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首页> 外文期刊>Journal of AOAC International >Determination of Pesticides in Water Samples from the Wieprz-Krzna Canal in the Leczynsko-Wlodawskie Lake District of Southeastern Poland by Thin-Layer Chromatography with Diode Array Scanning and High-Performance Column Liquid Chromatography withDio
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Determination of Pesticides in Water Samples from the Wieprz-Krzna Canal in the Leczynsko-Wlodawskie Lake District of Southeastern Poland by Thin-Layer Chromatography with Diode Array Scanning and High-Performance Column Liquid Chromatography withDio

机译:薄层色谱-二极管阵列扫描-Dio-高效液相色谱法测定波兰东南部莱岑斯基-沃兹瓦斯基湖区维普茨-克尔兹纳运河水质中的农药

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High-performance thin-layer chromatography with diode array scanning (TLC-DAD) and high-performance column liquid chromatography with a diode array detector (HPLC-DAD) were used to screen water samples for pesticides. Atrazine, clofentezine, chlorfenvinphos, hexaflumuron, terbuthylazine, lenacyl, neburon, bitertanol, and metamitron were enriched from canal water samples by solid-phase extraction (SPE) on octadecyl silane (C18)/styrene-divinylbenzene-1, C18, C18 Polar Plus, and cyanopropyl (CN) cartridges. Recovery rates were high for all extraction materials except CN, for which values for all pesticides were lower. SPE was used for both preconcentration and fractionation of the analytes. Analytes were eluted by means of methanol and dichloromethane. Methanol eluates were analyzed by HPLC-DAD and dichloromethane eluates by TLC-DAD. The method was validated for precision, repeatability, and accuracy. Calibration graphs were linear between 0.1 and 50.0 mu g/mL for all pesticides, and correlation coefficient (r) values were between 0.9994 and 1.000 as determined by HPLC-DAD. Calibration graphs were linear between 0.1 and 1.5 mu g/spot for all pesticides, and r values were between 0.9899 and 0.9987 as determined by TLC-DAD. The limit of detection was between 0.04 and 0.23 mu g/spot for TLC-DAD and 0.02 and 0.45 mu g/mL for HPLC-DAD.
机译:使用带有二极管阵列扫描的高效薄层色谱(TLC-DAD)和带有二极管阵列检测器的高效柱液相色谱(HPLC-DAD)来筛查农药中的水样。通过在十八烷基硅烷(C18)/苯乙烯-二乙烯基苯-1,C18,C18 Polar Plus上进行固相萃取(SPE)从运河水样中富集去津,氯芬太嗪,氯芬芬膦,六氟磺隆,丁苯噻嗪,lenacyl,neburon,bitertanol和metamitron和氰丙基(CN)墨盒。除CN以外,所有提取材料的回收率均很高,而所有农药的回收率均较低。 SPE用于分析物的预浓缩和分馏。用甲醇和二氯甲烷洗脱分析物。通过HPLC-DAD分析甲醇洗脱液,通过TLC-DAD分析二氯甲烷洗脱液。验证了该方法的准确性,可重复性和准确性。对于所有农药,校准曲线在0.1和50.0μg / mL之间呈线性关系,通过HPLC-DAD测定,相关系数(r)值在0.9994和1.000之间。所有农药的校准曲线在0.1和1.5μg /点之间是线性的,通过TLC-DAD测定,r值在0.9899和0.9987之间。对于TLC-DAD,检测极限为0.04至0.23μg / mL,对于HPLC-DAD,检测极限为0.02至0.45μg / mL。

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