• Title/Summary/Keyword: LC/MSD

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Application of On-Line SPE-LC/MSD to Measure Perfluorinated Compounds (PFCs) in Water (On-Line SPE-LC/MSD 시스템을 이용한 수중의 과불화 화합물(PFCs) 분석)

  • Son, Hee-Jong;Yoom, Hoon-Sik;Jung, Jong-Moon;Jang, Seung-Ho
    • Journal of Korean Society of Environmental Engineers
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    • v.35 no.2
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    • pp.75-83
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    • 2013
  • We applied a sensitive method based on on-line solid-phase extraction (SPE) and liquid chromatography/mass spectrometry (LC/MSD) using an electrospray interface for the determination of eleven perfluorinated compounds (PFCs) in water. The on-line connection suppressed the target loss by keeping the cartridge from drying, which resulted in improvement of the recovery and saving of the analytical time. For the on-line solid-phase extraction of 10 mL water samples, recoveries were between $80.4{\pm}5.2%{\sim}109.5{\pm}1.4%$ and limit of quantification (LOQ) were 3.6~15.9 ng/L for the PFCs. The total PFCs concentrations of the tributaries and main stream of Nakdong River water samples were in the range of $8.0{\sim}678.6{\mu}g/L$.

Molecular Size Distributions of NOM in Conventional and Advanced Water Treatment Processes (기존수처리 공정 및 고도정수처리 공정에서 NOM의 분자크기 분포 변화)

  • Choi, Il-Hwan;Jung, Yu-Jin
    • Journal of Korean Society on Water Environment
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    • v.24 no.6
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    • pp.682-689
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    • 2008
  • The purpose of this study was to find out the variation between molecular size distribution (MSD) of natural organic matter (NOM) in raw waters after different water treatment processes like conventional process (coagulation, flocculation, filtration) followed by advanced oxidation process (ozonation, GAC adsorption). The MSD of NOM of Suji pilot plant were determined by Liquid Chromatography-Organic Carbon Detection (LC-OCD) which is a kine of high-performance size-exclusion chromatography (HPSEC) with nondispersive infrared (NDIR) detector and $UV_{254}$ detector. Five distinct fractions were generally separated from water samples with the Toyopearl HW-50S column, using 28 mmol phosphate buffer at pH 6.58 as an eluent. Large and intermediate humic fractions were the most dominant fractions in surface water. High molecular weight (HMW) matter was clearly easier to remove in coagulation and clarification than low molecular weight (LMW) matter. Water treatment processes removed the two largest fractions almost completely shifting the MSD towards smaller molecular size in DW. No more distinct variation of MSD was observed by ozone process after sand filtration but the SUVA value were obviously reduced during increase of the ozone doses. UVD results and HS-Diagram demonstrate that ozone induce not the variation of molecular size of humic substance but change the bond structure from aromatic rings or double bonds to single bond. Granular activated carbon (GAC) filtration removed 8~9% of organic compounds and showed better adsorption property for small MSD than large one.

Evaluating the prediction models of leaf wetness duration for citrus orchards in Jeju, South Korea (제주 감귤 과수원에서의 이슬지속시간 예측 모델 평가)

  • Park, Jun Sang;Seo, Yun Am;Kim, Kyu Rang;Ha, Jong-Chul
    • Korean Journal of Agricultural and Forest Meteorology
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    • v.20 no.3
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    • pp.262-276
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    • 2018
  • Models to predict Leaf Wetness Duration (LWD) were evaluated using the observed meteorological and dew data at the 11 citrus orchards in Jeju, South Korea from 2016 to 2017. The sensitivity and the prediction accuracy were evaluated with four models (i.e., Number of Hours of Relative Humidity (NHRH), Classification And Regression Tree/Stepwise Linear Discriminant (CART/SLD), Penman-Monteith (PM), Deep-learning Neural Network (DNN)). The sensitivity of models was evaluated with rainfall and seasonal changes. When the data in rainy days were excluded from the whole data set, the LWD models had smaller average error (Root Mean Square Error (RMSE) about 1.5hours). The seasonal error of the DNN model had the similar magnitude (RMSE about 3 hours) among all seasons excluding winter. The other models had the greatest error in summer (RMSE about 9.6 hours) and the lowest error in winter (RMSE about 3.3 hours). These models were also evaluated by the statistical error analysis method and the regression analysis method of mean squared deviation. The DNN model had the best performance by statistical error whereas the CART/SLD model had the worst prediction accuracy. The Mean Square Deviation (MSD) is a method of analyzing the linearity of a model with three components: squared bias (SB), nonunity slope (NU), and lack of correlation (LC). Better model performance was determined by lower SB and LC and higher NU. The results of MSD analysis indicated that the DNN model would provide the best performance and followed by the PM, the NHRH and the CART/SLD in order. This result suggested that the machine learning model would be useful to improve the accuracy of agricultural information using meteorological data.

A Survey on Safety of Commercial Fruit Teas in Gwangju Area (유통 열매 차류의 안전성 조사 - 구기자, 오미자, 산수유를 중심으로 -)

  • Kan, In-Sook;Lee, Hyang-Hee;Seo, Jung-Mi;Oh, Mu-Sul;Jeong, Ji-Hee;Yu, Yen-A;Cho, Bae-Sik;Seo, Kye-Won;Kim, Eun-Sun;Moon, Yong-Woon
    • Journal of Food Hygiene and Safety
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    • v.26 no.2
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    • pp.100-106
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    • 2011
  • This study was conducted to investigate the residue amount of harmful materials on the 113 commercial fruit teas (Gugija, Omija, Sansuyu) in Gwangju area. It was performed using the GC-ECD, GC-NPD, GC-MSD and the LC-UVD, LC-FLD, LC-MSD to analyze 200 pesticides. The heavy metals were determined using a Mercury analyzer and AAS. The sulfur dioxides were analyzed by modified Monnier-Williams method. The residual pesticides were detected in 4 samples (Gugija). The mean values of heavy metal contents (mg/kg) were Pb, 0.024; Cd, 0.031; As, 0.010; Hg, 0.003. The measured values of Pb, Cd, As, Hg showed within MRLs. The sulfur dioxides were over MRLs in 4 samples (Gugija). These results will be used to establish on the regulation of commercial fruit teas in Gwangju area.

A Survey on Harmful Materials of Commercial Medical Herb in Gwangju Area (광주지역 유통 한약재의 유해물질 잔류실태조사)

  • Lee, Hyang-Hee;Seo, Jung-Mi;Oh, Mu-Sul;Gang, In-Sook;Park, Jong-Jin;Seo, Kye-Won;Ha, Dong-Ryong;Kim, Eun-Sun
    • Journal of Food Hygiene and Safety
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    • v.25 no.2
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    • pp.83-90
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    • 2010
  • This study was conducted to investigate the residue amount of harmful materials on the 153 commercial medical herbs in Gwangju area. It was performed using the GC-ECD, GC-NPD, GC-MSD and the LC-UVD, LC-FLD, LC-MSD to analyze 200 pesticides. The heavy metals were determined using a Mercury analyzer and AAS. The sulfur dioxides were analyzed by modified Monnier-Williams method. The residual pesticides were detected in 7 samples, and were over MRLs (Maximum Risk Levels) in 2 samples (1.3%). The mean values of heavy metal contents (mg/kg) were Pb, 0.570; Cd, 0.081; As, 0.082; Hg, 0.0093. The measured values of Pb, As, Hg showed within MRLs. The excess samples of MRLs were 3 samples (changchul 2, cheongung 1) on Cd. The sulfur dioxides were over MRLs in 7 samples (4.6%), hwanggi and gugija. These results will be used to establish on the regulation of commercial medical herbs in Gwangju area.

A study of the metabolites for 7-keto-DHEA-acetate in human urine (뇨시료에 함유된 7-keto-DHEA-acetate의 대사체에 관한 연구 (I))

  • Kim, Yunje;Lee, Jinhee
    • Analytical Science and Technology
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    • v.17 no.4
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    • pp.337-346
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    • 2004
  • 7-keto-dehydroepiandrosterone-acetate (7-keto-DHEA-acetate) is an anabolic steroids, and we studied basically to the metabolites of it after human dosing. We tested the matrix effect from human urine to detect the 7-keto-DHEA-acetate. And LC/ESI/MS and GC/MSD was used to detect the metabolites in dosed urine. We found the some unknown compound from dosed urine (M1, M2, M3, M4 and M5), and from these results, we supposed that these compounds have the more than 3 hydroxyl and/or ketone group. Metabolite M1 was supposed that molecular weight is 302 and 3-,17-diketone and 7-hydroxyl compound (7-OH-androstendione). Metabolite M2 was supposed that the molecular weight was same to M1 and 7-,17-diketone and 3-hydroxyl compound (7-keto-DHEA).

Bioequivalence of $Enalacc^{TM}$ Tablet to $Renitec^{TM}$ Tablet(Enalapril maleate 10 mg)

  • Cho, Sung-Hee;Ha, Yong-Hwa;Hong, Sung-Je;Seo, Seong-Hoon;Rew, Jae-Hwan;Kim, Dong-Hyun;Lee, Kyung-Tae
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.244.3-245
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    • 2003
  • ABSTRACT-The purpose of the present study was to evaluate the bioequivalence of two enalapril maleate tablest, $Renitec^{TM}$(MSD Korea Ltd.) and $Enalace^{TM}$(Welfide Korea Ltd.), according to the guidelines of Korea Food and Drug Administration (DFDA). Twenty-four normal male volunteers, 22.33 ${\pm}$ 2.55 year in age and 66.54 ${\pm}$ 8.30 kg in body weight, were divided into two groups and a randomized 2${\times}$2 cross-over study was employed. After two tablets containing 10 mg of enalapril maleate per tablet were orally administered, blood was taken at predetermined time intervals and concentrations of enalapril in plasma were determined using LC-MS-MS. (omitted)

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Monitoring of pesticide residues in commercial agricultural products in the northern area of Seoul, Korea (서울 북부지역 유통 농산물의 농약 잔류실태)

  • Han, Sung-Hee;Park, Sung-Kyu;Kim, Ouk-Hee;Choi, Young-Hee;Seoung, Hyun-Jung;Lee, Young-Ju;Jung, Jung-Hee;Kim, Yun-Hee;Yu, In-Sil;Kim, Yoo-Kyung;Han, Ki-Young;Chae, Young-Zoo
    • The Korean Journal of Pesticide Science
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    • v.16 no.2
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    • pp.109-120
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    • 2012
  • This study was conducted to monitor 284 pesticides residue level in 2,914 commercial agricultural products in the northern area of Seoul in 2011 by the multi class pesticide multiresidue analysis methods in Korea Food Code using GC, HPLC, GC-MSD and, LC-MSD. The detection rate of pesticide residues were 14.8% (431/2,914). The order of agricultural products in which the pesticide residues were detected was perilla leaves 40.0% (28/70), chamnamul 35.5% (11/31), amaranth 30.0% (3/10) and spinach 27.7% (38/137) etc. The percentage of products that exceeded the MRLs (maximum residue limits) were 1.0% (31/431). Those products that exceeded MRLs were ginseng (6), perilla leaves (4), leek (4), welsh onion (3) and sedeum (3) etc. The 59 kinds of the pesticides were detected on this study, 21 pesticides of them were detected over MRLs. Detection rate of fungicides (56.4%) was higher than that of insecticides (42.1%). And procymidone was detected with considerable high frequency. Additionally, residual residual violates pesticides were in the order of tolclofos-methyl, endosulfan, dimethomorph, diniconazole and fludioxonil. According to the agricultural marketing channels, detection and excess rate of them were monitored. Detection and excess rate of samples circulated in agricultural traditional market were highest. The estimated daily intakes (EDI) of the pesticides were compared to personal acceptable daily intakes (PADI) in order to risk assessment by food consumption. Diazinon in Korean cabbage showed the highest %ADI, 2.9901 and others showed below 3.0 %ADI. Overall, these results indicate that residue levels of pesticides detected were evaluated as safe.

Characteristics of Thiosulfinates and Volatile Sulfur Compounds from Blanched Garlic Reacted with Alliinase (Alliinase 첨가에 의한 열처리 마늘로부터 생성된 함황 화합물의 특성)

  • Choi, Yoon-Hee;Shim, You-Sin;Kim, Cheong-Tae;Lee, Chan;Shin, Dong-Bin
    • Korean Journal of Food Science and Technology
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    • v.39 no.6
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    • pp.600-607
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    • 2007
  • In this study, attempts were made to develop a method for controlling the volatile sulfur compounds in garlic. Crude alliinase extracted from fresh garlic was applied to garlic pulp blanched far 5 min at $100^{\circ}C$, and the changes in the thiosulfinates and volatile compounds of the blanched garlic pulp reacted with the enzyme were investigated. Eight kinds of thiosulfinates from garlic were separated by HPLC, and identified by LC/MS/MS. When the alliinase was added to the blanched garlic pulp at 100, 200, 300, or 400 units, and reacted for 15 min, respectively, thiosulfinates were generated in the amounts of 37, 68, 77, and 80% of the fresh garlic content (control). Under the same conditions, we analyzed the volatile compounds, where 28 peaks were identified by GC/MSD. Of the 28 peaks, 23 were volatile sulfur compounds. The results of the analysis showed that all the volatile compounds were generated at amounts of 25, 36, 66, and 76% of the content of the control, respectively. These results indicate that the sulfur compound content of garlic can be regulated, depending upon the reaction conditions of allinase.