4^th World Congress on Chromatography August 07-09, 2017 Rome, Italy

Kahtan J Hasson is a Pharmacist since 1970 with Master degree from Herriot-Watt University, UK. He is a Lecturer at Al-Rasheed University and an R&DrnConsultant at Al-Safa Company for pharmaceutical industries, Baghdad.

Diclofenac sodium is widely used in medicine as anti-infl ammatory and antirheumatic agent. Th e therapeutic dose ofrnthis drug is 75 mg by parenteral administration, however, diclofenac sodium is slightly soluble in water, and therefore,rnit is prepared as 3 ml ampoule contains 25 mg/ml. Th e available commercial products of diclofenac sodium ampoules havernused diff erent types of solubilizing agents as benzyl alcohol which is an irritant in a concentration more than 3% while thernother manufacturers used propylene glycol which has toxic impurities. In this work, I tried to prepare diclofenac sodiumrninjection by using hydroxy propyl beta cyclodextrins, a natural and safe excipient in formulation of ampoule solution whichrnformed an inculcation complex compounds with diclofenac sodium, render it very soluble and more stable. Th e fi nishedrnproduct of ampoules were subjected to the stability study by storing the samples at 40°C and 75% RH for six months and thernphysico-chemical properties of the samples were tested at diff erent periods. Th e results showed no change in appearance ofrnthe ampoules solution along the study time. In addition, a reversed –phase high pressure liquid chromatographic method wasrndeveloped and applied in studying the behavior and resistance of diclofenac sodium in its solution to the high temperaturernchallenger. Th e developed HPLC method was proved to be accurate and able to detect the degradation products of diclofenacrnsodium in solution.

María Ramos Payan has expertise in “Improving sample preparation techniques focused on microfl uidic-chip devices as miniaturization”. The novelty of her\r\nmicrofl uidic devices offer more advantages than the existing methodologies. The devices work either using biological and environmental samples and can be\r\ncoupled on-line to HPLC or mass spectrometry. She has also demonstrated the applicability of microchip devices for diagnostic diseases as diabetes. She has\r\nworked at different institutions (University of Seville, University of Huelva, University of Lund, University of Copenhagen and University of North Carolina, USA).\r\nCurrently, she works at Microelectronic National Center of Barcelona and Universitat Autonoma of Barcelona with the aim of implementing optical detection into\r\nmicrofl uidic devices for multiple different applications.

Statement of the Problem: Th e most critical stage of the analytical process is the preparation of the sample requiring diff erent\r\nstages prior to analysis, long extraction times, large volumes of reagents, etc., with the objective of obtaining a good cleanup\r\nfor the analysis by instrumental techniques (as HPLC). Nowadays, one of the dominant trends in sample preparation is\r\nminiaturization and automation. In this paper, we present the advantages presented by the use of microfl uidic systems in this\r\nfi eld. Th ese devices allow working in diff erent confi gurations depending on the nature of the analyte to be extracted: either by\r\nliquid phase micro-extraction or by electro membranes.\r\nMethodology: Our group has demonstrated the possibility of on-line and off -line analysis by HPLC. Two pumps are used\r\nto introduce the sample and the acceptor phase into the microfl uidic device. Th e microfl uidic device is fabricated using\r\ntwo patterned plates of poly (methyl methacrylate), which are symmetrical. Th e channels are separated by a polypropylene\r\nmembrane. For off -line analysis, the acceptor outlet (extract) is collected and injected directly into a HPLC. For on-line\r\nanalysis, the acceptor outlet is connected to the HPLC.\r\nFindings: Th is type of device provides high selectivity, clean-up, reduces sample volume and low consumption of reagents,\r\nsignifi cantly reduces time of analysis and has demonstrated its ability to online coupling with HPLC. Additionally, the\r\nmicrochip-devices are reusable (allow membrane exchange) and each membrane is stable during more than 10 consecutive\r\nmicro extractions.\r\nConclusion & Signifi cance: Th e miniaturization and automatization of sample treatment procedures (on-chip) off er\r\nmultiple advantages compared with existing traditional techniques. It also, off ers excellent clean-up either with biological or\r\nenvironmental samples and signifi cantly reduces the time of analysis from the sample collection till data obtaining.

Maria Ramos Payan has expertise in improving sample preparation techniques focused on microfl uidic-chip devices as miniaturization. The novelty of her\r\nmicrofl uidic devices offer more advantages than the existing methodologies. The devices work either using biological and environmental samples and can be\r\ncoupled on-line to HPLC or Mass Spectrometry. She has also demonstrated the applicability of microchip devices for diagnostic diseases as diabetes. She has\r\nworked at different institutions (University of Seville, University of Huelva, University of Lund, University of Copenhagen and University of North Carolina, USA).\r\nCurrently, she works at Microelectronic National Center of Barcelona and Universitat Autonoma of Barcelona with the aim of implementing optical detection into\r\nmicrofl uidic devices for multiple applications.

This experimental work reports the study based on two working modes that can be used when liquid phase micro extraction\r\nis integrated into a microfl uidic-chip device. Th e study compares enrichment factors, extraction effi ciencies and detection\r\nand quantifi cation limits. Th e microfl uidic device has been tested with acid drugs as model analytes. Transport phenomena\r\nare faster on the micro-scale, and therefore extractions can be carried out quickly. Th is comes from the fact that the transport\r\nin LPME is governed by diff usion and that the time required for mixing scales with the square of the length, and then, the\r\ndiff usion path is much shorter in microfl uidic devices on chip. Th e study was carried out using a microfl uidic device consisting\r\non two patterned plates of poly (methyl methacrylate), which are symmetrical. In the front side, a channel was used as donor\r\n(sample) solution whereas in the back side, the channel was used as acceptor phase. Five non-steroidal anti-infl ammatories\r\nwere extracted from acid sample solution (pH 1.5), through the SLM, and into alkaline solution functioning as acceptor phase\r\n(pH 12). Two diff erent working modes were tested: double-fl ow mode and stopped-fl ow mode. For double-fl ow working\r\nmode, a donor fl ow rate within the range of 1-30 μL min-1 was tested, keeping the acceptor fl ow rate at 1 μL min-1 (table 1).\r\nHowever, the acceptor fl ow rate was stopped during the extraction (stagnant conditions). As seen in table 1, when the acceptor\r\nfl ow is turned off during the extraction time, high enrichment factor signifi cantly increases with the extraction time for all\r\ncompounds. As an example, the IBU is enriched by a factor of 75 aft er 25 minutes extraction consuming only 500 μL of sample.\r\nOn the other hand, a double-fl ow working mode is preferred when very high extraction effi ciencies are desired.

Maria Ramos Payan has expertise in improving sample preparation techniques focused on microfl uidic-chip devices as miniaturization. The novelty of her\r\nmicrofl uidic devices offer more advantages than the existing methodologies. The devices work either using biological and environmental samples and can be\r\ncoupled on-line to HPLC or Mass Spectrometry. She has also demonstrated the applicability of microchip devices for diagnostic diseases as diabetes. She has\r\nworked at different institutions (University of Seville, University of Huelva, University of Lund, University of Copenhagen and University of North Carolina, USA).\r\nCurrently, she works at Microelectronic National Center of Barcelona and Universitat Autonoma of Barcelona with the aim of implementing optical detection into\r\nmicrofl uidic devices for multiple applications.

This experimental work reports the fi rst microfl uidic-chip based system for liquid-phase microextraction (LPME-chip)\r\nfor the determination of fl uoroquinolones in water samples. In 2011, a HPLC DAD–FLD method combined with prior\r\ntraditional hollow fi ber-liquid phase microextraction was developed for the sensitive determination of eight widely used\r\nfl uoroquinolones. However, high sample volumes and longer extraction times were needed. In the recent years, miniaturization\r\nof analytical procedures has been a tendency with the aim of reducing costs, extraction times and improving extraction\r\neffi ciencies. We present a poly (methyl methacrylate) microfl uidic chip based on a double-fl ow working mode for the extraction\r\nof six fl uoroquinolones in water samples. 1-octanol was used as support liquid membrane. Extraction parameters were fi xed\r\nat pH 3 (donor phase), pH 12 (acceptor phase) and 1 μL/min for both acceptor and sample fl ow rate; resulting in extraction\r\neffi ciencies over 40%. Th is technique off er faster extractions in only 5 minutes and minimum sample volume (less than 10 μL).