• Title/Summary/Keyword: quantitation

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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.

Development and validation of an analytical method for fungicide fenpyrazamine determination in agricultural products by HPLC-UVD (HPLC-UVD를 이용한 살균제 fenpyrazamine의 시험법 개발 및 검증)

  • Park, Hyejin;Do, Jung-Ah;Kwon, Ji-Eun;Lee, Ji-Young;Cho, Yoon-Jae;Kim, Heejung;Oh, Jae-Ho;Rhee, Kyu-Sik;Lee, Sang-Jae;Chang, Moon-Ik
    • Analytical Science and Technology
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    • v.27 no.3
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    • pp.172-180
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    • 2014
  • Fenpyrazamine which is a pyrazole fungicide class for controlling gray mold, sclerotinia rot, and Monilinia in grapevines, stone fruit trees, and vegetables has been registered in republic of Korea in 2013 and the maximum residue limits of fenpyrazamine is set to grape, peach, and mandarin as 5.0, 2.0, and 2.0 mg/kg, respectively. Very reliable and sensitive analytical method for determination of fenpyrazamine residues is required for ensuring the food safety in agricultural products. Fenpyrazamine residues in samples were extracted with acetonitrile, partitioned with dichloromethane, and then purified with silica-SPE cartridge and eluted with hexane and acetone mixture. The purified samples were determined by HPLC-UVD and confirmed with LC-MS and quantified using external standard method. Linear range of fenpyrazamine was between $0.1{\sim}5.0{\mu}g/mL$ with the correlation coefficient (r) 0.999. The average recovery ranged from 71.8 to 102.7% at the spiked level of 0.05, 0.5, and 5.0 mg/kg, while the relative standard deviation was between 0.1 and 7.3%. In addition, limit of detection and limit of quantitation were 0.01 and 0.05 mg/L, respectively. The results revealed that the developed and validated analytical method is possible for fenpyrazamine determination in agricultural product samples and will be used as an official analytical method.

Establishment of Pre-Harvest Residue Limit(PHRL) of Insecticide Chlorfenapyr and Fungicide Fenarimol during Cultivation of Chwinamul(Aster scaber) (취나물의 재배기간 중 살충제 Chlorfenapyr와 살균제 Fenarimol의 생산단계 농약잔류허용기준의 설정)

  • Lim, Jong-Sung;Hong, Ji-Hyung;Lee, Cho-Rong;Han, Kook-Tak;Lee, Yu-Ri;Lee, Kyu-Seung
    • Korean Journal of Environmental Agriculture
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    • v.30 no.1
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    • pp.52-59
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    • 2011
  • BACKGROUND: This study was performed to investigate pre-harvest residue limit (PHRL) in Chwinamul, to estimate biological half-life for residue of each pesticide. Chwinamul was sprayed with pesticides of standard and double application rate. Chlorfenapyr and fenarimol were sprayed once on Chwinamul at 10 days before harvest, and it was sampled 7 times and analysed the residual change of two pesticides. METHODS AND RESULTS: Chwinamul sample was extracted with acetonitrile and partitioned with dichloromethane, and pesticide residues were determined with GCECD. Method quantitation limit (MQL) of chlorfenapyr was 0.10 mg/kg and that of fenarimol was 0.02 mg/kg. Recoveries of chlorfenapyr at two fortification levels of 1.0 and 5.0 mg/kg were $94.2{\pm}$1.70 and $99.0{\pm}1.61%$, respectively. Recoveries of fenarimol at two fortification levels of 0.2 and 1.0 mg/kg were $92.1{\pm}2.14$ and $83.1{\pm}1.98%$, respectively. CONCLUSION(s): The biological half-lives of chlorfenapyr were about 3.5 days at standard application rate, and 3.4 days at double application rate. The biological half-lives of fenarimol were about 6.0 days at standard application rate, and 5.9 days at double application rate. The PHRLs of chlorfenapyr were recommended as 13.02 and 6.25 mg/kg for 10 and 5 days before harvest, respectively. And the PHRLs of fenarimol were recommended as 2.80 and 1.67 mg/kg for 10 and 5 days before harvest, respectively.

Development of Analytical Methods of Spinosad in Agricultural Commodities by HPLC with UV Detector and Monitoring (HPLC-UVD를 이용한 농산물 중 스피노사드 분석법 개선 및 잔류실태 조사)

  • Kim, Hee-Yun;Choi, Sun-Hee;Chung, So-Young;Choi, Hee-Ju;Kim, Yong-Hoon;Cho, Min-Ja;Seo, Eun-Chae;Han, Kyoung-Jin;Choi, Jae-Chun;Park, Hee-Ok;Ha, Sang-Chul;Shin, Il-Shik;Eom, Ji-Yoon
    • Korean Journal of Food Science and Technology
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    • v.43 no.2
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    • pp.125-133
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    • 2011
  • The purpose of this study was to develop a methodology to detect spinosad which are difficult to analyze by multi-component simultaneous analysis of pesticide residues. We monitored spinosad due to the paucity of related information. The spinosad was determined using HPLC with UV detector at 250 nm. Correlation coefficient ($r^2$) for standard curve of spinosad A and D at standard concentration of 0.1-5.0 mg/kg were 0.999, respectively. Limit of quantitation (LOQ) of HPLC analysis was 0.005 mg/kg while limit of detection (LOD) was 0.001 mg/kg. Recovery experiments were conducted on five representative agricultural products to validate the analytical method. The recovery of proposed methods ranged from 74.9% to 104.0% and relative standard deviations were less than 10%. Spinosad residues were investigated in 16 commodities collected from 22 provinces. In this study, residues on all samples were not detected.

Investigation of Scatter and Septal Penetration in I-131 Imaging Using GATE Simulation (GATE 시뮬레이션을 이용한 I-131 영상의 산란 및 격벽통과 보정방법 연구)

  • Jung, Ji-Young;Kim, Hee-Joung;Yu, A-Ram;Cho, Hyo-Min;Lee, Chang-Lae;Park, Hye-Suk
    • Progress in Medical Physics
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    • v.20 no.2
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    • pp.72-79
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    • 2009
  • Scatter correction for I-131 plays a very important role to improve image quality and quantitation. I-131 has multiple and higher energy gamma-ray emissions. Image quality and quantitative accuracy in I-131 imaging are degraded by object scatter as well as scatter and septal penetration in the collimator. The purpose of this study was to estimate scatter and septal penetration and investigate two scatter correction methods using Monte Carlo simulation. The gamma camera system simulated in this study was a FORTE system (Phillips, Nederland) with high energy, general-purpose, parallel hole collimator. We simulated for two types of high energy collimators. One is composed of lead, and the other is composed of artificially high Z number and high density. We simulated energy spectrum using a point source in air. We estimated both full width at half maximum (FWHM) and full width at tenth maximum (FWTM) using line spread function (LSF) in cylindrical water phantom. We applied two scatter correction methods, triple energy window scatter correction (TEW) and extended triple energy window scatter correction (ETEW). The TEW method is a pixel-by pixel based correction which is easy to implement clinically. The ETEW is a modification of the TEW which corrects for scatter by using abutted scatter rejection window, which can overestimate or the underestimate scatter. The both FWHM and FWTM were estimated as 41.2 mm and 206.5 mm for lead collimator, respectively. The FWHM and FWTM were estimated as 27.3 mm and 45.6 mm for artificially high Z and high density collimator, respectively. ETEW showed that the estimation of scatter components was close to the true scatter components. In conclusion, correction for septal penetration and scatter is important to improve image quality and quantitative accuracy in I-131 imaging. The ETEW method in scatter correction appeared to be useful in I-131 imaging.

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Analysis of Isolated Proteinuria on School Urinary Mass Screening (학교 신체 검사에서 발견된 단독 단백뇨에 대한 연구)

  • Kim Cheol- Min;Hahn HyeWon;Lee Byung-Sun;Park Young Seo
    • Childhood Kidney Diseases
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    • v.6 no.1
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    • pp.61-67
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    • 2002
  • Purpose: The urinary mass screening program in school aged population has been performed since 1981, but the consensus on the follow-up schedule and the management of isolated proteinuria has not been reached yet. The aim of this study was to investigate the cause of isolated proteinuria and to propose a guideline for the treatment and follow-up afterwards Methods: The medical records of 114 cases of isolated proteinuria detected through the analysis of urinary mass screening and evaluated at the pediatric outpatient clinic of Asan Medical Center from January 1990 to July 2001 have been reviewed. Results: The classification of isolated proteinuria was as follows. Transient proteinuria $32\%$, orthostatic proteinuria $65\%$, persistent proteinuria $3\%$, In orthostatic proteinuria group, daytime and nighttime proteinuria were $319.2{\pm}189.1\;mg/dL$ and $56.5{\pm}56.1\;mg/dL$. In persistent proteinuria group, daytime and nighttime proteinuria were $1140{\pm}540.5\;mg/dL$ and $289{\pm}58\;mg/dL$. After 30 month follow-up, 2 cases of persistent proteinuria were needed renal biopsy and 1 case revealed focal segmental glomerular sclerosis. In all cases, serum creatinine, albumin and complements levels were normal. In the orthostatic proteinuria group, no significant renal diseases were detected. Conclusion: Since most of the isolated proteinuria detected through the school urinary mass screening were orthostatic proteinuria or transient proteinuria, initially aggressive diagnostic method such as renal biopsy is not needed and regular follow- up with quantitation of proteinuria is warranted.(J Korean Soc Pediatr Nephrol 2002 ; 6 61-7)

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A Rapid Analysis of 226Ra in Raw Materials and By-Products Using Gamma-ray Spectrometry (감마분광분석을 이용한 원료물질 및 공정부산물 중 226Ra 신속분석방법)

  • Lim, Chung-Sup;Chung, Kun-Ho;Kim, Chang-Jong;Ji, Young-Yong
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.15 no.1
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    • pp.35-44
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    • 2017
  • A gamma-ray peak of $^{226}Ra$ (186.2 keV) overlaps with one of $^{235}U$ (185.7 keV) in a gamma-ray spectrometry system. Though reference peaks of $^{235}U$ can be used to correct the peak interference of $^{235}U$ in the analysis of $^{226}Ra$, this requires a complicated calculation process and a high limit of quantitation. On the other hand, evaluating $^{226}Ra$ using the correction constant in the overlapped peak can make a rapid measurement of $^{226}Ra$ without the complicated calculation process as well as overcome the disadvantage in the indirect measurement of $^{214}Bi$, which means the confinement of $^{222}Rn$ gas in a sample container and a time period to recover the secular equilibrium. About 93 samples with 6 species for raw-materials and by-products were prepared to evaluate the activity of $^{226}Ra$ using the correction constant. The results were compared with the activity of $^{214}Bi$, which means the indirect measurement of $^{226}Ra$, to validate the method of the direct measurement of $^{226}Ra$ using the correction constant. The difference between the direct and indirect measurement of $^{226}Ra$ was generally below about ${\pm}20%$. However, in the case of the phospho gypsum, a large error of about 50% was found in the comparison results, which indicates the disequilibrium between $^{238}U$ and $^{226}Ra$ in the materials. Application results of the contribution ratio of $^{226}Ra$ were below about ${\pm}10%$. The direct measurement of $^{226}Ra$ using the correction constant can be an effective method for its rapid measurement of raw materials and by-products because the activity of $^{226}Ra$ can be produced with a simple calculation without the consideration of the integrity of a sample container and the time period to recover the secular equilibrium.

Determination of finasteride in human serum by LC-MS/MS (LC-MS/MS를 이용한 혈청 중 finasteride 분석)

  • Nam, Hye-Seon;Nam, Kyong-Hee;Jung, Su-Hee;Lee, Jang-Woo;Kang, Jin-Yeong;Hong, Soon-Keun;Kim, Tae-Sung;Kang, Tae-Seok;Yoon, Hae-Jung;Lee, Kwang-Ho;Rhee, Gyu-Seek
    • Analytical Science and Technology
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    • v.24 no.5
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    • pp.345-351
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    • 2011
  • A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed and validated for the determination of finasteride in human serum. Beclomethasone was used as internal standard (IS) and liquid-liquid extraction (LLE) using methyl tert-butyl ether (MTBE) was carried out to isolate analyte. The mass transitions monitored in multiple reaction monitoring (MRM) in positive ion mode were m/z 373.2${\rightarrow}$305.2 for finasteride and m/z 409.3${\rightarrow}$391.2 for IS. Retention times of finasteride and IS were 5.81 and 5.46 min, respectively. The limit of quantitation (LOQ) was 0.1 ng/mL and the calibration curve showed good linearity in the range of 0.1~20.0 ng/mL ($R^2$=0.9997). The intra-day assay precision and accuracy were in the range 6.3~10.6% and 97.3~103.6%, respectively, and the inter-day assay precision and accuracy were in the range 0.8~5.2% and 99.8~102.5%, respectively. The sample extract recovery of the method was 80~83%.

Establishment of Pre-Harvest Residue Limit for Pyrimethanil and Methoxyfenozide during Cultivation of grape (포도(Vitis vinifera L.) 중 Pyrimethanil 및 Methoxyfenozide의 생산단계 잔류허용기준 설정)

  • Kim, Ji Yoon;Woo, Min Ji;Hur, Kyung Jin;Manoharan, Saravanan;Kwon, Chan-Hyeok;Hur, Jang Hyun
    • The Korean Journal of Pesticide Science
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    • v.19 no.2
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    • pp.81-87
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    • 2015
  • The present study was aimed to predict the pre-harvest residue limits (PHRLs) of pyrimethanil (fungicide) and methoxyfenozide (insecticide) in grape, and to estimate their biological half-lives and residual characteristics. The pesticides were sprayed once on grape in two different fields 10 days before harvest. At the end of 0, 1, 2, 3, 5, 7 and 10 days after application, samples were harvested for further analysis. The residual pesticides were extracted with acetonitrile and partitioned with dichloromethane, and the high-performance liquid chromatography with diode array detector (HPLC/DAD) was employed for the residue analysis. The results obtained in the present study show that the limit of detection of both pesticides were found to be $0.01mg\;kg^{-1}$. The recoveries of these pesticides were ranged between 80.6% and 102.5% with coefficient of variation lower than 10%. The biological half-lives of both pesticides were observed in field 1 and field 2 which shows 7.7 and 7.4 days for pyrimethanil and 5.1 and 6.1 days for methoxyfenozide, respectively. Further, the PHRL of pyrimethanil and methoxyfenozide was found to be $8.90mg\;kg^{-1}$ and $5.51mg\;kg^{-1}$, respectively at 10 days before harvest. Consequently, the present study suggests that the residual amounts of both pesticides will be lower than the maximum residue limits (MRLs) when grape is harvested.

Exposure and Risk Assessment for Operator Exposure to Insecticide Acetamiprid during Water Melon Cultivation in Greenhouse using Whole Body Dosimetry (수박 시설재배에서 살충제 Acetamiprid 사용 시 전신노출법에 의한 농작업자의 노출 및 위해성평가)

  • Kim, Eunhye;Lee, Jiho;Sung, Jeonghee;Lee, Jonghwa;Shin, Yongho;Kim, Jeong-Han
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.247-257
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    • 2014
  • Assessment for operator's dermal and inhalation exposure to acetamiprid during cultivation of water melon in greenhouse was carried out. For dermal exposure measurement, whole body dosimetry (WBD) was performed as the first trial in Korea. WBD consists of cotton/polyester outer clothes and cotton inner clothes. Hand exposure was measured by washing of nitrile gloves and hands while head exposure was monitored by face/neck wipe technique. Inhalation exposure was monitored with personal air sampling pumps and IOM sampler (glass fiber filter). Analytical limit of quantitation was 2.5 ng/mL. Good reproducibility (C.V < 8.7%), linearity ($R^2$ > 0.99) and recovery (70~119%) were obtained. Field recovery of acetamiprid was 77~95%. During mixing/loading, hand exposure of acetamiprid was about 10 times ($229.7{\mu}g$) more than that of application case ($20.9{\mu}g$). During application, total dermal exposure was $1207.4{\mu}g$. Exposure of lower legs was $1132.1{\mu}g$, which is 93.8% of the total dermal exposure. Inhalation exposure during mixing/loading and application was not detected. Margin of safety (MOS) was calculated for risk assessment using male Korean average body weight (70 kg) and acceptable operator exposure level ($124{\mu}g/kg/day$) to give 140, suggesting that health risk of operator during treatment of acetamiprid for water melon in greenhouse could be safe.