气相色谱- ecd分析桔黄中杀菌剂丙氯嗪的含量

Gyeong-Seok Oh, Myung-sub Yoon Myung-sub Yoon, Seung-Hyun Yang, Hoon Choi
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引用次数: 0

摘要

背景:在韩国,咪唑类杀菌剂被广泛用于水果和蔬菜。中药中丙氯嗪残留的分析评价方法是对其进行安全管理的必要条件。本研究建立了一种气相色谱- ecd法定量测定桔梗中丙氯嗪的方法。代谢物2,4,6-三氯酚(2,4,6- t)被归类为丙氯嗪的代表性残留定义,因此被用作评估丙氯嗪总残留的目标化合物。所有含有2,4,6- t的残基转化为2,4,6- t,并进行GC-ECD。方法与结果:为验证该方法的适用性,对该方法进行了优化,以测定桔黄中丙氯嗪及其代谢物2,4,6- t的含量。用丙酮法提取丙氯嗪及其代谢物2,4,6- t残渣。提取液用二氯甲烷稀释并直接分馏,以去除水相中的极性共萃取物。将提取液分解为2,4,6- t,通过优化后的氨丙基固相萃取(SPE)纯化分离的离子缔合物。本方法的定量限(MLOQs)分别为0.04 mg/kg和0.02 mg/kg,考虑到原氯嗪在黄芪中的最大残留限量(MRL)为0.05 mg/kg。在两种浓度(MLOQ和10 MLOQ)下进行了回收率试验,回收率为82.1 ~ 89.7%。方法重复性好(变异系数< 2.8%),在0.005 ~ 0.5 μg/mL范围内线性合理(r2 > 0.9986)。结论:所建立的方法符合中草药中农药的定量测定标准。因此,该方法可用于中草药中丙氯嗪的制度监测。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Analysis of Fungicide Prochloraz in Platycodi Radix by GC-ECD
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 μg/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.
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