % and 0.6 ~ 3.3 %, respectively by spiking tests in the ranges of 20 mg/kg and 40 mg/kg using matrixes such as highlighter pen ink, board marker ink, chalk marker pen ink and painter marker ink.

Optimization of Analytical Conditions for the Quantification of Explosive Compounds in Soil using HPLC (HPLC에 의한 토양내 화약물질 정량분석조건 최적화)

  • Cho, Jung-Hyun;Bae, Bum-Han;Kim, Kye-Hoon
    • Journal of Soil and Groundwater Environment
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    • v.14 no.1
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    • pp.51-60
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    • 2009
  • A series of experiments was performed to develop an optimized analytical procedure for the analysis of explosives in soil by HPLC with soil samples collected at two live-fire military shooting ranges. The minimum amount of soil to be collected, Wmin, for the analysis of explosive compounds was 125g, based on the segregation and homogeneity constants that account for soil heterogeneity and non-homogeneous distribution of target explosive compounds. The optimization of extraction and HPLC analytical conditions were also studied based on analytes CV values. The most effective soil/ extractant ratio was estimated to be 10g-pretreated soil/20 mL acetonitrile as extractant. The optimized HPLC elution conditions for the separation of US EPA designated 14 explosive compounds, were column temperature 30${\circ}C$, eluents ratio of isopropanol: acetonitrile: water = 18 : 12: 70, and flow rate of 0.8 mUmin at 230 nm. However, UV wavelength 254 nm was better for the analysis of NB, 2,4-DNT, 2NT, 4NT, and 3NT.

Study on analysis of PAHs in consumer products (공산품 함유 PAHs 분석법에 관한 연구)

  • Song, Moon Hwan;Cho, Young Dal;Choe, Eun Kyung
    • Analytical Science and Technology
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    • v.27 no.4
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    • pp.201-212
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    • 2014
  • Polycyclic aromatic hydrocarbons (PAHs) that are carcinogenic and persistent will be restricted in consumer products from December 27, 2015 by EU REACH regulation. Pretreatment using Soxhlet extraction and quantitative analysis by GC-MS were studied to develop the method for analyzing 18 PAHs in consumer products as well as to detect the amounts and the kinds of PAHs in consumer products such as grips of a bag and a hammer, a cable and a plastic sandal. Linearity and precisions were evaluated by analyses of the standard PAH solutions ranging from 0.3125 mg/L to 5.00 mg of each of 18 PAHs. Linearity of resulting standard curves for all 18 PAHs were obtained with $R^2$ above 0.999. Precisions of the retention times and the peak areas were found to be 0.00%~0.05% and 1.16%~3.69% of relative standard deviations, respectively. The recoveries for spiked samples were all around 95%~105% after Soxhlet extration using three different solvents such as dichloromethane, hexane and toluene. The limits of quantitation for 18 PAHs in solutions and polymer samples by GC-MS were evaluated to be 0.327 mg/L (Benzo[ghi]perylene)~0.464 mg/L (Acenaphthylene) and 1.635 mg/kg (Benzo[ghi]perylene)~2.32 mg/kg (Acenaphthylene) based upon dilution factor of 5, respectively. Under the developed analytical method, only trace amounts of phenanthrene were detected in three samples while 15 kinds of PAHs including phenanthrene were detected in a grip of hammer with concentrations of maximum 83.4 mg/kg of Phenanthrene and minimum 8.5 mg/kg of Acenaphthylene. Further studies are needed to decrease the quantitation limit and to check the feasibility of decreasing Soxhlet time as well as to demonstrate cases that the clean up is required.

Determination of Neonicotinoid Pesticides in Commercial Agricultural Products by LC-MS/MS (LC-MS/MS를 이용한 농산물중 Neonicotinoid 계 농약분석)

  • Hwang, Lae-hong;Yang, Hye-ran;Lee, Jae-kyoo;Kim, Chang-kyu;Kim, Min-jung
    • Journal of Food Hygiene and Safety
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    • v.35 no.4
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    • pp.312-318
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    • 2020
  • A method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for neonicotinoid pesticide analysis in agricultural products. Four compounds (imidacloprid, clothianidin, acetamiprid, thiacloprid) were extracted with acetonitrile from agricultural products and cleaned up by NH2 solid-phase extraction procedure, and eluted with 0.1% formic acid in methanol/dichloromethane (5/95, v/v). The limit of detection and quantification were 0.0001-0.0005 mg/kg and 0.001 mg/kg, respectively. The mean recoveries of neonicotinoid pesticide from agricultural products were in the range of 90.7-100.9% and 94.4-99.8%, as spiked at 0.2 mg/kg and 0.02 mg/kg, respectively. This validation satisfied the national criteria for pesticide analytical methods. In summary, The present method is fast, precise and sensitive enough for the Positive List System (PLS), and we conclude that the method is also suitable for neonicotinoid pesticide determination in a wide range of agricultural products.

Quality Characteristics of Retorted Chicken Breast Products Packaged in a Multilayer Barrier Tray During Chilled Storage (차단성 다층 트레이에 포장된 레토르트 닭 가슴살제품의 냉장 중 품질 특성)

  • Jang, Dong-Hyun;Lee, Keun-Taik
    • Food Science of Animal Resources
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    • v.32 no.4
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    • pp.483-490
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    • 2012
  • Ready-to-eat chicken breasts were packaged in a multilayer, gas-tight tray with top film and various quality changes were investigated during the 24 wk of storage at $10^{\circ}C$. Over the storage period, total aerobes, mesophilic aerobic and anaerobic spore formers, and Clostridium spp. were not detected above 1.0 log CFU/g (detection limit). The residual oxygen ratio in the head space of tray and pH values tended to decrease with storage time, namely from initial values of 5.7% and 6.56 to 3.3% and 6.34 at week 24, respectively. Thiobarbituric acid reactive substances and volatile basic nitrogen values increased from 0.52 mg malonaldehyde (MA)/kg and 2.1 mg/100 g initially, to 3.70 mg MA/kg and 39.9 mg/100 g at week 24, respectively. In terms of the change in meat color during storage, the samples showed a slight increasing trend of CIE $a^*$, $b^*$, and ${\Delta}E$ values over the storage period until week 24 (p<0.05). The change in brine color showed a similar trend with meat of which Hunter $b^*$ and ${\Delta}E$ values increased slightly during storage during 24 wk (p<0.05). The values for the transmittance degree of brine in the samples tended to decrease. Moreover, values for the absorbance degree tended to increase with storage time until week 24. The sensory scores for color, texture, odour, and flavour were evaluated below 5.0 (marketability level) after 24 wk of storage. Based on this sensory evaluation, it could be concluded that retorted RTE chicken breast could remain marketable for at least 20 wk at $10^{\circ}C$.

Comparative Study of the Efficiency of GC with Large Volume Injector and SPE Clean-up Process Applied in QuEChERS Method (GC-대용량 주입장치와 SPE를 적용한 QuEChERS 잔류농약 분석법의 효율성 비교)

  • Park, Young Jun;Hong, Su Myeong;Kim, Taek Kyum;Kwon, Hye Young;Hur, Jang Hyun
    • The Korean Journal of Pesticide Science
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    • v.19 no.4
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    • pp.370-393
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    • 2015
  • This study was conducted to compare STQ method, multi-residue method in Korean food code and QuEChERS method for validated selected and accuracy, reproducibility and efficiency. A total of 45 selected and targeted pesticides were the analyzed by GC and 5 of them were crops (apple, potato, green pepper, rice, soy bean). $R^2$ values were calculated in the standard calibration curve was over 0.990. Recovery tests were performed by three replications in two levels and the relative standard deviation of the repeated experiments was less than 30%. The average percentage of recoveries in the multi-residue method in Korean food code was 89.13%, QuEChERS method was 92.45% and STQ method was 85.28%. In addition, matrix effects in multi-residue method in Korean food code was 24.61%, QuEChERS method was 23.98% and STQ method showed 11.24%. The STQ method is easy and showed high clean-up effect in extracting the sample solution than the QuEChERS method and clean-up with C18, PLS, PSA cartridge columns. A large volume of the sample was injected in order to compensable for the problem, that occurred due to high detection limit in the analyser. When the STQ method was applied using a large volume injector, the standard calibration curve showed a higher linearity $R^2=0.990$, and method detection limit was 0.01 mg/kg. It showed an average recovery of 91.84% and the relative standard deviations of three replications repeated in two level process was less than 30% and had an average matrix effect of 17.90%.

Development of a Nuclease Protection Assay With Sandwich Hybridization (NPA-SH) to Monitor Heterosigma akashiwo (Heterosigma akashiwo를 모니터하기 위한 뉴클레아제 보호 분석이 통합된 샌드위치 혼성(NPA-SH)의 개발)

  • Kang, Mingyeong;Park, Mirye;Kim, Kang Eun;Lee, Taek-Kyun
    • Journal of Life Science
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    • v.30 no.1
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    • pp.26-31
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    • 2020
  • Heterosigma akashiwo is a globally distributed raphidophyte that forms blooms and causes significant losses to the aquaculture industry in many coastal countries. The development of a fast and sensitive detection method is therefore required to facilitate the appropriate warning of harmful algal blooms. In this study, a nuclease protection integrated with sandwich hybridization (NPA-SH) assay was developed to both qualitatively and quantitatively detect H. akashiwo. The NPA, capture and signal probes were designed by nucleotide sequencing of H. akashiwo. The applicability of NPA-SH was evaluated using cultured H. akashiwo cells and field samples collected at Goseong Bay, Korea. The results show that this method has good applicability and effectiveness in analyzing cultured cells and field samples. A linear regression equation for the quantitative analysis of H. akashiwo was obtained, and the lower detection limit of the assay was 1×104 cells/ml. There was no statistically significant difference in the results of H. akashiwo quantitation using NPA-SH compared to those obtained using a microscope. These results indicate that NPA-SH can be a good alternative to the traditional microscopic method used to monitor H. akashiwo.