• Title/Summary/Keyword: method detection limit

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K+ Ion-Selective PVC Membrane Electrodes with Neutral Carriers (중성운반체를 이용한 K+ 이온선택성 PVC막 전극)

  • Kim, Yong-Ryul;Cho, Kyoung-Sub;Kang, An-Soo
    • Applied Chemistry for Engineering
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    • v.9 no.5
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    • pp.734-741
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    • 1998
  • Electrode characteristics were studied in the interface between sample solutions and $K^+$ ion selective PVC membrane electrodes containing neutral carriers, dibenzo-18-crown-6(D18Cr6) and valinomycin(Val). The effect of doping of base electrolytes, the chemical structure and the content of carrier, variation of plasticizer, membrane thickness, and concentration variation of sample solution on the response characteristics of electrode such as the measured Nernstian slope, the detection limit, the linear response range, and potentiometric selectivity coefficients, were studied. In order to synthesize the membrane D18Cr6 and Val as neutral carriers were used, and complex between the carrier and $K^+$ ions were used as active materials. PVC membrane electrodes were made of plasticizers (DBP, DOS, and DBS), the base electrolyte[potassium tetraphenylborate(KTPB)], and solvent(THF). The chemical structure of carrier D18Cr6 was best for electrode and ideal electrode characteristics were appeared especially in case of doping of TPB. The optimum carrier content was about 3.23 wt % in case of D18Cr6 and Val. DBP was best as a plasticizer. As membrane thickness decreased the electrode characteristics was improved. But its characteristics were lowered below the optimum membrane thickness because of the elution of carrier, deterioration of membrane strength, etc. In the case of D18Cr6, the selectivity coefficients by the mixed solution method for the $K^+$ ion were in the order of $NH_4{^+}>Ca^{2+}>Mg^{2+}>Na^+$.

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Detection and Monitoring of Benzylpenicillin Residues in Livestock and Marine Products (유통 축·수산물 중 잔류벤질페니실린의 검출 및 모니터링)

  • Lee, Hyo Jeong;Kang, Young Won;Lee, Soo Min;An, Kyung A;Lee, Ryun Kyung;Seo, Sang Cheol;Lee, Ju Hee;Im, Moo Hyeog;Lee, Jeong Rim;Hong, Choong Man;Chang, Moon Ik;Cho, Yoon Jae
    • Korean Journal of Food Science and Technology
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    • v.46 no.3
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    • pp.288-294
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    • 2014
  • Penicillin and its salts, including the benzatine, procaine, and sodium salts, have been widely used in human and veterinary medicine. Owing to their low toxicity, they currently form the most important group of antibiotics. However, overdose and abuse of these antibiotics may lead to potential risk in human health. Therefore, this study was conducted to validate the analysis method established by the Korea Food Code in 2012 and to monitor the levels of benzylpenicillin residues in products with reference to the maximum residue level (MRL). Of the 232 product samples tested, benzylpenicillin was detected in 11 livestock products and 2 marine products. Benzylpenicillin concentrations were found to be lower than the MRL in 12 products; however, the concentration of benzylpenicillin was found to be greater than the MRL in 1 pork product. The limit of quantification (LOQ) for benzylpenicillin was found to be 0.001-0.002 mg/kg, with an average recovery of 90.4-115.3%. Calibrations showed good linearity of 0.995 over a range of 0.002-0.05 mg/kg.

Determination of Additives Content in Aviation Turbine Fuel Using Multi-dimensional GC-MS (Multi-dimensional GC-MS를 이용한 항공터빈유의 첨가제 분석)

  • Youn, Ju Min;Jang, Yoon Mi;Yim, Eui Soon;Kim, Seong Lyong;Kang, Yong
    • Journal of the Korean Applied Science and Technology
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    • v.35 no.4
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    • pp.1260-1268
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    • 2018
  • To improve fuel performance and specific characteristics of long storage and moving through fuel systems additives should be added in kerosene type aviation turbine fuel (AVTUR) such as antioxidant, fuel system icing inhibitor (FSII), electric conductivity improvers and so on. The dosage of additives has to be analyzed qualitatively and quantitatively due to inspect the quality of abnormal fuel and distinguish other petroleum products. Multi-dimensional GC-MS (MDGC-MS) with Deans switching technique are applied the determination of antioxidant and FSII, which are added with AVTUR containing complex mixture of hydrocarbons. Antioxidant and FSII in the range of 2.5-20 mg/L was quantitatively and qualitatively analyzed using MDGC-MS and the detection limit was about twice as low as that of the 1-dimensional GC-MS results. The method in this study has been higher peak resolution compared with GC-MS and could be simultaneously analyzed different two additives without sample pre-treatment.

A Study on Experimental Prediction of Landslide in Korea Granite Weathered Soil using Scaled-down Model Test (축소모형 실험을 통한 국내 화강암 풍화토의 산사태 예측 실험 연구)

  • Son, In-Hwan;Oh, Yong-Thak;Lee, Su-Gon
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.6
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    • pp.439-447
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    • 2019
  • In this study, experiments were conducted to establish appropriate measures for slopes with high risk of collapse and to obtain results for minimizing slope collapse damage by detecting the micro-displacement of soil in advance by installing a laser sensor and a vibration sensor in the landslide reduction model experiment. Also, the behavior characteristics of the soil layer due to rainfall and moisture ratio changes such as pore water pressure and moisture were analyzed through a landslide reduction model experiment. The artificial slope was created using granite weathering soil, and the resulting water ratio(water pressure, water) changes were measured at different rainfall conditions of 200mm/hr and 400mm/hr. Laser sensors and vibration sensors were applied to analyze the surface displacement, and the displacement time were compared with each other by video analysis. Experiments have shown that higher rainfall intensity takes shorter time to reach the limit, and increase in the pore water pressure takes shorter time as well. Although the landslide model test does not fully reflect the site conditions, measurements of the time of detection of displacement generation using vibration sensors show that the timing of collapse is faster than the method using laser sensors. If ground displacement measurements using sensors are continuously carried out in preparation for landslides, it is considered highly likely to be utilized as basic data for predicting slope collapse, reducing damage, and activating the measurement industry.

A Survey on the Residual Pesticides on Agricultural Products on the Markets in Incheon from 2016 to 2018 (인천광역시 유통 농산물의 최근 3년간 잔류농약 실태조사)

  • Park, Jeong-Eun;Lee, Mi-Yeon;Kim, Sun-Hoi;Song, Sung-Min;Park, Byung-Kyu;Seo, Soon-Jae;Song, Jae-Yong;Hur, Myong-Je
    • Korean Journal of Environmental Agriculture
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    • v.38 no.3
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    • pp.205-212
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    • 2019
  • BACKGROUND: This survey conducted on agricultural products in Incheon for the past three years from 2016 to 2018 to detect residual pesticides and to monitor the use of pesticides. METHODS AND RESULTS: Residual pesticides were analyzed for a total of 5,937 agricultural products in Samsan wholesale market, traditional market and large retailers in Incheon. Samples were analyzed by multi class pesticide method using GC-MS/MS, LC-MS/MS, GC-ECD/NPD, and UHPLC. In 59 cases (1.0%) residual pesticides were detected improperly and these cases exceeded maximum residue limits (MRLs). CONCLUSION: The ratios of violative agricultural products were similar each year at approximately 1.0% per year, but the residual pesticide detection rates with the limit included in the samples were shown to be gradually decreasing to 17.9%, 12.6%, and 11.2% annually. The frequency of violative residual pesticides was high in order of Diazinon, Chlorpyrifos, Iprodione, etc. Residual pesticide monitoring might be needed in the future continuously, as violations in agricultural products distributed in Incheon are shown at a similar level every year.

Immobilization of As and Pb in Contaminated Soil Using Bead Type Amendment Prepared by Iron NanoparticlesImpregnated Biochar (철 나노 입자가 담지된 바이오차 기반 비드 형태 안정화제를 이용한 비소 및 납 오염토양의 안정화)

  • Choi, Yu-Lim;Kim, Dong-Su;Kang, Tae-Jun;Yang, Jae-Kyu;Chang, Yoon-Young
    • Journal of Environmental Impact Assessment
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    • v.30 no.4
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    • pp.247-257
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    • 2021
  • In this work, Iron Nano-Particles Impregnated BioChar/bead (INPBC/bead) soil amendment was developed to increase biochar's reactivity to As in soil and preventing possible wind loss. Prior to preparation of INPBC/bead, INPBC was produced utilizing lignocellulosic biomass and Fe(III) solution in a hydrothermal method, followed by a calcination process. Then, the bead type amendment, INPBC/bead was produced by cross-linking reaction of alginate with INPBC. FT-IR, XRD, BET, and SEM-EDS analyses were utilized to characterize the as-synthesised materials. The particle size range of INPBC/bead was 1-4 mm, and different oxygen-containing functional groups and Fe3O4 crystalline phase were produced on the surface of INPBC/bead, according to the characterization results. The soil cultivation test was carried out in order to assess the stabilization performance of INPBC/bead utilizing As and Pb-contaminated soil obtained from an abandoned mining location in South Korea. After 4 weeks of culture, TCLP and SPLP extraction tests were performed to assess the stabilization efficacy of the amendment. The TCLP and SPLP findings revealed that raising the application ratio improved stabilizing efficiency. The As stabilization efficiency was determined to be 81.56 % based on SPLP test findings for a 5% in (w/w) INPBC/bead treatment, and the content of Pb in extracts was reduced to the limit of detection. According to the findings of this study, INPBC/bead that can maintain pH of origin soil and minimize wind loss might be a potential amendment for soil polluted with As and heavy metals.

TLC, HPTLC FINGERPRINTING AND ACUTE ORAL TOXICITY EVALUATION OF HABB-E-AZARAQI: A NUX-VOMICA-BASED TRADITIONAL UNANI FORMULATION

  • Ara, Shabnam Anjum;Viquar, Uzma;Zakir, Mohammed;Husain, Gulam Mohammed;Naikodi, Mohammed Abdul Rasheed;Urooj, Mohd;Kazmi, Munawwar Husain
    • CELLMED
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    • v.11 no.3
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    • pp.13.1-13.9
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    • 2021
  • Background and Objective: Nux-vomica based traditional Unani formulation, Habb-e-Azaraqi (HAZ) is an important drug used by Unani physicians since several decades. It possesses Muqawwi-i-A'sab (nervine tonic), Muharrik-i-A'sab (nervine stimulant) properties and is an effective treatment option for diseases like Laqwa (facial palsy), Falij (paralysis), Niqris (gout) and Waja'al-Mafasil (arthritis) etc. The aim of the study is to access and provide information of HAZ for its TLC, HPTLC Fingerprinting defining its clear qualitative perspective and acute oral toxicity evaluation for its safety assessment which was not done earlier, thus contributing in the field of research. Materials and Methods: The chief ingredient, nux-vomica was detoxified as per method mentioned in Unani Pharmacopeia before its use in formulation. TLC and HPTLC was developed under four detection system i.e., UV 366nm, UV 254nm, exposure to iodine vapours and after derivatization with anisaldehyde sulphuric acid. Acute toxicity studies were performed as per OECD Guidelines 425 at a limit dose of 2000 mg/kg. Observations were done for signs of toxicity, body weight, and feed consumption at regular intervals followed by haematological and biochemistry evaluation. Results: The generated data proved the authenticity and established the TLC and HPTLC profile of the formulation. Acute toxicity revealed no significant differences in HAZ-treated animals with respect to body weight gain, feed consumption, haematology, clinical biochemistry evaluation. No significant gross pathological observation was noticed in necropsy. Conclusion: Data of the present study is substantial and scientific proof of HAZ in terms of standardization and toxicity study that can be utilize in future research activities.

Analysis of malachite green and leuco-malachite green in sea food (수산식품 중 말라카이트그린 및 류코말라카이트그린의 분석)

  • Choi, Dongmi;Hong, Soongun;Im, Moohyeog;Jeong, Jiyoon;Chang, Moonik;Park, Kunsang;Hong, Mooki;Woo, Gunjo
    • Analytical Science and Technology
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    • v.19 no.2
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    • pp.142-148
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    • 2006
  • To determine malachite green and leuco-malachite green residues in sea food, a liquid chromatographic method has been optimized. The target compounds were extracted in the homogenized edible tissues with a mixture of McIlvaine buffer-acetonitrile and partitioned against dichloromethane. After concentrating the lower layer, the resulting residues were re-dissolved in methanol and analyzed by the HPLC with visible detector at 620 nm using acetonitrile-acetate buffer. For the analysis of leuco-malachite green with malachite green simultaneously, post-column packed with lead(IV) oxide was used for oxidizing leuco-malachite green to malachite green. The correlation coefficients($r^2$) was 0.9989 for malachite green, and 0.9995 for leuco-malachite green. The limit of detection was 0.005 mg/kg for the combined of malachite green and leuco-malachite green at signal/noise${\geq}3$. The recovery rate was within a reliable range of 84~98% (CV 3~16%). Leuco-malachite green were detected in carp and crusian carp.

Determination of fluoride in fluorite mine wastewater by ion chromatography with post-wash technique (후세척-이온크로마토그래피를 이용한 형석 광산 폐수 중 플루오라이드 정량)

  • Song, Kyung-Sun;Eum, Chul-Hun;Kim, Sang-Yeon
    • Analytical Science and Technology
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    • v.19 no.5
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    • pp.383-388
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    • 2006
  • Simple post-wash method by ion chromatography (IC) was established for the rapid and precise determination of fluoride ion in wastewater from mine in fluorite mineralized area. High sulfate in sample was retained in a pre-column and less strongly held fluoride ion was transferred to the principal separation system using modified conventional IC with switching technique. An analytical column with high capacity (AS 9 HC) was used as a pre-column to retain the amount of high sulfate. A guard column (AG 14) as a separation column was used to increase the response of fluoride and reduce the system pressure. According to the recovery of fluoride ion with one detector and the observation of sulfate peak with another conductivity detector, the optimum switching time of 10-port chromatographic injector was 4.3 min. The limit of detection (S/N = 3) of fluoride in synthetic solution containing $500mg\;L^{-1}$ sulfate was $2.4{\mu}g/L$, with $25{\mu}L$ sample volume.

Levels of sulfonamides for animals in food (식품 중 설폰아마이드계 동물용의약품의 잔류실태)

  • Jeong, Jiyoon;Hong, Mooki;Choi, Dongmi
    • Analytical Science and Technology
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    • v.20 no.1
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    • pp.84-90
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    • 2007
  • To determine levels of 11 sulfonamides for animals in food, simultaneously, a selective method of high performance liquid chromatography with UV detector has been applied. The targets were sulfachlorpyridazine (SCP), sulfadiazine (SDZ), sulfadimethoxine (SDM), sulfisoxazole (SSX), sulfamerazine (SMZ), sulfamethazine (SMT), sulfamethoxazole (SMX), sulfamethoxypyridazine (SMP), sulfamonomethoxine (SMM), sulfaquinoxaline (SQX) and sulfathiazole (STZ). Food samples were beef, pork, chicken, milk and whole egg that were collected at the main 6 cities in Korea as Seoul, Busan, Daejon, Incheon, Mokpo and Gangneung. After homogenizing food samples with sodium phosphate solution and acetonitrile, it was extracted with n-hexane. The mobile phase gradient was a mixture of 5 mM potassium phosphate (pH 3.25) and methanol with a gradient ratio from 100:0 to 30:70. The UV wavelength was 270 nm. The overall recoveries were ranged from 75% to 95% and the limit of detection was minimum 0.004 mg/kg for SMT, and 0.007 mg/kg for STZ at signal/noise > 3, respectively. As results, sulfonamide drugs were not detected in most of the selected food samples, however, sulfamonomethoxine was detected in meat. The determined level of sulfamonomethoxine were 0.03 and 0.06 mg/kg for beef that were below the MRLs.