Microextraction of Rosmarinic Acid Using CMK-3 Nanoporous Carbon in a Packed Syringe
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Microextraction of Rosmarinic Acid Using CMK-3 Nanoporous Carbon in a Packed Syringe Akram Rahimi • Payman Hashemi Alireza Badiei • Mehdi Safdarian • Marzieh Rashidipour
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Received: 11 October 2012 / Revised: 13 April 2013 / Accepted: 17 April 2013 / Published online: 26 April 2013 Ó Springer-Verlag Berlin Heidelberg 2013
Abstract CMK-3 nanoporous carbon was prepared and used as an efficient sorbent for microextraction in packed syringe of rosmarinic acid in Rosmarinus officinalis L. (rosemary). In the proposed method, only 2 mg of the nanoporous material, inserted between a syringe’s barrel and needle, was sufficient for the extraction with minimum consumption of organic solvents. Sample preparation was performed on the packed bed using a laboratory-made programmable apparatus. The apparatus was designed and used for automation of the conditioning, sampling, washing and elution steps of the method, and increasing the reproducibility of the experiments. For optimization of the experimental parameters, a central composite design method was used. Under the optimized conditions (i.e., number of adsorption cycles 14 times, number of elution cycles ten times and volume of elution 100 lL), an extraction recovery of 90 (±4.5) % was obtained for rosmarinic acid. The same packing bed could be used for at least 80 extractions without significant changes in its properties. The efficiency of the nanoporous sorbent was found to be superior to that of activated carbon, by a factor of about 17. The proposed method was successfully applied to the extraction of three rosemary samples before analysis by HPLC.
A. Rahimi P. Hashemi (&) M. Safdarian Department of Chemistry, Faculty of Science, Lorestan University, Khoramabad, Iran e-mail: [email protected] A. Badiei School of Chemistry, College of Science, University of Tehran, Tehran, Iran M. Rashidipour Razi Herbal Medicines Research Center, Lorestan University (Medical Sciences), Khoramabad, Iran
Keywords High performance liquid chromatography Microextraction in packed syringe CMK-3 nanoporous carbon Rosmarinic acid
Introduction Sample preparation is of critical importance for the analysis, especially for samples with a complex matrix. The purpose of this step is to remove interfering materials and enrichment of the analytes. Among commonly used sample preparation methods, liquid–liquid extraction is time-consuming and require the use of organic solvents, which are dangerous for health and the environment. Solid phase extraction (SPE) also requires relatively large quantities of sample and solvents or solvent mixtures [1–4]. Solid phase microextraction (SPME), due to its simple, solventless and flexible properties, has gained a widespread acceptance in many areas as an alternative to the conventional sampling techniques [5–7]. The major disadvantages of SPME in quantitative analysis are low recovery and high sensitivity to the nature of sample matrix. Microextraction in packed syringe (MEPS) was first described by Abdel-Rehim [8], as a new d
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