• Title/Summary/Keyword: method detection limit

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Development of Multi-Residue Methods for Carbamate Pesticides by the Enzyme Inhibition Test (효소 저해법을 이용한 Carbamate계 농약의 다성분 잔류분석법 개발)

  • Kim, Jung-Ho
    • Journal of Environmental Science International
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    • v.17 no.12
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    • pp.1325-1330
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    • 2008
  • This study was carried out with the detection for multiresidue of the carbamate pesticide such as carbaryl and cabofuran by enzyme-inhibition method. The check time for determination of acetylcholinesterase(AChE) activity was selected at 60 sec. The AChE activity in chicken brain determined by the Ellman's method was $162{\mu}$mol/min/g protein. $I_{50}$ for AChE by carbamate pesticide with wet kit was 0.169mg/L of carbaryl and 0.089mg/L of cabofuran, respectively. The incubation time for enzyme kit with substrate kit was 30min for determination of AChE activity. Enzyme kit with substrate kit was stable at $4^{\circ}C\;and\;25^{\circ}C$ for 5 days. Limit detection concentration of carbaryl with dry kit for AChE was 0.05mg/L. The dry kit such as wet kit applied Enzyme-Inhibition(EI) method with AChE was confirmed the multi residue method to detect the carbamate pesticides.

Simultaneous Analysis of Prohibited Antibiotics (Fluoroquinolones) in Seawater and Effluents Released by Aquaculture Using LC-MS/MS (LC-MS/MS를 이용한 해수 및 수산용수 중 플루오로퀴놀론계 항생제 동시 분석법 정립)

  • Mikyoung Lee;In-Seok Lee;Minkyu Choi;Sunggyu Lee;Won-Chan Lee
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.56 no.4
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    • pp.428-437
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    • 2023
  • A simultaneous analytical method was developed and validated for the analysis of prohibited fluoroquinolone (FQ) antibiotics including norfloxacin, ofloxacin, and pefloxacin, released by aquaculture in seawater and effluents. The samples were filtered, and extracts were obtained using a solid phase extraction cartridge with methanol (MeOH). The extracts were concentrated, and analyzed using ultra-performance liquid chromatography-tandem mass spectrometry. Two different columns and four different mobile phases were compared to achieve optimal separation and sensitivity for target compounds. Typical validation parameters including linearity, recovery of surrogate standard, instrument detection limit (IDL), limit of quantification (LOQ), and method detection limit (MDL) were evaluated. The linearity of calibration curves was over 0.999. Recoveries of surrogate ranged from 87.6% to 113%. The LOQ of target compounds was approximately 3-8 times lower than those reported in previous studies. The IDL and MDL were 0.06-0.57 and 0.06-0.37 ng/L, respectively. Seven effluent samples collected from an aquaculture located in Jeju were analyzed; however, not all target compounds were detected in the samples, suggesting that the banned antibiotics were not used. Overall, this established method was able to simultaneously analyze the three FQ antibiotics, and may be useful for monitoring prohibited antibiotics in the fishery industry.

Extraction Characteristics and Quantitational Methods for Total Petroleum Hydrocarbons in Soil

  • Jeon, Chi-Wan;Lee, Jung-Hwa;Song, Kyung-Sun;Lee, Sang-Hak;Lee, Jung-Min
    • Proceedings of the Korean Environmental Sciences Society Conference
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    • 2003.11a
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    • pp.119-122
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    • 2003
  • Quantitation methods of total petroleum hydrocarbons to determinate oil contaminated level in soil were discussed. Extraction characteristics of several pretreatment methods and practical detection limit and reappearances in gas chromatography/mass spectrometry. with each pretreatment method were investigated. The obtained results showed that the newly adopted quantitation method and mechanical shaking extraction method using methanol with extraction solvent are more practical and applicable to real sample than the conventional methods. In applying these methods to gasoline, kerosene, fuel oil which are major source of soil contamination, the practical quantitation limit and % relative standard deviation was able to determine with range of 2.5 - 10 ppm, 5 - 7 %.

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A Study about the Construction of Intelligence Data Base for Micro Defect Evaluation (미소 결함 평가를 위한 지능형 데이터베이스 구축에 관한 연구)

  • 김재열
    • Proceedings of the Korean Society of Machine Tool Engineers Conference
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    • 2000.04a
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    • pp.585-590
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    • 2000
  • Recently, It is gradually raised necessity that thickness of thin film is measured accuracy and managed in industrial circles and medical world. Ultrasonic Signal processing method is likely to become a very powerful method for NDE method of detection of microdefects and thickness measurement of thin film below the limit of Ultrasonic distance resolution in the opaque materials, provides useful information that cannot be obtained by a conventional measuring system. In the present research, considering a thin film below the limit of ultrasonic distance resolution sandwiched between three substances as acoustical analysis model, demonstrated the usefulness of ultrasonic Signal processing technique using information of ultrasonic frequency for NDE of measurements of thin film thickness, sound velocity, and step height, regardless of interference phenomenon. Numeral information was deduced and quantified effective information from the image. Also, pattern recognition of a defected input image was performed by neural network algorithm. Input pattern of various numeral was composed combinationally, and then, it was studied by neural network. Furthermore, possibility of pattern recognition was confirmed on artifical defected input data formed by simulation. Finally, application on unknown input pattern was also examined.

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Development of a Sensitive Bioassay Method for Quorum Sensing Inhibitor Screening Using a Recombinant Agrobacterium tumefaciens

  • Kim Yeon Hee;Kim Young Hee;Kim Jung Sun;Park Sunghoon
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.10 no.4
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    • pp.322-328
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    • 2005
  • Acylhomoserine lactones (AHLs) are known to be the triggering molecules in the quorum sensing mechanism of many gram-negative bacteria. In order to detect AHL inhibitors that are potential biofilm inhibitors, a convenient and sensitive bioassay was developed based on the $\beta$-galactosidase activity ($\beta$-GAL) of a recombinant Agrobacterium tumefaciens strain. A series of commercially available AHLs were tested for inducing $\beta$-GAL at varying concentrations in agar-plate and liquid cultures of the reporter strain. All AHLs tested exhibited a concentration­dependent induction, and octanoyl homoserine lactone (OHL) showed the highest sensitivity with a detection limit of 0.1 nM in the liquid culture assay. When fimbrolide, a known quorum sensing inhibitor, was added, induction of $\beta$-GAL by OHL was repressed. The repression at a constant OHL concentration was dependent on the fimbrolide concentration with the detection limit below 1 ppm, indicating that this assay is a sensitive method for screening AHL inhibitors.

Monitoring of Residual Sulfur Dioxide in Herbal Medicines (유통 한약재의 잔류이산화황에 대한 모니터링)

  • Kim, Mi-Kyeong;Hur, Moon-Hye;Lee, Chang-Hee;Jin, Jong-Seong;Jin, Sun-Kyung;Lee, Young-Ja
    • Korean Journal of Pharmacognosy
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    • v.35 no.4 s.139
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    • pp.276-282
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    • 2004
  • This study has been conducted to investigate the amount of residual sulfur dioxide for herbal medicines of 30 species which are purchased in 13 different regions (Bonghwa, Busan, Chunju, Jecheun, Kwangiu, Keumsan, Seoul, Taeku, Cheungdu, Xian, Beijing, Tokyo and Osaka). The sulfur dioxide residues were determined in the collected 386 samples by the modified Monier-Williams method. The residues of sulfur dioxide in 386 samples ranged from ND (under detection limit) to 2808 ppm. The sulfur dioxide in Cassiae Semon, Cinnamomi Ramulus, Cervi Cornu, Hoelen, Crataegi Fructus, Artemisiae Argyi Herba, Scolopendrae Corpus, Schizandrae Fructus and Cyperi Rhizoma were detected under the detection limit regardless of the collected regions. The sulfur dioxide residues in herbal medicines collected in domestic regions were relatively lower than those in foreign regions. There are no standards for sulfur dioxide residual limits of herbal medicines in Korea. This results will provide the scientific basis for the standardization of sulfur dioxide residues in Korea Pharmacopoeia.

Analysis of Carbonyl Compounds using DNPH Cartridge with LC-MS (DNPH cartridge/LC-MS 방법에 의한 카르보닐화합물 분석에 관한 연구)

  • Cho Deok-Hee;Song Il-Seok
    • Journal of Korean Society for Atmospheric Environment
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    • v.22 no.2
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    • pp.201-208
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    • 2006
  • Several carbonyl compounds are important because of their irritant and toxic properties, mutagenicity and carcinogenicity. Therefore, they are regulated in korean odor emission standard. In this study, atmospheric pressure ionization-mass spectrometry(API-MS) is used for the analysis of carbonyl compounds after derivatization with 2, 4-dinitrophenylhydrazine (DNPH) and liquid chromatographic separation. In the negative ion mode, the $[M-H]^-$ pseudomolecular ions are most abundant for the carbonyls. Analytical parameters such as linearity, repeatability and minimum detection limit were evaluated. The linearities ($r^2$) for carbonyls were $0.9977{\sim}0.9999$ when analyte concentration ranges from $25\;to\;250{\mu}g/L$(n=6). The relative standard deviations (%RSD) for carbonyls were $0.55{\sim}3.51%$ for concentration of $100{\mu}g/L$(n=5). The minimum detection limit (MDL) was $1.88{\mu}g/L$(0.27 ppb) for i-valeraldehyde. It was shown that LC-MS method has a great potential for carbonyl compounds analysis.

Properties and Activitiy Screening of Chromone Derivatives (크로몬 유도체의 물성 및 활성검색)

  • 김영로;이상현;김경순;정춘식;정재훈;김박광
    • YAKHAK HOEJI
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    • v.44 no.2
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    • pp.107-114
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    • 2000
  • We have synthesized 4-isonitroso-4H-1-benzopyran and 4-amino-2,3-dihydro -4H-1-benzopyran of chromone derivatives by using condensation method. Physico-chemical properties of these compounds were measured and analyzed by UV and HPLC method. The correlation coefficient of their methanol solutions by UV were 0.9992 and 0.9994, respectively. And oxime compound was resolved within 4 min and had a detection limit of 3 ng at S/N=3 by HPLC using a reversed phase column with three solvents(MeOH, $H_2O$, HAc). The amino compound was resolved within 4.5 min and had a detection limit of 10 ng at S/N=3 by HPLC under the same conditions. Anti-diabetic effect of chromone derivatives were investigated in the streptozotocin (STZ)-induced diabetic rats. Diabetes was induced in male Sprague-Dawley rats by injections of STZ (45 mg/kg, i.v). The investigation of the hair growth effect of isonitrosobenzopyran and 4-aminobenzopyran on the hair of black mouse (C57BL/6) was also carried out. The administraion of their ethanol solution to the black mouse (C57BU/6) through skin them promoted the growth of hair.

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Rapid Detection for Salmonella spp. by Ultrafast Real-time PCR Assay (Ultrafast Real-time PCR법을 이용한 살모넬라의 신속 검출)

  • Kim, Seok Hwan;Lee, Yu-Si;Joo, In-Sun;Kwak, Hyo Sun;Chung, Gyung Tae;Kim, Soon Han
    • Journal of Food Hygiene and Safety
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    • v.33 no.1
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    • pp.50-57
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    • 2018
  • Salmonella continue to be a major cause of food poisoning worldwide. The rapid detection method of food-borne Salmonella is an important food safety tool. A real-time polymerase chain reaction (PCR) has been used as a rapid method for the detection of pathogens. It has been recently reported that NBS LabChip real-time PCR is a novel, ultrafast, and chip-type-convenient real-time PCR system. We developed the assay method based on NBS LabChip real-time PCR for the rapid detection of Salmonella, which its reaction time was within 20 minutes. Two target genes (invA and stn) were selected to design target specific primers and probes. The new method was validated by checking specificity and sensitivity (limit of detection). This study included forty-two target and twenty-one non-target strains to assess the specificity. This assay was able to identify the 42 Salmonella strains correctly. The limit of detection (LOD) was $10^1copies/{\mu}L$ in Salmonella genomes DNA, while LOD incubated for 4 hr in the inoculated sausage sample ranged from $10^1CFU/g$ to $10^2CFU/g$ as an inoculated cell count. The assay developed in this study could be applied for the investigation of food poisoning pathogens.

Analytical Characteristics of GC/MS and HPLC according to the Concentration Distribution of PAHs (PAHs 농도 분포에 따른 GC/MS와 HPLC의 분석특성에 관한 연구)

  • Hong, Jwa-Ryung;Choi, Kwang-Min
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.25 no.3
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    • pp.312-321
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    • 2015
  • Objectives: The purpose of this study was to determine the best method to analyze PAHs at extremely low concentrations. To this end, 16 PAHswere analyzed simultaneously by GC/MS, HPLC/FLD and HPLC/UVD, and the analytical characteristics of HPLC and GC/MS were compared. Methods: This study was conducted by GC/MS and HPLC/FLD/UVD, and evaluated linearity, precision and detection limit. Standard solutions were prepared for 21 samples in the range of $0.00001{\sim}1.0{\mu}g/mL$ and the samples were divided into four groups. All samples were made in three sets and analysis was replicated seven times. Results: Sixteen PAHs could be simultaneously separated by HPLC and GC/MS, and the adequate equipment was HPLC/FLD. The retention times by HPLC were shorter than GC/MS, and HPLC had better separation for most PAHs than GC/MS. The peaks of naphthalene and naphthalene-D8 partially overlapped for GC/MS. HPLC/FLD had a 20-2000 times lower limit of detection than GC/MS and UVD. However FLD was not adequate for analyzing acenaphthylene because it has too low a fluorescence quantum yield to be detected. The precision of HPLC/FLD/UVD and GC/MS showed less than 20% at $0.001{\mu}g/mL$ PAHs and when the concentration was higher, the coefficient of variation was decreased. HPLC/FLD was better for the overall detection of limits. Conclusions: The results indicate that the HPLC/FLD method has good linear range, precision and a detection of limits from $0.00001{\sim}0.0001{\mu}g/mL$ for all 16 PAHs. This study contributes to providing useful data for analysis technology and can be applied to occupational exposure measurement for PAHs in workplaces.