Helalat-Nezhad Zahra, Ghanemi Kamal, Fallah-Mehrjardi Mehdi
Department of Marine Chemistry, Faculty of Marine Science, Khorramshahr University of Marine Science and Technology, P.O. BOX 669, Khorramshahr, Iran.
Department of Marine Chemistry, Faculty of Marine Science, Khorramshahr University of Marine Science and Technology, P.O. BOX 669, Khorramshahr, Iran.
J Chromatogr A. 2015 May 15;1394:46-53. doi: 10.1016/j.chroma.2015.03.053. Epub 2015 Mar 27.
A novel sample preparation method based on the complete dissolution of marine biological samples in choline chloride-oxalic acid (ChCl-Ox) deep eutectic solvent was developed for fast and efficient extraction of eight polycyclic aromatic hydrocarbons (PAHs) using minimum volumes of cyclohexane. The extracted PAHs were purified and then measured by high-performance liquid chromatography-fluorescence detection (HPLC-FL). The effect of key parameters on extraction recoveries and precision was investigated. At optimized conditions, the studied samples were dissolved under atmospheric pressure in ChCl-Ox (1:2) at 55°C for 30min, which is considerably lower than the temperature used in the classical and current methods. After dissolution, it took approximately 20min to quantitatively extract the PAHs from ChCl-Ox using 5mL cyclohexane. Depending on the analyte, the developed method was linear over the calibration range 1.0-250, 2.0-250, and 5.0-250ngg(-1), with r(2)>0.996. The detection limits of the method were between 0.50 and 3.08ngg(-1). The intra-day and inter-day precisions (based on the relative standard deviation, n=5) of the spiked PAHs at a concentration level of 50ngg(-1) were better than 12.6% and 13.3%, respectively. Individual PAH recoveries from spiked marine fish and macroalgae samples were in the range of 71.6% to 109.6%. For comparison, the spiked samples were also subjected to the Soxhlet extraction method. The simplicity of the procedure, high extraction efficiency, short analysis time, and use of safe and inexpensive components suggest the proposed method has a high potential for utilization in routine trace PAH analysis in biological samples.
开发了一种基于将海洋生物样品完全溶解于氯化胆碱 - 草酸(ChCl - Ox)低共熔溶剂的新型样品制备方法,以使用最小体积的环己烷快速高效地提取8种多环芳烃(PAH)。提取的PAH经过纯化,然后通过高效液相色谱 - 荧光检测(HPLC - FL)进行测定。研究了关键参数对提取回收率和精密度的影响。在优化条件下,所研究的样品在55°C下于常压下溶解于ChCl - Ox(1:2)中30分钟,这大大低于经典方法和现有方法所使用的温度。溶解后,使用5mL环己烷从ChCl - Ox中定量提取PAH大约需要20分钟。根据分析物的不同,所开发的方法在校准范围1.0 - 250、, 2.0 - 250和5.0 - 250ng g(-1)内呈线性,r(2)>0.996。该方法的检测限在0.50至3.08ng g(-1)之间。加标PAH在浓度水平为50ng g(-1)时的日内和日间精密度(基于相对标准偏差,n = 5)分别优于12.6%和13.3%。加标海洋鱼类和大型藻类样品中单个PAH的回收率在71.6%至109.6%范围内。为了进行比较,加标样品也采用索氏提取法进行处理。该方法操作简单、提取效率高、分析时间短,且使用安全廉价的成分,表明该方法在生物样品中常规痕量PAH分析中具有很高的应用潜力。