首页> 外文期刊>Journal of AOAC International >Development and Validation of an HPLC Method for Determination of Spirotetramat and Spirotetramat cis enol in Various Vegetables and Soil
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Development and Validation of an HPLC Method for Determination of Spirotetramat and Spirotetramat cis enol in Various Vegetables and Soil

机译:高效液相色谱法测定各种蔬菜和土壤中螺四灵和螺四灵的方法的建立和验证

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摘要

An easy and simple analytical method was standardized and validated for the estimation of residues of spirotetramat and its metabolite spirotetramat cis enol in various substrates: okra fruits, brinjal leaves and fruits, green chili, red chili, and soil. The samples were extracted with acetonitrile, diluted with brine solution, partitioned into dichloromethane, dried over anhydrous sodium sulfate, and cleaned up by treatment with activated charcoal powder. Final clear extracts were concentrated undervacuum and reconstituted with HPLC grade acetonitrile. Residues were estimated using HPLC with a photodiode array detector and a C_(18) column, and confirmed by HPTLC. Acetonitrile was used as the mobile phase at 0.4 mL/min. Both spirotetramat and spirotetramat cis enol presented distinct peak at retention times of 8.518 and 7.598 min, respectively. Consistent recoveries ranging from 82 to 97% for spirotetramat and spirotetramat cis enol were observed when samples were spiked at 1.00 to 0.03 mg/kg levels. The LOQ of the method was found to be 0.03 mg/kg. The analytical method was validated in terms of parameters, including selectivity, linearity, precision, and accuracy.
机译:标准化了一种简便易行的分析方法,并对其在各种基质(秋葵果实,茄子叶和果实,绿色辣椒,红色辣椒和土壤)中估计螺旋藻及其代谢产物螺旋藻顺式烯醇的残留量进行了验证。样品用乙腈萃取,用盐水溶液稀释,分配到二氯甲烷中,用无水硫酸钠干燥,并用活性炭粉末处理进行净化。将最终澄清的提取物在真空下浓缩,并用HPLC级乙腈重构。使用带光电二极管阵列检测器的HPLC和C_(18)色谱柱估算残留物,并通过HPTLC确认。乙腈以0.4 mL / min的流速用作流动相。螺旋体和螺旋体顺式烯醇均在保留时间分别为8.518和7.598分钟处呈现出明显的峰。当样品加标浓度为1.00至0.03 mg / kg时,可以观察到螺四溴甲烷和螺四溴甲烷顺式烯醇的回收率从82%到97%不等。该方法的最低定量限为0.03 mg / kg。该分析方法已通过参数验证,包括选择性,线性,精密度和准确性。

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