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Determination of Oxycarboxin Residues in Agricultural Commodities Using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 Oxycarboxin의 분석)

  • Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.37 no.2
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    • pp.117-124
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    • 2018
  • BACKGROUND: Oxycarboxin(5,6-dihydro-2-methyl-N-phenyl-1,4-oxathiin-3-carboxamide-4,4-dioxide) as oxanthiin is a systemic fungicide commonly used for control of various pathogens in agronomic and horticultural crops. In an effort to develop an analytical method to trace the fungicide, a method using HPLC equipped with UVD/MS was studied. METHODS AND RESULTS: Oxycarboxin was extracted with acetone from hulled rice, soybean, Kimchi cabbage, green pepper, and apple samples. The extract was diluted with saline water, followed by liquid-liquid extraction with methylene chloride. Florisil column chromatography was employed for the purification of the extracts. Oxycarboxin was determined on a Zorbax SB-AQ $C_{18}$ column by HPLC with UVD. Accuracy of the proposed method was validated by the recovery tests from crop samples fortified with oxycarboxin at 3 levels per crop. CONCLUSION: Mean recoveries ranged from 78.3% to 96.1% in five representative agricultural commodities. The coefficients of variation were less than 10%, and limit of quantitation of oxycarboxin was 0.04 mg/kg. A confirmatory technique using LC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. The method was reproducible and sensitive to determine the residue of oxycarboxin in agricultural commodities.

Analysis of gibberellic acid from fruits using HPLC/UV-vis (HPLC/UV-vis을 이용한 과일류 중의 지베렐린 산 분석)

  • Ma, Kyung Na;Cho, Hyun-Woo;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.26 no.1
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    • pp.19-26
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    • 2013
  • Gibberllic acid ($GA_3$) is one of gibberellins (GAs) that are a class of plant growth hormones that exert profound and diverse effects on plant growth and development. $GA_3$ is essentially non-UV absorbing and is difficult to assay by UV-detector. For effective extraction of gibberellic acid from fruits by using liquid-liquid extraction, optimized pH and extraction solvent were established. The selective and sensitive derivative of $GA_3$ for HPLC/UV-vis was derivatized using phenacyl bromide, and the experimental factors, including reaction time, reaction temperature and amount of derivatizing reagent and base were investigated for the effective synthesis. The derivatized $GA_3$ with phenacyl bromide was effectively analyzed by HPLC/UV-vis. The structure of derivatized $GA_3$ was confirmed by HPLC/ESI-MS. For apple, LOD and LOQ were 0.008 mg/kg and 0.027 mg/kg, respectively. For pear, LOD and LOQ were 0.003 mg/kg, 0.012 mg/kg, respectively. The established method can be applied to more effective analysis of $GA_3$ from plant and food.

HPLC-based Analysis of Biogenic Amines in Aging-Cheese (HPLC를 이용한 숙성치즈로부터 바이오제닉 아민 분석법 개발)

  • Park, Jong-Hyuk;Lee, Sang-Cheon;Moon, Hye-Jung;Oh, Jeon-Hui;Song, Gi-Bong
    • Journal of Dairy Science and Biotechnology
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    • v.34 no.3
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    • pp.187-191
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    • 2016
  • Biogenic amines have been used as chemical indicators of fermented foods. So far, several chromatography methods have been developed to detect biogenic amines in foods. However, few methods have identified these compound in domestic cheese. We analyzed the biogenic amines (histamine dihydrochloride, tyramine hydrochloride, ${\beta}$-phenylethylamine hydrochloride, putrescine dihydrochloride, cadaverine, spermidine, tryptamine hydrochloride, ethanolamine hydrochloride and butylamine) in cheese by using HPLC. The calibration curves of the biogenic amines were found to be linear over the concentration range of 10-50 ppm with a correlation coefficient of above 0.99. The limit of detection (LOD) and limit of quantitation (LOQ) of the biogenic amines in the given order were 3.7 and 11.3 ppm, 3.4 and 10.4ppm, 3.4 and 10.3 ppm, 4.0 and 12.2 ppm, 3.4 and 10.4 ppm, 3.4 and 10.5 ppm, 3.5 and 10.7 ppm, 4.1 and 12.5 ppm, and 3.4 and 10.4 ppm, respectively. Recovery rates of the biogenic amines in the given order were 112, 104, 93, 108, 91, 102, 101, and 92%, respectively. The findings of this study suggest that HPLC is a suitable method for the determination of biogenic amines, thereby indicating its potential application in the quality control of aging cheese.

Development of Individual Residue Analysis Method for Cyanazine in Agricultural Commodities as an Unregistered Herbicide in Korea (국내 미등록 제초제 cyanazine의 농산물 중 개별 잔류분석법 개발)

  • Choung, Myoung-Gun;Im, Moo-Hyeog
    • The Journal of the Korean Society of International Agriculture
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    • v.30 no.4
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    • pp.339-346
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    • 2018
  • Cyanazine is a member of the triazine family of herbicides. Cyanazine is used as a pre- and post-emergence herbicide for the control of annual grasses and broadleaf weeds. This experiment was conducted to establish a determination method for cyanazine, as domestic unregistered pesticide, residue in major agricultural commodities using HPLC-DAD/MS. Cyanazine 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 saline water and partitioned to dichloromethane for remove polar extractive 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 a $C_{18}$ column in HPLC, cyanazine was successfully separated from co-extractives of sample, and sensitively quantitated by diode array detection at 220 nm. Accuracy and precision of the proposed method was validated by the recovery experiment on every major agricultural commodity samples fortified with cyanazine at 3 concentration levels per agricultural commodity in each triplication. Mean recoveries were ranged from 83.6 to 93.3% in five major representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation(LOQ) of cyanazine was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring(SIM) technique was also provided to clearly identify the suspected residue.

Determination of Amisulbrom Residues in Agricultural Commodities Using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 Amisulbrom의 잔류분석)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Kim, Min-Ji;Hwang, Young-Sun;Hong, Seung-Beom;Lee, Young Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.321-329
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    • 2014
  • This experiment was conducted to establish an analytical method for residues of amisulbrom, as recently developed an oomycete-specific fungicide showing inhibition of fungal respiration, in crops using HPLC-UVD/MS. Amisulbrom residue was extracted with acetonitrile from representative samples of five raw products which comprised apple, green pepper, kimchi cabbage, potato and hulled rice. The extract was diluted with 50 mL of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice sample, 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, amisulbrom was successfully separated from sample co-extractives and sensitively quantitated by ultraviolet absorption at 255 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery test on every crop samples fortified with amisulbrom at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 85.3% to 105.6% 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 amisulbrom was 0.04 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. The proposed method was sensitive, reproducible and easy-to-operate enough to routinely determine the residue of amisulbrom in agricultural commodities.

Development of an Official Method for Measurement of Fluazinam Residues for Quarantine of Imported and Exported Horticultural Products (수출입 원예작물의 검역을 위한 살균제 Fluazinam의 공정 잔류분석법 개발)

  • Kim, Gyeong-Ha;Ahn, Kyung-Geun;Kim, Gi-Ppeum;Hwang, Young-Sun;Chang, Moon-Ik;Kang, In-Kyu;Lee, Young Deuk;Choung, Myoung-Gun
    • Horticultural Science & Technology
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    • v.34 no.1
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    • pp.183-194
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    • 2016
  • This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was $0.004mg{\cdot}kg^{-1}$ in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.

Development of Analytical Method for Fipronil Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Fipronil의 잔류 분석법 개발)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;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.34 no.4
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    • pp.309-317
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    • 2015
  • BACKGROUND: An analytical method was developed using GC-ECD/MS to precisely determine the residue of fipronil, a phenylpyrazole insecticide used to control a wide range of foliar and soil-borne pests.METHOD AND RESULTS: Fipronil residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and fipronil was partitioned into n-hexane/dichloromethane (20/80, v/v) to remove polar co-extractives in the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fipronil was separated and quantitated by GC-ECD using a DB-17 capillary column. Accuracy of the proposed method was validated by the recovery from crop samples fortified with fipronil at 3 levels per crop in each triplication.CONCLUSION: Mean recoveries ranged from 86.6% to 106.0% in five representative agricultural commodities. The coefficients of variation were less than 10%. Limit of quantitation of fipronil was 0.004 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 residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fipronil in agricultural commodities.

Determination of Quintozene Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Quintozene의 잔류분석)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Hwang, Young-Sun;Hong, Seung-Beom;Lee, Young Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.195-203
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    • 2015
  • Quintozene, pentachloronitrobenzene (PCNB) is a contact fungicide for control of soilborne phytopathogenic fungi during cultivation of diverse crops. It was introduced to agricultural use around 1930's as a substitute for mercurial disinfectants. Although quintozene had been first registered in Korea on 1969. However, now it was banned to use due to its high residue levels in selected harvest products. Also, high possibility is expected that the residue may be contained in imported agricultural commodities as it is still used widely over the world. Therefore, this study was conducted to establish a determination method for quintozene residue in crops using GC/ECD/MS. Quintozene residue was extracted with acetonitrile from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and n-hexane partition was followed to recover quintozene from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The quintozene was quantitated by GLC with ECD, using a DB-1 capillary column. The crops were fortified with quintozene at 3 levels per crop. Mean recoveries ranged from 79.9% to 102.7% in five representative agricultural commodities. The coefficients of variation were less than 4.3%. Quantitative limit of quintozene was 0.004 mg/kg in representative five crop samples. A GC/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 quintozene in agricultural commodities.