• Analytical Science and Technology
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• v.26 no.3
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• pp.174-181
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• 2013

Pyrifluquinazon is classified with a quinazoline insecticide that regulates food intake by controling the feeding behavior acting on the endocrine or nervous system of pests such as aphids and white fly. To keep safety on pyrifluquinazon residues in agricultural commodities a simple, accurate and rapid analytical method was developed and validated using high performance liquid chromatograph (HPLC-UVD). The pyrifluquinazon residues acidified with 1% formic acid in samples were extracted with acetonitrile and partitioned with hexane subsequently to dichloromethane then purified with silica solid phase extraction (SPE) cartridge. The purified samples were detected using HPLC-UVD. The method was validated using apple and pear spiked with pyrifluquinazon at 0.02, 0.05 and 0.1 mg/kg and hulled rice, pepper, soybean at 0.05 and 0.1 mg/kg. Average recoveries were 70.5~107.9% with relative standard deviation less than 10%. The result of recoveries and overall coefficient of variation of a laboratory results in Gwangju regional FDA and Daejeon regional FDA was followed with Codex guideline (CODEX CAC/GL 40). This method is appropriated at pyrifluquinazon residues determination and will be used as official method of analysis.

• Korean Journal of Environmental Agriculture
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• v.42 no.1
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• pp.71-81
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• 2023

An accurate and easy-to-use analytical method for determining isocycloseram and its metabolites (SYN549431 and SYN548569) residue is necessary in various food matrixes. Additionally, this method should satisfy domestic and international guidelines (Ministry of Food and Drug Safety and Codex Alimentarius Commission CAC/GL 40). Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) was used to determine the isocycloseram and its metabolites residue in foods. To determine the residue and its metabolites, a sample was extracted with 20 mL of 0.1% formic acid in acetonitrile, 4 g magnesium sulfate anhydrous and 1 g sodium chloride and centrifuged (4,700 G, 10 min, 4℃). To remove the interferences and moisture, d-SPE cartridge was performed before LC-MS/MS analysis with C₁₈ column. To verify the method, a total of five agricultural commodities (hulled rice, potato, soybean, mandarin, and red pepper) were used as a representative group. The matrix-matched calibration curves were confirmed with coefficients of determination (R²) ≥ 0.99 at a calibration range of 0.001-0.05 mg/kg. The limits of detection and quantification were 0.003 and 0.01 mg/kg, respectively. Mean average recoveries were 71.5-109.8% and precision was less than 10% for all five samples. In addition, inter-laboratory validation testing revealed that average recovery was 75.4-107.0% and the coefficient of variation (CV) was below 19.4%. The method is suitable for MFDS, CODEX, and EU guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

• Journal of Food Hygiene and Safety
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• v.31 no.6
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• pp.432-438
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• 2016

Ethoxyquin (EQ, 1,2-dihydro-6-ethoxy-2,2,4-trimethyl-quinoline) is quinoline-based antioxidant used in the animal feed and food industry to protect the raw materials and final products against oxidation. In recent years the use of synthetic antioxidants in fishmeal ingredients carry-over to farmed fish fillets has received increasing attention in food safety. This study was conducted to develop an analytical method to determine EQ in aquatic products. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with 1 N HCl (in case of flatfish extracted with 1 N HCl containing 10% acetonitrile). Then, solid phase extraction (SPE) was used for the cleanup. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.99, analyzed at 0.005-0.2 mg/kg concentration. The developed method was validated according to the Codex Alimentarius Commission (CAC) guideline. The limits of quantitation for EQ were 0.01 mg/kg. Average recoveries ranged from 81.3% to 107%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was below 10%. The analytical method was characterized with high accuracy and acceptable sensitivity to meet CODEX guideline requirements and would be applicable to analyze the EQ residue in aquatic products.

• Computers and Concrete
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• v.14 no.5
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• pp.599-612
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• 2014

This paper presents the effects of the construction stages using time dependent material properties on the structural behaviour of concrete arch dams. For this purpose, a double curvature Type-5 arch dam suggested in "Arch Dams" symposium in England in 1968 is selected as a numerical example. Finite element models of Type-5 arch dam are modelled using SAP2000 program. Geometric nonlinearity is taken into consideration in the construction stage analysis using P-Delta plus large displacement criterion. In addition, the time dependent material strength variations and geometric variations are included in the analysis. Elasticity modulus, creep and shrinkage are computed for different stages of the construction process. In the construction stage analyses, a total of 64 construction stages are included. Each stage has generally $6000m^3$ concrete volume. Total duration is taken into account as 1280 days. Maximum total step and maximum iteration for each step are selected as 200 and 50, respectively. The structural behaviour of the arch dam at different construction stages has been examined. Two different finite element analyses cases are performed. In the first case, construction stages using time dependent material properties are considered. In the second case, only linear static analysis (not considered construction stages) is taken into account. Variation of the displacements and stresses are obtained from the both analyses. It is highlighted that construction stage analysis using time dependent material strength variations and geometric variations has an important effect on the structural behaviour of arch dams. The maximum longitudinal, transverse and vertical displacements obtained from construction stages and static analyses are 1.35 mm and 0 mm; -8.44 and 6.68 mm; -4.00 and -9.90 mm, respectively. In addition, vertical displacements increase from the base to crest of the dam for both analyses. The maximum S11, S22 and S33 stresses are obtained as 1.60MPa and 2.84MPa; 1.39MPa and 2.43MPa; 0.60MPa and 0.50MPa, respectively. The differences between maximum longitudinal, transverse, and vertical stresses obtained from construction stage and static analyses are 78%, 75%, and %17, respectively. On the other hand, there is averagely 12% difference between minimum stresses for all three directions.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.124-134
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• 2019

An analytical method was developed for the determination of broflanilide and its metabolites in agricultural products. Sample preparation was conducted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and LC-MS/MS (liquid chromatograph-tandem mass spectrometer). The analytes were extracted with acetonitrile and cleaned up using d-SPE (dispersive solid phase extraction) sorbents such as anhydrous magnesium sulfate, primary secondary amine (PSA) and octadecyl ($C_{18}$). The limit of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The recovery results for broflanilide, DM-8007 and S(PFP-OH)-8007 ranged between 90.7 to 113.7%, 88.2 to 109.7% and 79.8 to 97.8% at different concentration levels (LOQ, 10LOQ, 50LOQ) with relative standard deviation (RSD) less than 8.8%. The inter-laboratory study recovery results for broflanilide and DM-8007 and S (PFP-OH)-8007 ranged between 86.3 to 109.1%, 87.8 to 109.7% and 78.8 to 102.1%, and RSD values were also below 21%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food and Drug Safety Evaluation guidelines (2016). Therefore, the proposed analytical method was accurate, effective and sensitive for broflanilide determination in agricultural commodities.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.227-234
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• 2019

An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.

• Computers and Concrete
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• v.22 no.3
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• pp.337-353
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• 2018

The present study focuses on examining the structural behaviour of steel-fibre-reinforced concrete (SFRC) beams under high rates of loading largely associated with impact problems. Fibres are added to the concrete mix to enhance ductility and energy absorption, which is important for impact-resistant design. A simple, yet practical non-linear finite-element analysis (NLFEA) model was used in the present study. Experimental static and impact tests were also carried out on beams spanning 1.3 meter with weights dropped from heights of 1.5 m and 2.5 m, respectively. The numerical model realistically describes the fully-brittle tensile behaviour of plain concrete as well as the contribution of steel fibres to the post-cracking response (the latter was allowed for by conveniently adjusting the constitutive relations for plain concrete, mainly in uniaxial tension). Suitable material relations (describing compression, tension and shear) were selected for SFRC and incorporated into ABAQUS software Brittle Cracking concrete model. A more complex model (i.e., the Damaged Plasticity concrete model in ABAQUS) was also considered and it was found that the seemingly simple (but fundamental) Brittle Cracking model yielded reliable results. Published data obtained from drop-weight experimental tests on RC and SFRC beams indicates that there is an increase in the maximum load recorded (compared to the corresponding static one) and a reduction in the portion of the beam span reacting to the impact load. However, there is considerable scatter and the specimens were often tested to complete destruction and thus yielding post-failure characteristics of little design value and making it difficult to pinpoint the actual load-carrying capacity and identify the associated true ultimate limit state (ULS). To address this, dynamic NLFEA was employed and the impact load applied was reduced gradually and applied in pulses to pinpoint the actual failure point. Different case studies were considered covering impact loading responses at both the material and structural levels as well as comparisons between RC and SFRC specimens. Steel fibres were found to increase the load-carrying capacity and deformability by offering better control over the cracking process concrete undergoes and allowing the impact energy to be absorbed more effectively compared to conventional RC members. This is useful for impact-resistant design of SFRC beams.

• Korean Journal of Environmental Agriculture
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• v.28 no.3
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• pp.310-325
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• 2009

Veterinary drugs have been used to prevent livestock diseases for many years. In spite of having advantages, sometimes indiscriminate application, overdose and abuse may cause risk for human. Therefore, management and risk assessment of veterinary drugs become essential to ensure food safety. So the National Veterinary Research & Quarantine Service (NVRQS) impose on registration for use of veterinary drugs also Korea Food and Drug Administration (KFDA) fixed the maximum residue limits (MRLs) for veterinary drugs in food. Basically, KFDA set MRLs based on the veterinary drugs residual data. Moreover, KFDA estimates the theoretical maximum daily intake (TMDI) with food consumption data and population mean body weight. Recently, 116 veterinary drug MRLs including banned veterinary drugs have been established and other 32 veterinary drugs MRLs will be established within 2009. In 2010, MRLs among antibiotics and synthetic antibacterial agents in livestock fishery products (including milk and eggs) and honey (including royal jelly and propolis) which have not been set in Korea Food Code and Codex Alimentarius Commission (CAC) will be regulated as uniform limit (0.03 mg/kg). In future, veterinary drugs will be controlled strictly to strengthen public health by improving analytical method.

• Journal of Information Management
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• v.8 no.5
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• pp.130-140
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• 1975

이용자(利用者) 중심(中心)의 대화방식(對話方式) 시스팀을 개발(開發)하고 시험(試驗)하였다. 2년(年)동안 280개의 프로파일로 CA - Condensates 데이터 베이스내에서 정보(情報)를 검색(檢索)해 보았다. 그 시스팀의 작업능률(作業能率)을 사용(使用)한 데이터 베이스와 하드웨어의 구조(構造), 소프트웨어 패키지, 이용자(利用者)의 수(數), 그리고 정보(情報)센터에서 제공(提供)한 보조(補助)에 따라 평가(評價)하였다. 대화식(對話式) 검색방법(檢索方法)이나 이용자(利用者)의 요구(要求)를 양화(量化)하는 것, 그리고 여러가지 분야별(分野別)로 검색(檢索)하는 방법(方法) 등 이용자(利用者)의 요구(要求)를 보다 충실(充實)하게 만족(滿足)시킬 수 있는 여러가지 방법(方法)들을 논의(論議)하였다. 모든 정보(情報)시스팀의 목적(目的)은 적시(適時)에 올바른 정(情)보를 적자(適者)에게 제공(提供)하는 것이라고 잘 알려져 있다. 다시 말해서, 정보(情報)시스팀의 주요목적(主要目的)은 이용자(利用者)의 요구(要求)를 충족(充足)시켜 주는 것이다. 이러한 관념(觀念)의 변화(變化)는 정보처리(情報處理)에 큰 변화(變化)를 가져와 정보(情報)시스팀의 적응성(適應性)을 증가(增加)시키기 위해 여러 가지 새로운 방법(方法)들이 개발(開發)되었다. 정보(情報)시스팀들 사이의 상호작용(相互作用), 사람과 컴퓨터와의 대화(對話), 그리고 컴퓨터의 조력(助力)으로 이용자(利用者)의 프로파일을 작성(作成)하는 것 등은 이용자(利用者)의 요구(要求)를 존중(尊重)하고, 필요(必要)한 정보(情報)를 쉽게 찾기 위해서 고안(考案)된 것이다. 한편, 우리들은 이용자(利用者)의 특성(特性)이나 배경(背景), 그리고 문헌(文獻)에 대한 그의 습성(習性) 등에 대해서 얼마나 모르고 있는가를 깨닫게 된다. 상기(上記)의 내용(內容)을 요약(要略)하면, 근대정보(近代情報) 시스팀은 다음의 필요조건(必要條件)을 만족(滿足)해야 한다. 1) 이용자(利用者)의 요구(要求)에 호응(呼應)하기 위해서 적합(適合)한 일련(一連)의 정보(情報)를 제공(提供)해야 한다. 2) 이용자(利用者)와의 관계(關系)에서 시스팀은 적극적(積極的)이어야 한다. 즉, 프로파일 검색공식(檢索公式)에서 유발(誘發)되는 잘못을 지시(指示)하고 지적(指適)할 수 있어 야 한다. 나아가서 컴퓨터의 조력(助力)으로 프로파일을 작성(作成)하고 쉽게 수정(修正)할 수 있는 바람직하다. 우리들은 상기(上記)한 필수조건(必須條件)에 일치(一致)하도록 노력(努力) 하고 Bratislava에 위치(位置)하고 있는 슬로박 과학원(科學院)의 무기화학연구소(無機化學硏究所)와 화학공업경제연구소(化學工業經濟硏究所)가 공동(共同)으로 개발(開發)한 시스팀이 상기(上記)의 특수성(特殊性) 최소(最少)한 몇가지 도입(導入)하였다. 시스팀은 CACS라는 작업명하(作業名下)에서 운영(運營)되었다. 대략 15개월동안 280여개의 프로파일로 CA- Condensates 데이터베이스에서 정보(情報)를 검색(檢索)하여 이용자(利用者)들에게 최신정보(最新情報) 주지사업(周知事業)을 해 보았다. 우리들은 시스팀의 작업능률(作業能率)을 평가(評價)하고 이용자(利用者)의 요구(要求)를 만족(滿足)시키는 최선(最善)의 방법(方法)을 모색(摸索)하였다. 우선 이용자(利用者)와 시스팀사이를 밀접(密接)하게 연결(連結)하는데 중점(重點)을 두었다. 작업능률(作業能率Z)을 분석(分折)해 보고 우리들은 효율(效率)에 영향(影響)을 주는 인자(因子)는 다음의 4가지 주요분류(主要分類)에 속한다는 결론(結論)을 얻었다. (1) 검색(檢索)하는 데이터 베이스 (2) 情報시스팀, 소프트웨어 패키지 그리고 하드웨어 구조(構造) (3) 이용자(利用者)의 특성(特性)과 그의 요구(要求) (4) 정보(情報)센터가 이용자(利用者)에게 제공(提供)하는 보조(補助)

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.22-29
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• 2019

Validamycin A is an aminoglycoside fungicide produced by Streptomyces hygroscopicus that inhibits trehalase. The purpose of this study was to develop a method for detecting validamycin A in agricultural samples to establish MRL values for use in Korea. The validamycin A residues in samples were extracted using methanol/water (50/50, v/v) and purified with a hydrophilic-lipophilic balance (HLB) cartridges. The analyte was quantified and confirmed by liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~0.5 ng) into a blank extract with $R^2$ > 0.99. The limits of detection and quantification were 0.005 and 0.01 mg/kg, respectively. For validation validamycin A, recovery studies were carried out three different concentration levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) with five replicates at each level. The average recovery range was from 72.5~118.3%, with relative standard deviation (RSD) less than 10.3%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the NIFDS (National Institute of Food and Drug Safety) guideline (2016). Therefore, the proposed analytical method is accurate, effective and sensitive for validamycin A determination in agricultural commodities.