GC-ECD를 이용한 한약재 길경(Platycodi Radix) 중 살균제 Prochloraz의 분석
Analysis of Fungicide Prochloraz in Platycodi Radix by GC-ECD
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초록
BACKGROUND: Prochloraz has been widely used as an imidazole fungicide on fruits and vegetables in Korea. Analytical approaches to evaluate prochloraz residues in herbal medicine are required for their safety management. In this study, we developed a GC-ECD method for quanti-tative determination of prochloraz in Platycodi Radix. The metabolite 2,4,6-trichlorophenol (2,4,6-T) was used as a target compound to evaluate total prochloraz residues as it is categorized to a representative residue definition of prochloraz. All residues containing 2,4,6-T were con-verted to 2,4,6-T and subjected to GC-ECD. METHODS AND RESULTS: In order to verify the ap-plicability, the method was optimized for determining prochloraz and it metabolite 2,4,6-T in Platycodi Radix. Prochloraz and its metabolite 2,4,6-T residuals were ex-tracted using acetone. The extract was diluted with and partitioned directly into dichloromethane to remove polarco-extractives in the aqueous phase. The extract was de-composed to 2,4,6-T, and then the partitioned ion-asso-ciate was finally purified by optimized aminopropyl sol-id-phase extraction (SPE). The limits of quantitation of the method (MLOQs) were 0.04 mg/kg and 0.02 mg/kg, respectively for prochloraz and 2,4,6-T, considering the maximum residue level (MRL) of prochloraz as 0.05 mg/kg in Platycodi Radix. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and re-sulted in good recoveries (82.1-89.7%). Good repro-ducibilities were obtained (coefficient of variation < 2.8%), and the linearities of calibration curves were rea-sonable (r2 > 0.9986) in the range of 0.005-0.5 μg/mL. CONCLUSION(S): The method developed in this study was successfully validated to meet the guidelines re-quired for quantitative determination of pesticides in herbal medicine. Thus, the method could be useful to monitor prochloraz institutionally in herbal medicine.
Abstract
BACKGROUND: Prochloraz has been widely used as an imidazole fungicide on fruits and vegetables in Korea. Analytical approaches to evaluate prochloraz residues in herbal medicine are required for their safety management. In this study, we developed a GC-ECD method for quanti-tative determination of prochloraz in Platycodi Radix. The metabolite 2,4,6-trichlorophenol (2,4,6-T) was used as a target compound to evaluate total prochloraz residues as it is categorized to a representative residue definition of prochloraz. All residues containing 2,4,6-T were con-verted to 2,4,6-T and subjected to GC-ECD. METHODS AND RESULTS: In order to verify the ap-plicability, the method was optimized for determining prochloraz and it metabolite 2,4,6-T in Platycodi Radix. Prochloraz and its metabolite 2,4,6-T residuals were ex-tracted using acetone. The extract was diluted with and partitioned directly into dichloromethane to remove polarco-extractives in the aqueous phase. The extract was de-composed to 2,4,6-T, and then the partitioned ion-asso-ciate was finally purified by optimized aminopropyl sol-id-phase extraction (SPE). The limits of quantitation of the method (MLOQs) were 0.04 mg/kg and 0.02 mg/kg, respectively for prochloraz and 2,4,6-T, considering the maximum residue level (MRL) of prochloraz as 0.05 mg/kg in Platycodi Radix. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and re-sulted in good recoveries (82.1-89.7%). Good repro-ducibilities were obtained (coefficient of variation < 2.8%), and the linearities of calibration curves were rea-sonable (r2 > 0.9986) in the range of 0.005-0.5 μg/mL. CONCLUSION(S): The method developed in this study was successfully validated to meet the guidelines re-quired for quantitative determination of pesticides in herbal medicine. Thus, the method could be useful to monitor prochloraz institutionally in herbal medicine.
참고문헌 (13)
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