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04 포스터 발표 : 환경 화학 분야(PC) ; PC-15 : GC-μECD를 이용한 상추중 Metrafenone과 Boscalid분석을 위한 QuEChERS방법 비교
임소정 ( So Jeong Im ),무스픽 ( Md. Musfiqur Rahman ),김성우 ( Sung Woo Kim ),압두 ( A. M. Abd El-aty ),최정희 ( Jeong Heui Choi ),카빌 ( Md. Humayun Kabir ),팔하 ( Waziha Farha ),정다이 ( Da I Jung ),이영준 ( Young Jun Lee 한국환경농학회 2015 한국환경농학회 학술대회집 Vol.2015 No.-
Three versions of the QuEChERS method (quick,easy, cheap, effective, rugged and safe) . the original (unbuffered), modified acetate-buffered, and citrate-buffered versions were compared for thedetermination of metrafenone and boscalid residues in lettuce via gas chromatography-micro electron capture detector (GC-μECD). Onlymodified acetate-buffered version provided acceptable and more consistent recoveries for both of the target analytes than the other versions. Matrix matched calibration curves prepared for the analytes provided good linearity over the calibration ranges with the co-efficient of determination (r2) ≥ 0.998. Limit of detection (LOD) and quantification (LOQ) were 0.003 and 0.01 mg/kg for both of the analytes. Method was validated in triplicate at two fortification level and recovery of modified acetate buffered version was ranges between 77.0 and 88.1% with relative standard deviation (RSD) < 5 for the quantified analytes. The developed method was applied to the field incurred lettuce sample where half-life of metrafenone and boscalid were found 2.6 and 2.9 days respectively for double doses and 3.4 and 3.6 days respectively for triple doses.
04 포스터 발표 : 환경 화학 분야(PC) ; PC-14 : LC-MS/MS를 이용한 돼지, 닭고기, 계란중 Phorate와 대사체의 분석법 개발
무스픽 ( Md. Musfiqur Rahman ),김성우 ( Sung Woo Kim ),최정희 ( Jeong Heui Choi ),이영준 ( Young Jun Lee ),압두 ( A. M. Abd El-aty ),팔하 ( Waziha Farha ),정다이 ( Da I Jung ),카빌 ( Md. Humayun Kabir ),임소정 ( So Jeong Im 한국환경농학회 2015 한국환경농학회 학술대회집 Vol.2015 No.-
An analytical method was validated for phorate and its five metabolites (phoratesulfone, phoratesulfoxide, phorateoxon, phorateoxonsulfone, and phorateoxonsulfoxide) in pork, chicken, and egg using LC-MS/MS. The method was validated following MFDS (ministry of food and drug safety, Republic of Korea) official method developed for beef and milk. Extraction was carried out following QuEChERS using acidified acetonitrile and salt and purification was conducted via dSPE using primary secondary amine (PSA) and C18 sorbent. Calibration curve in matrix was linear with determination coefficient (r2) ≥ 0.995 for all of the analyte in three target matrices. Limit of detection (LOD) and quantification (LOQ) were 0.001 and 0.004 mg/kg for all of the matrices. Recovery was performed at three fortification level resulted acceptable values ranging from 74.22 and 119.89% with relative standard deviation (RSD)<6%. The developed method can be applied for routine analysis of phorate and its metabolites in different animal origin.
구두발표(OC)-농업화학 및 생태,식품분야 : LC-MS/MS를 이용한 녹차 중 디노테퓨란과 대사체 분석
무쉬픽 ( Musfiqur Rahman ),최정희 ( Jeong Heui Choi ),김성우 ( Sung Woo Kim ),임소정 ( So Jeong Im ),정다이 ( Da I Jung ),압두 ( Abd El Aty ),심재한 ( Jae Han Shim ) 한국환경농학회 2014 한국환경농학회 학술대회집 Vol.2014 No.-
A simultaneous analytical method was developed for dinotefuran and its metabolites (MNG, UF, and DN) in green tea using tandem mass spectrometry (LC/MS/MS). Matrix enhancement and suppression effect was observed for all of the analytes where recoveries were varied with these effects. Samples were extracted with QuEChERS extraction solvent acidic acetonitrile (ACN),partitioned with magnesium sulfate (MgSO4) and sodium acetate (NaOAc) and purified with dispersive solid phase extraction procedure (dSPE) using primary secondary amine (PSA) and C18 sorbent. We tried to increase the extraction efficiency by changing solvents and MeOH was found to be the best solvent for extraction of dinotefuran and its polar metabolites but due to having limitation to apply MeOH as a QuEChERS solvent for lacking of appropriate partitioning salt, ACN was selected as an extraction solvent. Recovery of DN was found < 70% when compared with matrix matched calibration, whereas it was within the range (70-120%) when compared with solvent calibration for matrix enhancement effect. The opposite situation was observed for MNG and dinotefuran due to matrix suppression effect. The recoveries of UF were consistent in spite of having little suppression effect. Calibration curves were linear over the calibration ranges for all the analytes with R2 ≥ 0.994. Limits of detection ranged from 0.0012 - 0.015 mg kg.1, whereas the limits of quantitation were 0.004 - 0.05 mg kg.1 for dinotefuran and its metabolites. The method was successfully applied to real samples, where dinotefuran and all metabolite residues were found in the field-incurred green tea samples.
구두발표(OC)-농업화학 및 생태,식품분야 : OC-02 ; 조리가 고추와 고춧잎 중 pyridaben의 잔류양상 변화에 미치는 영향
김성우 ( Sung Woo Kim ),최정희 ( Jeong Heui Choi ),카빌 ( Humayun Kabir ),팔하 ( Waziha Farha ),무스픽 ( Musfiqur Rahman ),압두 ( Abd El Aty ),심재한 ( Jae Han Shim ) 한국환경농학회 2014 한국환경농학회 학술대회집 Vol.2014 No.-
Peppers are very beneficial crops which include high levels of antioxidants and sufficient in polyphenol, flavonoids, and capsaicinoids. In Republic Korea, peppers have been commonly used as the seasoning for the spicy of korea foods. Pesticides are very important to protect agricultural crops from insect and led to an increase of crop productivity and improvement of crop qualities. However, they may have negative health effects on consumers because of residue properties of them in crops. so it is very essential to control pesticide residues in raw and processed food to protect consumers from health problem resulted from detected pesticide residues. Analysis of pyridaben in samples was carried out using modified original QuEChERS method and LC-MS/MS. The recovery in processed and unprocessed samples ranged from 79.9 .105.1% with relative standard deviations ≤15%. Among different processing methods, blanching after washing (74.4% at single and 82.2% at double dose) was the most effective method to reduce the residual levels of pyridaben in peppers. So, It is recommended to blanch pepper fruits and leaves after washing before eating them for assuring safety of consumers from them.
05 포스터 발표 : 환경 화학 분야(PC) ; PC-03 ; LC/MS/MS를 이용한 현미와 볏짚 중 orthosulfamuron 잔류물 분석
이영준 ( Young Jun Lee ),최정희 ( Jeong Heui Choi ),김성우 ( Sung Woo Kim ),정다이 ( Da I Jung ),임소정 ( So Jeong Im ),무스픽 ( Musfiqur Rahman ),압두 ( Abd El Aty ),심재한 ( Jae Han Shim ) 한국환경농학회 2014 한국환경농학회 학술대회집 Vol.2014 No.-
Rice is one of the most consumed grain in the world because of its nutritional value. Orthosulfamuron, a selective and systemic herbicide, was used to control the post-emergence of annual and perennial broad leaves weeds, sedges, and barnyard grass in rice field. In this study, a modified QuEChERS method was used to extract orthosulfamuron residues from brown rice followed by tandem mass spectrometry. analysis in positive ion electrospray ionisation(ESI+). A determination coefficient ( R2) of > 0.994 was computed from matrix-matched calibration ranges of 0.01 to 2.0 mg/kg. Recoveries at two fortification levels (0.1 and 0.5 mg/kg) were acceptable (88.1 - 100.6%) with relative standard deviations (RSDs)<8%. The limit of quantitation (LOQ), 0.03 mg/kg, was comparatively low compared to the maximum residue limit (MRL = 0.05 mg/kg) set by the Ministry of Food and Drug Safety in the Republic of Korea. The method was successfully applied to field samples and none of the samples contain a residue higher than the limit of detection.
농식품 환경 분야(PF) : PF-15 ; GC/ECD를 이용한 소고기, 닭고기, 우유 중 델타메쓰린 잔류 분석
정다이 ( Da I Jung ),최정희 ( Jeong Heui Choi ),김성우 ( Sung Woo Kim ),임소정 ( So Jeong Im ),이영준 ( Young Jun Lee ),무스픽 ( Musfiqur Rahman ),압두 ( Abd El Aty ),심재한 ( Jae Han Shim ) 한국환경농학회 2014 한국환경농학회 학술대회집 Vol.2014 No.-
In this study, a method was developed to determine deltamethrin residues in beef, chicken, and milk using gas chromatography equipped with electron capture detector. Samples were extracted with acetonitrile and MgSO4 and purified with SPE Florisil cartridge. Performance characteristics, including linearity, quantitation limit (LOQ), precision, and recovery were validated. A matrix-matched calibration was used for quantitation and recoveries obtained at 3 spiking levels; 15, 30, and 60 ㎍/kg, were satisfactory (74.8∼97.9 %). Precision and repeatability presented as relative standard deviation (RSDs) were < 8%. The limits of quantitation (LOQ) were estimated to be 10 ㎍/kg. The developed method was found to be able to determine the analyte with satisfactory intensity and accuracy in incurred samples.
05 포스터 발표 : 환경 화학 분야(PC) ; HPLC-UVD를 이용한 근대 중 아족시스트로빈 분석
팔하 ( Waziha Farha ),무스픽 ( Musfiqur Rahman ),카빌 ( Humayun Kabir ),최정희 ( Jeong Heui Choi ),김성우 ( Sung Woo Kim ),임소정 ( So Jeong Im ),정다이 ( Da I Jung ),압두 ( Abd El Aty ),심재한 ( Jae Han Shim ) 한국환경농학회 2014 한국환경농학회 학술대회집 Vol.2014 No.-
A new method was developed for analysis of Azoxystrobin in chard using HPLC-UVD. Samples were extracted using acetonitrile with salting out and purified usingsolid phase extraction (SPE) procedure. Linearity was excellent with determination coefficient (R2) >0.999. Recovery at 3 different spiking levels were ranged between 83.71-109.45% with relative standard deviation <3. The method was successfully applied to the field samples, which were collected randomly at 0 to 14 days’ post application. The rate of dis-appearance of Azoxystrobin on Chard was described as 1st order kinetics with half-life of 4.95 days.
05 포스터 발표 : 환경 화학 분야(PC) ; PC-07 ; HPLC-UVD를 이용한 근대에서의 아세타미프리드 분석
카빌 ( Humayun Kabir ),무스픽 ( Musfiqur Rahman ),팔하 ( Waziha Farha ),최정희 ( Jeong Heui Choi ),김성우 ( Sung Woo Kim ),임소정 ( So Jeong Im ),정다이 ( Da I Jung ),압두 ( Abd El Aty ),심재한 ( Jae Han Shim ) 한국환경농학회 2014 한국환경농학회 학술대회집 Vol.2014 No.-
An analytical method was developed to investigate dissipation pattern of acetamiprid in chard using high performance liquid chromatography (HPLC) coupled with ultra violet detector (UVD). Samples were extracted with acetonitrile and salt and purified through glass column due to matrix interferences. Calibration curve was linear with determination coefficient, R2> 0.999. Method was validated in triplicate with three different spiked concentration levels. Goodrecoveries was found and ranging from 91.19-97.64% with relative standard deviation, RSD <7. The validated method was applied to the field samples which were randomly collected after 0 to 14 days post application. The rate of disappearance of acetamiprid was described as first. order kinetics with a half-life of 4.07 days.
05 포스터 발표 : 환경 화학 분야(PC) ; LC-MS/MS를 이용한 현미와 볏짚에서의 Benzobicyclon과 대사체 잔류 분석
임소정 ( So Jeong Im ),최정희 ( Jeong Heui Choi ),김성우 ( Sung Woo Kim ),정다이 ( Da I Jung ),이영준 ( Young Jun Lee ),무스픽 ( Musfiqur Rahman ),압두 ( Abd El Aty ),심재한 ( Jae Han Shim ) 한국환경농학회 2014 한국환경농학회 학술대회집 Vol.2014 No.-
This study was carried out to develop an extraction as well as an analytical method for detecting benzobicyclon and its amino-substituted metabolite (1315P-570) in brown rice and rice straw using liquid chromatography-tandem mass spectrometry (LC/MS/MS) in positive ionmode with multiple reaction monitoring (MRM). The parent as well as the metabolite in rice and rice straw were extracted and analyzed under the same conditions. The matrix-matched calibrations showed good linearity with determination coefficients ( R2) of > 0.994. Recoveries at two different spiking levels were satisfactory and ranged between 75.4.118.9% with relative standard deviations (RSDs) < 13% for both analytes. Under storage conditions (.20℃), the analyte and its metabolite were stable for up to 92 days. The limits of quantitation (LOQs) were lower than the maximum residue level (MRL) set by the Ministry of Food and Drug Safety for brown rice (0.1 mg/kg). Field trials with recommended or double the recommended dose revealed that the herbicide could safely be applied to rice and rice straw, as no residues were detected in the harvested samples. The sensitivity of the developed method was sufficient to ensure reliable determination of benzobicyclon and its metabolite in rice grain and rice straw.