• Korean Journal of Environmental Agriculture
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• v.40 no.4
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• pp.353-358
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• 2021

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 quantitative 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 converted to 2,4,6-T and subjected to GC-ECD. METHODS AND RESULTS: In order to verify the applicability, 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 extracted using acetone. The extract was diluted with and partitioned directly into dichloromethane to remove polar co-extractives in the aqueous phase. The extract was decomposed to 2,4,6-T, and then the partitioned ion-associate was finally purified by optimized aminopropyl solid-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 resulted in good recoveries (82.1-89.7%). Good reproducibilities were obtained (coefficient of variation < 2.8%), and the linearities of calibration curves were reasonable (r² > 0.9986) in the range of 0.005-0.5 ㎍/mL. CONCLUSION(S): The method developed in this study was successfully validated to meet the guidelines required for quantitative determination of pesticides in herbal medicine. Thus, the method could be useful to monitor prochloraz institutionally in herbal medicine.

• The Korean Journal of Pesticide Science
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• v.15 no.2
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• pp.114-124
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• 2011

The characteristics of pesticide residues by multiresidue analysis method using GC, HPLC and GC-MSD were examined for 18,069 numbers of 91 kinds of vegetables in Seoul from 2007 to 2009. Detection rates of pesticide residues were 11.2% in 2007, 8.5% in 2008 and 12.0% in 2009, respectively, and the excess rates of Maximum Residue Limits (MRLs) showed a declining tendency as 4.6% in 2007, 2.8% in 2008 and 2.1% in 2009, respectively. The pesticides exceeding MRLs were 43 ingredients in 2007, 30 ingredients in 2008 and 36 ingredients in 2009, respectively. The frequencies of pesticides exceeding MRLs were 71 of azoxystrobin in 2007, 29 of procymidone in 2008, 24 of endosulfan in 2009, respectively. The excess rate of mustard green for MRLs in comparison with sample numbers was the highest among vegetables analyzed more than 10 cases each year. As a result of comparing annually pesticide residues about pesticide ingredients showed high frequency rates for pesticide detection, there was a statistical significance for the detection quantities of diazinon, endosulfan, paclobutrazol and procymidone.

• Journal of the Korean Society of Food Science and Nutrition
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• v.39 no.8
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• pp.1165-1170
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• 2010

A method for the determination of four pesticide compounds, urea (isoproturon), bis-carbamate (phenmedipham), thiocarbamate (pyridate) and vinyllidenediamine (nitenpyram) were examined and analyzed by HPLC with C-18 column ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size). Mobile phase consisted of deionized water, acetonitrile and 50 mM $KH_2PO_4$ (pH 2.5). Isoproturon and phenmedipham analytical condition was isocratic elution of the column with 50% solvent A (acetonitrile) and 50% solvent B (deionized water); pyridate was 85% solvent A (acetonitrile) and 15% solvent B (deionized water) at a flow rate of 1 mL/min; and nitenpyram analytical condition was 90% solvent A (50 mM $KH_2PO_4$, pH 2.5) and 10% solvent B (acetonitrile) at a flow rate of 1 mL/min. In results, retention times were 6.12, 8.63, 9.40 and 12.76 min for isoproturon, phenmedipham, pyridate and nitenpyram, respectively. All injection volumes were $10\;{\mu}L$ and the limit of quantitation was 0.05 mg/kg for four pesticide compounds, respectively. Recovery rate test was performed with three farm products, rice, apple and soybean. Four pesticide compounds were spiked at concentrations of 0.05, 0.1 and 0.5 mg/kg. The recovery rates were ranged from 70.18% to 118.08% and the standard deviations of all experiments were within 10%.