Sadeghi Ramezan, Kobarfard Farzad, Yazdanpanah Hassan, Eslamizad Samira, Bayat Mitra
Department of Toxicology and Pharmacology, School of Pharmacy, Shahid Beheshti University of Medical Sciences, Tehran, Iran. ; Department of Environmental Health Engineering, School of Health, Shahrekord University of Medical sciences, Shahrekord, Iran.
Department of Medicinal Chemistry, School of Pharmacy, Shahid Beheshti University of Medical Sciences, Tehran, Iran. ; Phytochemistry Research Center, Shahid Beheshti University of Medical Sciences, Tehran, Iran.
Iran J Pharm Res. 2016 Winter;15(1):157-68.
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.
采用分散液液微萃取(DLLME)结合气相色谱 - 质谱联用(GC - MS)法对矿泉水样品中的13种多环芳烃(PAHs)进行萃取和测定。在此过程中,用汉密尔顿注射器将萃取溶剂(500 μL氯仿)和分散剂溶剂(1000 μL丙酮)的合适组合快速注入水样(10.00 mL)中。离心后,取500 μL下层有机相在温和的氮气流下吹干,再用氯仿重新溶解并注入GC - MS。结果发现氯仿和丙酮分别是最佳的萃取溶剂和分散剂溶剂。该方法通过加标校准曲线进行验证。富集因子范围为93至129,回收率范围为71至90%。所有PAHs的线性范围为0.10 - 2.80 ngmL⁻¹。以蒽 - d10为内标,水中PAHs的相对标准偏差(RSDs)对于大多数分析物(n = 3)在4 - 11%范围内。不同PAHs的检测限(LOD)在0.03至0.1 ngmL⁻¹之间。该方法成功应用于从德黑兰采集的矿泉水样品中PAHs的分析。