首页> 美国卫生研究院文献>Iranian Journal of Pharmaceutical Research : IJPR >Validation of an Analytical Method for Determination of 13 priority polycyclic aromatic hydrocarbons in mineral water using dispersive liquid-liquid microextraction and GC-MS
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Validation of an Analytical Method for Determination of 13 priority polycyclic aromatic hydrocarbons in mineral water using dispersive liquid-liquid microextraction and GC-MS

机译:分散液-液微萃取和GC-MS测定矿泉水中13种优先多环芳烃的分析方法的验证

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摘要

Dispersive liquid-liquid microextraction (DLLME) combined with gas chromatography–mass spectrometry (GC–MS) was used for the extraction and determination of 13 polycyclic aromatic hydrocarbons (PAHs) in mineral water samples. In this procedure, the suitable combination of extraction solvent (500 µL chloroform) and disperser solvent (1000 µL acetone) were quickly injected into the water sample (10.00 mL) by Hamilton syringe. After centrifugation, 500 µL of the lower organic phase was dried under a gentle stream of nitrogen, re-dissolved in chloroform and injected into GC-MS. Chloroform and acetone were found to be the best extraction and disperser solvent, respectively. Validation of the method was performed using spiked calibration curves. The enrichment factor ranged from 93 to 129 and the recovery ranged from 71 to 90%. The linear ranges for all the PAHs were 0.10-2.80 ngmL-1. The relative standard deviations (RSDs) of PAHs in water by using anthracene-d10 as internal standard, were in the range of 4-11% for most of the analytes (n = 3). Limit of detection (LOD) for different PAHs were between 0.03 and 0.1 ngmL-1. The method was successfully applied for the analysis of PAHs in mineral water samples collected from Tehran.
机译:分散液-液微萃取(DLLME)与气相色谱-质谱(GC-MS)结合用于萃取和测定矿泉水样品中的13种多环芳烃(PAH)。在此过程中,通过汉密尔顿注射器将萃取溶剂(500 µL氯仿)和分散剂(1000 µL丙酮)的合适组合快速注入水样(10.00 mL)中。离心后,将500 µL下层有机相在温和的氮气流下干燥,重新溶解于氯仿中,然后注入GC-MS中。发现氯仿和丙酮分别是最佳的萃取和分散溶剂。使用加标校准曲线对方法进行验证。富集因子范围从93到129,回收率范围从71到90%。所有多环芳烃的线性范围为0.10-2.80 ngmL -1 。对于大多数分析物(n = 3),使用蒽-d10作为内标,水中PAHs的相对标准偏差(RSD)在4-11%的范围内。不同PAHs的检出限(LOD)在0.03至0.1 ngmL -1 之间。该方法已成功应用于从德黑兰收集的矿泉水样品中的PAHs分析。

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