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Mass spectrometric analytical methods for the determination of endocrine disrupting chemicals (EDCs)

机译:质谱分析法测定内分泌干扰物(EDC)

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This paper describes a method for the determination of endocrine disrupting chemicals (EDCs) in waste water. The method involves a SPE-C-18 extraction followed by a SPE-silica gel column clean up and elution of the analytes with a mixture of acetone/pentane (2+1). Thereafter derivatisation of the analytes with heptafluorobutyric acid anhydride (HFBA) and analysis by gas chromatography/mass spectrometry (GC/MS) with positive electron impact ionisation (El) or negative chemical ionisation (NCl) using methane as reactant gas was performed. The two different ionisation techniques were compared and the negative chemical ionisation technique proved significant lower limits of detection (LODs) and quantitation (LOQs) than positive electron impact ionisation. Recoveries of the analytes in various spiked waste water samples ranged from 75.4 to 96.9%. The concentrations of the EDCs in feed waste water from three different waste water treatment plants (WWTPs) ranged from non-detectable up to a concentration of 10,305 ng/L for 4-NP and in the corresponding effluent samples from non-detectable to 723 ng/L for BPA.
机译:本文介绍了一种测定废水中内分泌干扰物(EDC)的方法。该方法包括SPE-C-18萃取,然后是SPE-硅胶柱净化,并用丙酮/戊烷(2 + 1)混合物洗脱分析物。此后,用七氟丁酸酐(HFBA)衍生分析物,并通过气相色谱/质谱(GC / MS)使用正电子碰撞电离(El)或负化学电离(NCl)进行分析,并使用甲烷作为反应气体。比较了两种不同的电离技术,并且负化学电离技术的检测限(LOD)和定量限(LOQs)比正电子碰撞电离明显更低。各种加标废水样品中分析物的回收率为75.4%至96.9%。来自三个不同废水处理厂(WWTP)的进料废水中EDC的浓度范围从无法检测到4-NP的浓度为10,305 ng / L,在相应的废水样品中浓度也从无法检测到723 ng / L表示BPA。

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