• Title/Summary/Keyword: partition division

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Establishment of Analytical Method for Pencycuron in Representative Agricultural Commodities by High-Performance Liquid Chromatography (대표 농산물 중 살균제 Pencycuron의 HPLC 정밀 잔류분석법 개발)

  • Lee, Hyeri;Choi, Hoon;Kim, Byung-Joon;Kim, Eunhye;Kim, Su-Hee;Lee, Jin-Beom;Lee, Young Deuk;Kim, Jeong-Han
    • The Korean Journal of Pesticide Science
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    • v.21 no.1
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    • pp.75-83
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    • 2017
  • The single residue analytical method was developed for determining fungicide pencycuron residues in various agricultural commodities with high-performance liquid chromatography (HPLC). Pencycuron residue was extracted with acetone from representative crops such as Korean cabbage, apple, brown rice and green pepper. After ethyl acetate/n-hexane partition and subsequent clean-up with silica gel chromatography, pencycuron residue was quantified by reversed phase HPLC with UV detection at 240 nm. The suspected residue of pencycuron was confirmed using selected-ion monitoring (SIM) LC/mass spectrometry (MS). Instrumental limit of quantitation (ILOQ) and method LOQ (MLOQ) were set at 2 ng and 0.02 mg/kg, respectively. Overall recoveries of pencycuron from different crop samples fortified at three levels (MLOQ, 10MLOQ, 100MLOQ) were 72~108%. This proposed method could be useful as official analytical method for quantification of pencycuron residues in agricultural commodities.

Analytical Method of Bentazone Residue in Agricultural Commodities Using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 bentazone의 분석법 확립)

  • Kim, Young-Hak;Lee, Su-Jin;Song, Lee-Seul;Hwang, Young-Sun;Lee, Young-Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.15 no.2
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    • pp.149-159
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    • 2011
  • Bentazone is benzothiadiazole group herbicide, and used to foliage treatment. This herbicide have already been widely used for cereals and vegetables planting in worldwide. This experiment was conducted to establish a determination method for bentazone residue in crops using HPLC-UVD/MS. Bentazone residue was extracted with acetone (adjusted pH 1 with phosphoric acid) from representative samples of five raw products which comprised hulled rice, soybean, apple, green pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover bentazone from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The bentazone was quantitated by HPLC with UVD, using a YMC ODS AM 303 ($4.6{\times}250$ mm) column. The crops were fortified with bentazone at 3 levels per crop. Mean recovery ratio were ranged from 82.0% for a 0.2 mg/kg in apple to 97.9% for a 0.02 mg/kg in Chinese cabbage. The coefficients of variation were ranged from 0.5% for a 0.02 mg/kg in soybean to 9.7% for a 0.02 mg/kg in Chinese cabbage. Quantitative limit of bentazone was 0.02 mg/kg in representative five crop samples. A LC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of bentazone in agricultural commodities.

Analytical Method for Flusulfamide as Benzenesulfonamide Fungicide, Residues in Major Agricultural Commodities (주요 농산물 중 Bezenesulfonamide계 살균제 Flusulfamide의 잔류 분석법)

  • Ahn, Kyung-Geun;Kim, Gi-Ppeum;Hwang, Young-Sun;Kang, In-Kyu;Lee, Young Deuk;Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.37 no.1
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    • pp.57-65
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    • 2018
  • BACKGROUND: An analytical method was developed using HPLC-UVD/MS to precisely determine the residue of flusulfamide, a benzenesulfonamide fungicide used to inhibit spore germination. METHODS AND RESULTS: Flusulfamide residue was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice, and soybean. The extract was diluted with large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, flusulfamide was successfully separated from co-extractives of sample, and sensitively quantitated by ultraviolet absorption at 280 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop sample fortified with flusulfamide at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries ranged from 82.3 to 98.2% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of flusulfamide was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue.

Determination of Methoxyfenozide, Chromafenozide and Tebufenozide Residues in Agricultural Commodities Using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 작물 중 methoxyfenozide, chromafenozide 및 tebufenozide의 분석법 확립)

  • Lee, Su-Jin;Kim, Young-Hak;Hwang, Young-Sun;Kwon, Chan-Hyeok;Do, Jeong-A;Im, Moo-Hyeog;Lee, Young-Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.14 no.1
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    • pp.37-48
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    • 2010
  • The diacylhydrazine insecticides, methoxyfenozide, chromafenozide and tebufenozide are new-generation insecticides. These insecticides induce premature molting and cause the death of insects by mimicking their hormone. Also, these insecticides have already been widely used for vegetables planting in worldwide. Highperformance liquid chromatography (HPLC) is the most widely used procedure for determination of each compound residues in crops. However, simultaneous analysis method of these diacylhydrazine insecticides was not reported. The purpose of this study is to develop a simultaneous determination procedure of methoxyfenozide, chromafenozide and tebufenozide residue in crops using HPLC-UVD/MS method. These insecticide residues were extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, apple, pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover these insecticides from the aqueous phase. Florisil column chromatography was additionally employed for final cleanup of the extracts. The analytes were quantitated by HPLCUVD/MS, using a $C_{18}$ column. The crops were fortified with each insecticide at two levels per crop. Mean recoveries ranged from 89.0 to 104.8% in five representative agricultural commodities. The coefficients of variation were less than 3.9%. Quantitative limits of methoxyfenozide, chromafenozide and tebufenozide were 0.04 mg/kg in crop samples. A HPLC-UVD/MS with selected-ion monitoring was also provided to confirm the suspected residues. The proposed simultaneous analysis method was reproducible and sensitive enough to determine the residues of methoxyfenozide, chromafenozide and tebufenozide in agricultural commodities.

An Energy-Efficient Clustering Using Division of Cluster in Wireless Sensor Network (무선 센서 네트워크에서 클러스터의 분할을 이용한 에너지 효율적 클러스터링)

  • Kim, Jong-Ki;Kim, Yoeng-Won
    • Journal of Internet Computing and Services
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    • v.9 no.4
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    • pp.43-50
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    • 2008
  • Various studies are being conducted to achieve efficient routing and reduce energy consumption in wireless sensor networks where energy replacement is difficult. Among routing mechanisms, the clustering technique has been known to be most efficient. The clustering technique consists of the elements of cluster construction and data transmission. The elements that construct a cluster are repeated in regular intervals in order to equalize energy consumption among sensor nodes in the cluster. The algorithms for selecting a cluster head node and arranging cluster member nodes optimized for the cluster head node are complex and requires high energy consumption. Furthermore, energy consumption for the data transmission elements is proportional to $d^2$ and $d^4$ around the crossover region. This paper proposes a means of reducing energy consumption by increasing the efficiency of the cluster construction elements that are regularly repeated in the cluster technique. The proposed approach maintains the number of sensor nodes in a cluster at a constant level by equally partitioning the region where nodes with density considerations will be allocated in cluster construction, and reduces energy consumption by selecting head nodes near the center of the cluster. It was confirmed through simulation experiments that the proposed approach consumes less energy than the LEACH algorithm.

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Analysis of Multiple Pesticide Residues in Apples and Pears Using Gas-Liquid Chromatography (Gas-Liquid Chromatography를 이용한 사과 및 배 중의 농약 다성분 잔류분석법)

  • Park, Ju-Hwang;Kim, Taek-Kyum;Oh, Chang-Hwan;Kim, Jeong-Han;Lee, Young-Deuk;Kim, Jang-Eok
    • Korean Journal of Environmental Agriculture
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    • v.23 no.3
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    • pp.148-157
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    • 2004
  • A rapid analytical method was developed to determine multiple pesticide residues in apples and pears using gas-liquid chromatography (GLC). The samples were extracted with water-miscible solvents and purified by cleanup procedures serially comprising liquid-liquid partition and solid-phase extraction (SPE). Each analyte was separated and determined by a high-resolution GLC equipped with electron-capture detector (ECD) and nitrogen-phosphorous detector (NPD). A total of 196 pesticides, which were previously classified into 5 groups each for ECD and NPD based on their retention behaviors on the capillary column and responses to the detector, were subjected to the recovery experiment. In compliance with the analytical criteria, 70 to 120% of recovery and less than 20% relative standard deviation the proposed method could be successfully applied to analyze 136 and 133 pesticide residues in apples and pears, respectively, which enabled not only rapid screening but quantitation of the residues. Even though less reliability was resulted from unacceptable recovery range, rest of pesticides including 43 and 45 analyzes in apples and pears, could be also detected for their identity. The proposed method fliled to cover 17 and 18 pesticides for apples and pears, which mostly showed high polarity or heat-lability but could be suitable far fast surveilance or monitoring of fruit harvests.

Determination of mandipropamid residues in agricultural commodities using high-performance liquid chromatography with mass spectrometry (고성능액체크로마토그래피를 이용한 농산물 중 Mandipropamid의 잔류분석법 확립)

  • Kwon, Chan Hyeok;Chang, Moon Ik;Im, Moo Hyeog;Choi, Hoon;Jung, Da I;Lee, Su Chan;Yu, Jin Young;Lee, Young Deuk;Lee, Jong Ok;Hong, Moo Ki
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.518-525
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    • 2008
  • Mandipropamid is a new mandelamide-type fungicide to control foliar Oomycete pathogens in some vegetables. An analytical method was developed to determine mandipropamid residues in agricultural commodities using high-performance liquid chromatography (HPLC) and liquid chromatography/mass spectrometry (LC/MS). Mandipropamid was extracted with methanol from grape, tomato, green pepper, Chinese cabbage and potato samples. The extract was diluted with saturated sodium chloride solution and distilled water, and dichloromethane partition was followed to recover the mandipropamid from the aqueous phase. Florisil column chromatography was employed to further remove interfering co-extractives prior to HPLC analysis. Reverse-phased HPLC was successfully applied to determine mandipropamid in sample extracts with the detection at its ${\lambda}_{max}$ (223 nm). Overall recoveries of mandipropamid from fortified samples averaged $99.8{\pm}1.7$ (n=6), $89.3{\pm}5.3$ (n=6), $98.7{\pm}2.2$ (n=6), $99.7{\pm}6.8$ (n=6) and $91.1{\pm}3.1$ (n=6) for grape, tomato, green pepper, Chinese cabbage and potato, respectively. Limit of quantification of the method was 0.02~0.04 mg/kg for all samples. A LC/mass spectrometry with selected-ion monitoring was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to determine the terminal residue of mandipropamid in agricultural commodities.

Determination of Fomesafen Residue in Agricultural Commodities Using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 fomesafen의 분석)

  • Lee, Su-Jin;Hwang, Young-Sun;Kim, Young-Hak;Nam, Mi-Young;Hong, Seung-Beom;Yun, Won-Kap;Kwon, Chan-Hyeok;Do, Jung-A;Im, Moo-Hyeog;Lee, Young-Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.14 no.2
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    • pp.95-103
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    • 2010
  • Fomesafen is a selective herbicide, and used to control annual and perennial broad-leaf grass on soybean and fruit fields in USA and China, but not introduced in Korea yet. So, MRL (Maximum Residue Level), and analytical method of fomesafen were not establishment in Korea. Therefore, this experiment was conducted to establish a determination method for fomesafen residue in crops using HPLC-UVD/MS. Fomesafen residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, apple, green pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover fomesafen from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The fomesafen was quantitated by HPLC with UVD, using a Shiseido CAPCELL-PAK UG C18 column. The crops were fortified with fomesafen at 3 levels per crop. Mean recovery ratio were ranged from 87.5% for a 0.4 ppm in hulled rice to 102.5% for a 0.4 ppm in apple. The coefficients of variation were ranged from 0.6% for a 2.0 ppm in hulled rice to 7.7% for a 0.04 ppm in green pepper. Quantitative limit of fomesafen was 0.04 mg/kg in representative 5 crop samples. A LC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fomesafen in agricultural commodities.

Simultaneous Pesticide Analysis Method for Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor and Trifluralin Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor 및 Trifluralin의 동시 분석)

  • Ahn, Kyung Geun;Kim, Gi Ppeum;Hwang, Young Sun;Kang, In Kyu;Lee, Young Deuk;Choung, Myoung Gun
    • Korean Journal of Environmental Agriculture
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    • v.37 no.2
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    • pp.104-116
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    • 2018
  • BACKGROUND: This experiment was conducted to establish a simultaneous analysis method for 7 kinds of herbicides in 3 different classes having similar physicochemical property as diphenyl ether(bifenox and oxyfluorfen), dinitroaniline (ethalfluralin and trifluralin), and chloroacetamide (metolachlor, pretilachlor, and thenylchlor) in crops using GC-ECD/MS. METHODS AND RESULTS: All the 7 pesticide residues were extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and directly partitioned into n-hexane/dichloromethane(80/20, v/v) to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. The analytes were separated and quantitated by GLC with ECD using a DB-1 capillary column. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop samples fortified with bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries of the 7 pesticide residues ranged from 75.7 to 114.8% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of the analytes were 0.004 (etahlfluralin and trifluralin), 0.008 (metolachlor and pretilachlor), 0.006 (thenylchlor), 0.002 (oxyfluorfen), and 0.02 (bifenox) mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residues. Therefore, this analytical method was reproducible and sensitive enough to determine the residues of bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin in agricultural commodities.

Effects of Dietary Beef Tallow, Soybean Oil and Squid Liver Oil on Growth and Body Composition of the Korean Rockfish Sebastes schlegeli, and Biochemical Changes with Starvation (사료 지질원으로 우지, 대두유 및 오징어 간유 첨가에 따른 조피볼락 Sebastes schlegeli의 성장 및 체성분 변화와 절식시 체내 대사)

  • LEE Sang-Min
    • Journal of Aquaculture
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    • v.7 no.1
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    • pp.63-76
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    • 1994
  • The effects of different dietary lipids on growth, body chemical composition, and nutrient partition of the Korean rockfish (43 g of initial mean weight) were studied. Fish were fed three experimental diets containing 1) $4.5\%$ squid liver oil, 2) $1\%$ squid liver oil and $3.5\%$ beef tallow, and 3) $1\%$ squid liver oil and $3.5\%$ soybean oil. Growth and feed efficiency were detarmined during a 19-week feeding period at water temperature of $15.5^{\circ}C$, and at the end of which body chemical compositions were analyzed. Remained fish were fasted for 45 days, and four fish were taken at 6, 12 and 24 hours, and 3, 15 and 45 days after the fasting to determine tissue compositions and hematological changes. Growth, feed efficiency, protein and lipid retention efficiency, hepatosomatic index(HSI), viscerosomatic index (VSI), and chemical composition of whole body and dorsal muscle were not affected by the different dietary lipids. Liver moisture content of fish fed squid liver oil diet was higher than that of fish fed beef tallow or soybean oil diet. Liver lipid content of fish fed beef tallow diet was higher than that of fish fed the other diets. Fatty acid composition of dorsal muscle and liver were affected by the different dietary lipids ; high levels of 20 : 5n-3 and 22 : 6n-3 from fish fed the diet containing squid liver oil, 18 : 1 from fish fed the diet containing beef tallow, and high 18 : 2n-6 and 18 : 3n-3 from fish fed the diet containing soybean oil were observed. Both HSI and VSI of fish fed three diets decreased with time after the begining of starvation. Liver glycogen did not change during the first 15 days of starvation and decreased thereafter, and that was not affected by the different dietary lipids. Lipid and protein contents in the dorsal muscle of fish decreased up to 15 days of starvation and remained unchanged thereafter, these were not different from each other. Glucose, free fatty acid, triglyceride and phospholipid concentrations in Fish serum were varied for the first 15 days of starvation, after that the concentrations of fish serum remained relatively stable in all the treatment groups with prolonged starvation. The results indicate that Korean rockfish can utilize fish oil, animal fat or vegetable oil equally as energy source when n-3HUF A is adquate.

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