• Title/Summary/Keyword: I-partition

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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.

Effect of Breed (Lean or Fat Pigs) and Sex on Performance and Feeding Behaviour of Group Housed Growing Pigs in a Tropical Climate

  • Renaudeau, D.;Giorgi, M.;Silou, F.;Weisbecker, J.L.
    • Asian-Australasian Journal of Animal Sciences
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    • v.19 no.4
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    • pp.593-600
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    • 2006
  • The effects of breed and sex on individual growth performance and feeding behaviour were studied between 45 and 90 kg BW in two replicates of forty group-housed pigs. The first and the second replicates were carried out during the warm season (i.e. between February and April 2003) and during the hot season (i.e. between August and October 2003), respectively. During the warm season, ambient temperature and relative humidity averaged $25.3^{\circ}C$ and 86.0%. The corresponding values for the hot season were $27.9^{\circ}C$ and 83.6%. The pigs were grouped in pens of 10 animals on the basis of breed (Creole or Large White) and sex (gilt or castrated male) and given ad libitum access to a grower diet (9.0 MJ/kg net energy and 158 g/kg crude protein) via feed intake recording equipment (Acema 48). An ear-tag transponder was inserted into each pig and this allowed the time, duration, and size of individual visits to be recorded. The growth performance and feeding pattern were significantly affected by breed, sex, and season. The Creole pigs (CR) had a lower average daily gain (ADG) (642 vs. 861 g/d, p<0.01) and carcass lean content ($LC_{90kg}$) (35.4 vs. 54.5%; p<0.01) and a higher backfat thickness at 90 kg BW ($BT_{90kg}$) (23.4 vs. 10.4 mm; p<0.01) than Large White pigs (LW) whereas the average daily feed intake (ADFI) was not affected by breed (2.34 vs. 2.22 kg/d, respectively for CR and LW pigs; p>0.10). Consequently, the food:gain ratio was higher in CR than in LW (3.65 vs. 2.58; p<0.01). CR had less frequent meals but ate more feed per meal than LW (5.9 vs. 8.8 meals/d and 431 vs. 279 g/meal; p<0.01). The rate of feed intake was lower (27.6 vs. 33.9 g/min; p<0.01) and the ingestion time per day and per meal were higher in CR than in LW (87.1 vs. 69.7 min/d and 15.8 vs. 8.4 min/meal; p<0.01). The ADFI and BT90 kg were higher (2.38 vs. 2.17 kg/d and 18.1 vs. 15.9 mm; p<0.05) and LC90 kg was lower (43.5 vs. 46.4%; p<0.01) in castrated males (CM) than in gilts (G) whereas ADG was not affected by sex (p = 0.12). The difference in lean content between CM and G was greater in CR than in LW. The ADFI and ADG were reduced during the hot season (2.18 vs.2.38 kg/d and 726 vs. 777 g/d, respectively; p<0.05) whereas feed conversion and carcass lean content were not affected by season (p>0.05). Average feeding time per meal and meal size decreased during the hot season (10.9 vs. 13.2 min/meal and 316 vs. 396 g/meal; p<0.01) whereas the rate of feed intake was not affected by season (p = 0.83). On average, 0.69 of total feed intake was consumed during the diurnal period. However, this partition of feed intake was significantly affected by breed, sex, and season. In conclusion, the breed, sex and season significantly affect performance and feeding pattern in growing pigs raised in a tropical climate. Moreover, the results obtained in the present study suggest that differences observed in BW composition between CR and LW are associated with difference in feeding behaviour, in particular, the short-term regulation of feed intake.

Residue Studies of Difenoconazole and Thiamethoxam during Cultivation of Sweet Persimmon for Export (수출용 단감에 대한 Difenoconazole과 Thiamethoxam의 잔류특성 연구)

  • Chang, Hee-Ra;Kang, Hae-Rim;Do, Jung-A;Oh, Jae-Ho;Hwang, In-Kyun;Kwon, Ki-Sung;Im, Moo-Hyeog;Kim, Kyun
    • Korean Journal of Environmental Agriculture
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    • v.31 no.3
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    • pp.248-254
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    • 2012
  • BACKGROUND: In order to elucidate residual characteristics of difenoconazole and thiamethoxam by treatment to sweet persimmons for one year and to generate the data for the maximum residue limit (MRL) establishment for those pesticides in or on sweet persimmon. METHODS AND RESULTS: Systemic fungicide difenoconazole WP (10% a.i.) and systemic insecticide thiamethoxam WG (10% a.i.) were sprayed onto 12~25-years-old sweet persimmons according to its preharvest interval (PHI), respectively, and then fresh sweet persimmons were harvested at 0, 1, 3, 7, 14, 21 days after treatment from pesticide-sprayed plots at each 3 sites. The analytical methods were evaluated to limit of quantification, linearity, specificity, reproducibility and recoveries. The crop samples were extracted with acetone and performed dichloromethane partition process. The extracted samples of difenoconazole were analyzed by GC-ECD and the thiamethoxam extracted samples were analyzed by HPLC with good sensitivity and selectivity of the method. The average recoveries of difenoconazole ranged from 87.5 to 99.5% with the percentage of coefficient variation in the range 4.1~7.6% at three different spiking levels(0.02, 0.2 and 2.0 mg/kg). And the average recoveries of thiamethoxam and clothianidin ranged from 88.8 to 98.9% and 83.2 to 96.6% with the percentage of coefficient variation in the range 3.6~5.0% and 3.8~9.4% at three different spiking levels(0.02, 0.2 and 2.0 mg/kg), respectively. The residue amounts ranges of difenoconazole were 0.2~0.56 mg/kg and the residue amount was decreased below the MRL level, 1.0 mg/kg, after 1 day harvest. The residue amounts ranges of thiamethoxam were 0.08~0.28 mg/kg and the residue amount was decreased below the MRL level, 0.5 mg/kg, after 1 day harvest. And the residue amount of clothianidin was below then 0.03 mg/kg for only one test site of 14 and 28 day samples. CONCLUSION: As a result, the residual amounts of difenoconazole and thiamethoxam were not exceeded the MRL of established criteria for sweet persimmon. The biological half-lives of difenoconazole and thiamethoxam were 13.6, 19.4, 16.3 and 10.0, 15.3, 14.0 days at each three test sites, respectively.

Development of Analytical Method for the Determination and Identification of Unregistered Pesticides in Domestic for Orange and Brown Rice(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide- (식품공전 분석법 미설정 농약의 잔류분석법 확립(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide-)

  • Chang, Hee-Ra;Kang, Hae-Rim;Kim, Jong-Hwan;Do, Jung-A;Oh, Jae-Ho;Kwon, Ki-Sung;Im, Moo-Hyeog;Kim, Kyun
    • Korean Journal of Environmental Agriculture
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    • v.31 no.2
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    • pp.157-163
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    • 2012
  • BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl, clomeprop, diflufenican, hexachlorobenzene, picolinafen, and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02~0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were $R^2$ >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2~8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2~6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.

Preferential Flow as Tested by Breakthrough Curves of Cl- and Cu2+ from Saturated Undisturbed Soil Core Samples under Steady Flow Conditions (포화 불교란 토양시료의 Cl- 및 Cu2+ 출현곡선에 의한 preferential flow의 검증)

  • Yoo, Sun-Ho;Han, Kyung-Hwa;Ro, Hee-Myong;Han, Gwang-Hyun
    • Korean Journal of Soil Science and Fertilizer
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    • v.33 no.2
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    • pp.71-78
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    • 2000
  • Preferential flow has recently been the subject of increasing interest because these phenomena contribute to solute transport in soils. Commonly, preferential flow paths are associated with macropores or highly structured soils. We presented an analysis of the measured breakthrough curves (BTCs) of $Cl^-$ and $Cu^{2+}$ ions to test the occurrence of preferential flow in soils using miscible displacement technique under steady flow conditions. We also analyzed soil water retention curves and from this curves induced cumulative pore size distribution of undisturbed soils, which sampled from Ap1, B1, and C horizons of Songjeong series soils (the fine loamy, mesic family of Typic Hapludults). In this study, miscible displacement experiment on C horizon was excluded, because it is structureless sandy loam with saturated hydraulic conductivity of $5.2cmhr^{-1}$. The saturated hydraulic conductivity of Ap1 horizon was $2.0cmhr^{-1}$, which was about 7 times higher than that of B1 horizon ($0.27cm hr^{-1}$). Cumulative pore size distribution predicted that Ap1 horizon had more macropores (pore diameter larger than $49{\mu}m$, equivalent to -6 kpa of soil matric potential) than B1 horizon. The hydrodynamic dispersion coefficient from chloride BTCs was estimated as $1.3cm^2hr^{-1}$ for B1 and $34cm^2hr^{-1}$ for Ap1 horizon. However the retardation factors of B1 and Ap1 horizon were significantly different, i.e. 1 and 0.6, respectively, which means that there was distinct partition between mobile water and immobile phase in Ap1 horizon. The copper retardation effect of Ap1 horizon was less than that of B1 horizon, even though cation exchange capacity of Ap1 horizon was higher than that of B1 horizon. Thus, breakthrough curves of $Cl^-$ and $Cu^{2+}$ obviously showed the probability that preferential flow would occur in Ap1 horizon.

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The Biochemical Studies on Stored Soy-sauce (저장(貯藏)간장의 생화학적(生化學的) 연구(硏究))

  • Chang, Chi-Hyun
    • Applied Biological Chemistry
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    • v.9
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    • pp.9-27
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    • 1968
  • Studies were carried out in order to elucidate chemical components and microflora in three types of soy-sauce, 12-year aged soy-sauce prepared by improved method. 7-year aged and 20-year aged soy-sauce prepared by ordinary method. They results are summarized as follows: 1. The followings are found to be the important factors affecting the quality of soy sauce. a. Organic acids, reducing sugars and free amino acids were increased in the course of storage. b. In the aged soy-sauces under study non-volatile organic acid increased while volatile organic acid decreased and the total acidity was dependent only upon tie latter. c. It was found that suit concentration decreased during the storage. 2. The results of investigation of microflora in the stored soy-sauce are shown as follows. Soy-sauce Improved Ordinary Microbe 12-Y. 20-Y. 7-Y. Aerobic bacteria colony/1ml. 6 123 2 Halophilic lactic acid bacteria colony/1ml. 4 6 10 Osmophilic yeast colony/1ml. $828{\times}10^4$ 248 - b. In the stored soy-sauces, aerobic bacteria are incapable of growing due to drop in pH value and the influence of salt concentration. c. Halophilic lactic acid bacteria are incapable of growing due to drop in pH value, even the salt concentrations decreased during the storage. d. Osmophilic yeast are still growing in low pH value and in the decreasing salt concentration during the strage. 3. The results of amino acid analysis by paper partition chromatographic and calorimetric methods are shown as follows. a. Fourteen kinds of amino acid and thirteen amino acids were detected in the soy-sauce of 12-year aged improved soy-sauce and 7-year aged and 20-year aged ordinary one, respectively. b. The contents of aspartic acid, glutamic acid, serine, valine, leucine, lysine, histidine and methionine increased in the 20-year aged ordinary soy-sauce compared to the 7-year aged one. On the other hand those of alanine, tyrosine, phenylalanine and cystine decreased. 4. The results of sugar analysis by paper chromatography are as follows. a. In the 12-year aged improved soy-sauce, galactose, glucose, arabinose, xylose, rhamnose, maltose and an unknown were detected, and their amounts were in the above order except maltose and an unknown. b. Both in the 7 and 12-year aged ordinary soy-sauces, galactose, arabinose, xylose, glucose and rhamnose were detected and the amounts of the sugars were in the above order. c. In the non-aged ordinary soy-sauce, glucose was not detected but detected from 7-year and 20-year aged ordinary soy-sauce. 5. The results of organic acid analysis by paper chromatography were as follows. a. As volatile acids, acetic, propionic and butyric acids were detected in the 7-year aged ordinary soy-sauce. On the other hand in both the 20-year aged ordinary soy-sauce and the 12-year aged improved ones, only acetic acid was abundant while propionic and butyric acids were round in trace. It was found that propionic and butyric acids, as the unpleasant flavor components, decreased during the storage. b. In the ordinary soy-sauce, citric acid were produced during the storage and lack, malic and tartaric acids increased in the course of aging while succinic, glycolic, fumaric and malonic acids were shown to decrease. Glutaric and oxalic acids disappeared. Citric acid was produced also in the improved soy-sauce, but lactic, tartaric, succinic, malic, and glycolic acids decreased, while both malonic and glutaric acids disappeared. From the above results the citric acid production was considered to be a favorable factor for the taste. c. In the aged soy-sauces, pyruvic, α-ketoglutaric and probably acetoacetic and oxaloacetic acids (both in trace) were present and their amounts were in the above order. All of the α-keto acid abruptly decreased during the storage.

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