• Title/Summary/Keyword: residual range

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Development of the Simultaneous Analysis of 36 Sulfonylurea Herbicide Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 제초제 Sulfonylurea계 36종 동시 시험법 개발)

  • Su Jung Lee;Jung Mi Lee;Gui Hyun Jang;Hyun-Kyung Kim;Ji Young Kim
    • Korean Journal of Environmental Agriculture
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    • v.42 no.2
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    • pp.139-151
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    • 2023
  • Sulfonylurea herbicides are widely used in agriculture because they have a long residual period and high selectivity. An analytical method was developed using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique for simultaneous determination of sulfonylurea herbicide residues in agricultural products by liquid chromatography tandem mass spectrometry and for establishment MRL (Maximum Residue Limit) of those herbicides in Korea. Extraction was performed using acetonitrile containing 0.1% formic acid with MgSO4 (anhydrous magnesium sulfate) and NaCl (sodium chloride) and the extract was cleaned up using MgSO4 and C18 (octadecyl). The matrix-matched calibration curves were composed of 7 concentration levels from 0.001 to 0.25 mg/kg and their coefficients of determination (R2) exceeded 0.99. The recoveries of three spiking levels (LOQ, 10LOQ, 50LOQ, n=5) were in the range of 71.7-114.9% with relative standard deviations of less than 20.0% for all the five agriculture products. All validation values met criteria of the European Union SANTE/11312/2021 guidelines and Food and Drug Safety Evaluation guidelines. Therefore, the proposed analytical method was accurate, effective, and sensitive for sulfonylurea herbicide residues determination in agricultural commodities.

Persistence Study of Thiamethoxam and Its Metabolite in Kiwifruit for Establishment of Import Tolerance

  • Il Kyu Cho;Gyeong Hwan Lee;Woo Young Cho;Yun-Su Jeong;Danbi Kim;Kil Yong Kim;Gi-Woo Hyoung;Chul Hong Kim
    • Korean Journal of Environmental Agriculture
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    • v.41 no.4
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    • pp.355-364
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    • 2022
  • BACKGROUND: Pre-harvest interval and decline pattern of thiamethoxam were determined in kiwifruit using liquid chromatography-tandem mass spectrometry (LCMS/MS). The study was carried out to propose import tolerance using OECD maximum residue limit (MRL) calculator for the export promotion of kiwifruit to Taiwan. METHODS AND RESULTS: The thiamethoxam residue in kiwifruit was determined by using the LC-TriQ-MS/MS with the analytical process to set up the import tolerance under greenhouse conditions for Taiwan. Excellent linearity was observed for all of the analytes with a determination coefficient (R2)≥0.99. The limit of quantification was determined to be 0.01 mg/kg for both thiamethoxam and clothianidin in kiwifruit. Linearity was determined from the co-efficient of determinants (R2) obtained from the seven-point calibration curve. The standard calibration curve showed as follows; 1) Site 1 (Gimje): y = 944,406X + 1,583 (R2=0.9995), 2) Site 2 (Goheung): y = 1,356,205X + 934 (R2=0.9983), and 3) Site 3 (Jangheung): y = 1,239,937X - 3,090 (R2=0.9908). The residue of thiamethoxam in the kiwifruit for three decline trials showed the range of 0.35 to 0.56 mg/kg in site 1 (Gimje), 0.24 to 0.55 mg/kg in site 2 (Goheung), and 0.28 to 0.42 mg/kg in site 3 (Jangheung), respectively. However, clothianidin was not detected in all of the treatments. The maximum residual amounts (decline) in the samples, sprayed according to the safe-use standard for thiamethoxam 10% WG in kiwifruit (30 days before harvest, 3 sprays every 7 days) were 0.56 mg/kg in site 1, 0.55 mg/kg in site 2, and 0.42 mg/kg in site 3, respectively. CONCLUSION(S): The import tolerance (IT) of thiamethoxam for kiwifruit may be proposed to be 0.9 mg/kg by using the OECD MRL calculator.

Development of a rapid HPLC method for the determination of penciclovir in human plasma using a monolithic column and its application to a bioequivalence study (모노리틱 칼럼을 이용한 혈장 중 펜시를로버의 HPLC 신속분석법 개발 및 이를 이용한 생물학적동등성시험)

  • Kim, Jin Hee;Park, Ah Yeon;Jung, Eun Ha;Lee, Cheol Woo;Lee, Tae Ho;Youm, Jeong-Rok
    • Analytical Science and Technology
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    • v.20 no.4
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    • pp.323-330
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    • 2007
  • A simple and rapid HPLC method with fluorescence detection(FLD) for quantitation of penciclovir in human plasma using a monolithic column was developed and validated. Penciclovir and ganciclovir(internal standard, I.S.) were separated on a Chromolith column RP-18e ($4.6{\times}100mm$) with a mobile phase consisting of a mixture of (A) methanol/50 mM sodium phosphate buffer containing 200 mg/L sodium dodecyl sulfate (3/97, pH 2.5) and (B) methanol/50 mM sodium phosphate buffer containing 200 mg/L sodium dodecyl sulfate (50/50, pH 2.5) at a flow gradient of $1.6{\sim}4.0mL/min$. The retention times of penciclovir and internal standard were less than 4.0 min. Calibration curve was linear ($R^2=0.9994$) over a concentration range of $0.1{\sim}5{\mu}g/mL$. Intra-day precision, accuracy and inter-day precision were 1.36~8.55 %, 92.8~100.0 % and 0.93~5.62 %, respectively with a limit of quantitation at $0.1{\mu}g/mL$. The present HPLC-FLD method is sensitive, precise and accurate. The method described herein has been successfully used for the bioequivalence study of a famciclovir formulation product after oral administration to healthy Korean volunteers.

Simultaneous analysis of residual glucocorticoids in egg by LC/MS/MS (LC/MS/MS를 이용한 계란 중 잔류 글루코코티코이드의 동시분석)

  • Jang, Mi-Ae;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.22 no.4
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    • pp.326-335
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    • 2009
  • A specific analytical method able to identify and quantify traces of six glucocorticoids residues in eggs were developed. The extraction and clean-up parameters for simultaneous analysis were evaluated and HPLC and spectrometric conditions were also established. For determination of glucocorticoids, 5 g of egg was transferred into a test tube, adjusted pH 5.2 with acetate buffer and was $\beta$-glucuronidase/arylsulfatase from Helix pomatia added. The mixture was centrifuged and supernatant was extracted twice with 20 mL n-hexane. The extraction was performed with HLB cartridge using methanol, followed by clean-up with silica cartridge using methanol/ethyl acetate (4/6, v/v). The analytes were determined by HPLC/ESI-MS/MS operating in the negative ion mode. Validation studies with fortified egg samples for established method were performed. The result of method validation gave good efficiency, linearity, accuracy and precision. The correlation coefficients ($r^2$) of the calibration curves appeared to be higher than 0.99 in egg, indicating excellent linearity. LOD was ranged 0.09 to $0.17{\mu}g/kg$, and recoveries for most compounds were in the range of 55.7-69.8%. This method can be used to determine ${\mu}g/kg$ levels of glucocorticoids in eggs.

Disassembly of the Package/PCB on Wasted LED Light and their Characterizations (LED 조명 모듈에 장착된 패키지/PCB의 분리 및 특성)

  • Seunghyun Kim;Ha Bich Trinh;Taehun Son;Jaeryeong Lee
    • Resources Recycling
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    • v.32 no.6
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    • pp.3-9
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    • 2023
  • Separation of LED packages from PCBs and analysis of the adhesive components was conducted to enhance the recycling potential of LED modules. LED package was separated from PCBs using heat treatment under optimal conditions: temperature of above 250 ℃ and time of 20 minutes. The separation equipment can be established using a hot air injector with controlling the rotational speed of the internal screw. The separation efficiency of each type of substrate (aluminum and glass fiber) was investigated with the thickness range of the adhesive materials (0.25-0.30 and 0.30-0.35 mm). Under the optimal conditions, the efficiency can reach to 97.5% for both types of substrates with adhesive materials of thickness 0.25~0.30mm. Characterization of the residual adhesive substances from the separated LED package and PCB using microwave digestion and ICP analysis showed that the residue contained of 95% of Sn, less than 5% of Cu and Ag.

On-orbit Thermal Characteristic for Multilayered High Damping Yoke Structure Based on Superelastic Shape Memory Alloy for Passive Vibration Control of Solar Panels (태양전지판의 수동형 제진을 위한 초탄성 형상기억합금 기반 적층형 고댐핑 요크 구조의 궤도상 열적 특성 분석)

  • Min-Young Son;Jae-Hyeon Park;Bong-Geon Chae;Sung-Woo Park;Hyun-Ung Oh
    • Journal of Aerospace System Engineering
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    • v.18 no.1
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    • pp.1-10
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    • 2024
  • In a previous study, a structure of a superplastic yoke consisting of a thin FR4 layer laminated with viscoelastic tape on both sides of a shape memory alloy (SMA) was proposed to reduce residual vibration generated by a deployable solar panel during high motion of a satellite. Damping properties of viscoelastic tapes will change with temperature, which can directly affect vibration reduction performance of the yoke. To check damping performance of the yoke at different temperatures, free damping tests were performed under various temperature conditions to identify the temperature range where the damping performance was maximized. Based on above temperature test results, this paper predicts temperature of the yoke through orbital thermal analysis so that the yoke can have effective damping performance even if it is exposed to an orbital thermal environment. In addition, the thermal design method was described so that the yoke could have optimal vibration reduction performance.

Investigation of the Effects of Wavelength Range and Absorption Cross-Section on Sulfur Dioxide Slant Column Density Retrieval Using Ground-Based UV Scattered Sunlight Measurement (지상 기반 태양 UV 산란광 관측을 이용한 이산화황 경사칼럼농도 산출 시 파장 구간 및 흡수단면적에 따른 영향 조사)

  • Gyeong Park;Buju Gong;Minji Kim;Hanlim Lee
    • Korean Journal of Remote Sensing
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    • v.40 no.4
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    • pp.377-385
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    • 2024
  • We investigated the effect of spectral fitting wavelength interval variations and selection of absorption cross-section on the sulfur dioxide slant column density (SCD) retrievals from the scattered sunlight observation using a UV-Vis hyperspectral instrument. The sulfur dioxide slant column densities were retrieved from the combinations of multiple spectral fitting intervals and absorption cross-sections. The observation was carried out at the site 0.53 km away from a combustion site located in Gimhae from December 1, 2023, to January 23, 2024. The radiances were obtained on the line of measurement sight toward the stack of the combustion facility. The best spectral fitting intervals were found to be from 305.7 to 321.1 nm. In terms of the absorption cross-section dependency, the SO2 (293 K), O3 (223 K, 243 K) show the best spectral fitting for the observed radiances with both the smallest fitting residual and SCD error. The effects of the fitting interval and cross sections found in this study can be useful information for improving SO2 retrievals based on UV hyperspectral measurements.

Detection of Abnormal CAN Messages Using Periodicity and Time Series Analysis (CAN 메시지의 주기성과 시계열 분석을 활용한 비정상 탐지 방법)

  • Se-Rin Kim;Ji-Hyun Sung;Beom-Heon Youn;Harksu Cho
    • The Transactions of the Korea Information Processing Society
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    • v.13 no.9
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    • pp.395-403
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    • 2024
  • Recently, with the advancement of technology, the automotive industry has seen an increase in network connectivity. CAN (Controller Area Network) bus technology enables fast and efficient data communication between various electronic devices and systems within a vehicle, providing a platform that integrates and manages a wide range of functions, from core systems to auxiliary features. However, this increased connectivity raises concerns about network security, as external attackers could potentially gain access to the automotive network, taking control of the vehicle or stealing personal information. This paper analyzed abnormal messages occurring in CAN and confirmed that message occurrence periodicity, frequency, and data changes are important factors in the detection of abnormal messages. Through DBC decoding, the specific meanings of CAN messages were interpreted. Based on this, a model for classifying abnormalities was proposed using the GRU model to analyze the periodicity and trend of message occurrences by measuring the difference (residual) between the predicted and actual messages occurring within a certain period as an abnormality metric. Additionally, for multi-class classification of attack techniques on abnormal messages, a Random Forest model was introduced as a multi-classifier using message occurrence frequency, periodicity, and residuals, achieving improved performance. This model achieved a high accuracy of over 99% in detecting abnormal messages and demonstrated superior performance compared to other existing models.

Determination of Optimun Coagulant Dosage for Effective Water Treatment of Chinyang Lake -The Effect of Coagulant Dosing on Remoaval of Colloidal Pollutants- (진양호소수의 효과적인 정수처리를 위한 최적응집제 주입량 결정 -콜로이드성 오염물질 처리를 위한 응집제 주입효과-)

  • 이원규;조주식;이홍재;허종수
    • Journal of Environmental Science International
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    • v.7 no.6
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    • pp.761-772
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    • 1998
  • This study was performed to determine the optimum coagulant dosing amount for effective treatment of raw water. The removal rate of turbidity and the variations of water qualities according to various dosage of coagulants such as Alum, PAC and PACS were investigated. The optimum coagulant dosing amount to make the lowest turbidity of water were 35mg/ι t of Alum, 30mg/ι of PAC and 10mg/ι of PACS in case of 5 NTU of raw water turbidity, and 30mg/ι of Alum, 25mg/ι of PAC and 10mg/ι of PACS in case of 10 NTU of that, respectively. The removal rates of turbidity at 4 min. and 8 min. of settling time were 10 and 72% of Alum, 44 and 62% of PAC and 25 and 55% of PACS in case of 5 NTU, and 52 and 70% of Alum, 90 and 95% of PAC and 10 and 28% of PACS in case of 10 NTU, respectively. Judging from the settling capability of floc., the reaction time of floe. formation and removal efficiency of turbidity, PAC was evaluated as more effective coagulant than Alum and PACS. Also PAC was regarded as the most effective coagulant when the water supply was changed sharply and the fluctuation of the surface loading occured with wide and sharp in settling basin. pH and alkalinity of the water were decreased with increasing coagulants dosage. But pH and alkalinity were not decreased below 5.8 which is the standard for drinking water quality, and 10mg/ι which is the limit concentration of floc. breakage, respectively. Residual Al of the treated water was decreased with increasing coagulants dosage in case of 5 and 10NTU of raw water turbidity. $KMnO_4$ consumption of the water was decreased with increasing coagulants dosage. The reduction rate of $KMnO_4$ consumption at the optimum coagulants dosage were 39% of Alum. 18% of PAC and 11% of PACS in case of 5 NTU of raw water turbidity, and 42% of Alum, 27% of PAC and 36% of PACS in case of 10 NTU of that, respectively. Any relationship was not found between the removal rate of turbidity and KMnO$_4$ consumption. TOC of the water was a bit decreased with increasing coagulants dosage up to 30mg/ι but not changed above 30mg/ι of coagulants dosage. The degree of TOC reduction was increased in the order of Alum, PAC and PACS treatment. Zeta potential of the colloidal floe. at the optimum coagulants dosage was in the range of -20~-15mV in case of 5 NTU of raw water turbidity and 0~0.5mV in case of 10 NTU of that. respectively. Although the kinds and dosages of coagulants were different, zeta potential range were fixed under the conditions of the best coagulation efficiency.

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Dorsal Mini-thoracotomy for PDA Closure in Premature Neonates (후방 소개흉술을 통한 미숙아 동맥관 개존증의 수술요법)

  • Lee, Hyang-Lim;Choi, Chang-Hyu;Son, Dong-Woo;Shim, So-Yeon;Park, Kook-Yang;Park, Chul-Hyun
    • Journal of Chest Surgery
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    • v.42 no.4
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    • pp.434-440
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    • 2009
  • Background: Surgical closure of a patent ductus arteriosus (PDA) can be considered when conservative medical treatment is ineffective or contraindicated. Low weight and earlier gestational age neonates who are treated with conservative medical therapy generally showed a higher failure rate. The morbidity of surgical PDA closure in such extremely low birth weight (ELBW) neonates is also high. Here we present the early results of a new technique for approaching the PDA through a dorsal minithoracotomy. Material and Method: From March 2006 to November 2008, 24 premature neonates underwent surgical PDA closure. The procedures were performed in the newborn intensive care unit via a 2 cm long dorsal minithoracotomy with the baby in the prone position with the left hemithorax elevated 30$^{\circ}$. Bimanual cotton swab blunt dissection completed the extrapleural accesstothe PDA and then two clips were applied. Tube thoracostomy was avoided if there was no meaningful pleural laceration. Result: The infants mean gestational age was 26.5$\pm$2.1 weeks (range: 23 to 30 weeks) and the average age at operation was 11$\pm$11 days. The mean body weight at operation was 933$\pm$271 grams (range: 570 to 1,700 grams). Eight patients expired, but there was no procedure-related death. Postoperative echocardiography revealed two cases of residual shunt but none of these shunts were detected on the follow up echocardiogram that was performed on the post operative 5 and 59 days. Conclusion: We concluded that the technique described here is an effective procedure in view of the satisfactory operative exposure and the low rate of complications.