Validation and robustness testing of a HPLC method for the determination of avermectins and moxidectin in animal liver samples using an alumina column clean-up

peer-reviewedA multi-residue method has been developed for the quantitative determination of moxidectin, abamectin, doramectin and ivermectin in liver samples, with capability for qualitative identification of the presence of eprinomectin. Liver samples are extracted with isooctane, followed by clean-up on alumina-N solid phase extraction (SPE) cartridges. Extracts are derivatised and determined by high-performance liquid chromatography (HPLC) with fluorescence detection. The method was validated using bovine liver fortified at levels of 4 and 20 μg kg−1 with the drugs. The mean recovery from bovine liver ranged between 90 and 96%. The intra and inter-assay variations showed RSD typically of <5% and <10%, respectively. The procedure was applied also to ovine and porcine liver, giving similar results. A robustness study, carried out on the alumina clean-up step, indicated that the step is relatively insensitive to method changes. However, significant differences overall were found for the type of alumina and/or commercial SPE cartridge used. The limit of quantitation of the method is 2 μg kg−1 (ppb)

Applications of micro-fluidic platforms integrating packed stationary phases

To design and fabricate novel centrifugal micro-fluidic platforms integrating packed stationary phases for solid-phase micro-extraction in a wide range of (bio)analytical applications. To design and fabricate novel micro-fluidic platforms integrating packed stationary phases capable of withstanding significant high pressures

Centrifugally-driven sample extraction, preconcentration and purification in microfluidic compact discs

Centrifugally driven micro-fluidic discs (µ-CDs) have attracted significant interest within the analytical science community over the last decade, primarily being focused on the potential of such platforms for performing parallel and/or multiplex biological assays and further application in biomedical diagnostics. More recently, µ-CD based devices have also been applied to environmental analysis as platforms for multi-sample extraction and transportation, prior to off-disc analysis in the laboratory. Therefore, this review critically summarises recent developments with µ-CD platforms for sample extraction, preconcentration, fractionation and purification in bioanalytical and environmental applications. In addition to also summarising the 10 common methods employed in the fabrication of µCD platforms, as applications of µ-CDs in sample extraction are generally based on enclosed series of extraction phases/micro-columns, the preparation of these stationary phases in micro-fluidic channels embedded in µ-CDs is also discussed

Development and optimisation of an improved derivatisation procedure for the determination of avermectins and milbemycins in bovine liver

peer-reviewedA robust procedure has been developed to overcome the instability problems experienced with the fluorescent derivative of eprinomectin. The procedure involves addition of acetic acid, together with the typical reagents methylimidazole and trifluoroacetic anhydride, to produce a fluorescent molecule that can be determined by high performance liquid chromatography (HPLC) with fluorescence detection. Derivatisation is completed in 30 min at 65 °C. This derivatisation procedure was shown to be suitable, also, for the related compounds, moxidectin, abamectin, doramectin and ivermectin. A multi-residue method for these compounds in bovine liver has been developed using the derivatisation procedure. Samples are extracted with acetonitrile; followed by clean-up on deactivated alumina and C18 solid phase extraction (SPE) cartridges. The method was validated using bovine liver fortified at levels of 4 and 20 mg kg21 with the drugs. The mean recovery ranged between 73 and 97%. The intraand inter-assay variations showed relative standard deviations typically of < 6% and < 14%, respectively. The limit of quantitation of the method is 2 mg kg21 (ppb)

Fabrication and characterization of nanotemplated carbon monolithic material

A novel hierarchical nanotemplated carbon monolithic rod (NTCM) was prepared using a novel facile nanotemplating approach. The NTCM was obtained using C60-fullerene modified silica gels as hard templates, which were embedded in a phenolic resin containing a metal catalyst for localized graphitization, followed by bulk carbonization, and template and catalyst removal. TEM, SEM, and BET measurements revealed that NTCM possessed an integrated open hierarchical porous structure, with a trimodal pore distribution. This porous material also possessed a high mesopore volume and narrow mesopore size distribution. During the course of carbonization, the C60 conjugated to aminated silica was partly decomposed, leading to the formation of micropores. The Raman signature of NTCM was very similar to that of multiwalled carbon nanotubes as exemplified by three major peaks as commonly observed for other carbon materials, i.e., the sp3 and sp2 carbon phases coexisted in the sample. Surface area measurements were obtained using both nitrogen adsorption/desorption isotherms (BET) and with a methylene blue binding assay, with BET results showing the NTCM material possessed an average specific surface area of 435 m2 g−1, compared to an area of 372 m2 g−1 obtained using the methylene blue assay. Electrochemical studies using NTCM modified glassy carbon or boron doped diamond (BDD) electrodes displayed quasi-reversible oxidation/reduction with ferricyanide. In addition, the BDD electrode modified with NTCM was able to detect hydrogen peroxide with a detection limit of below 300 nM, whereas the pristine BDD electrode was not responsive to this target compound

A review of oxyhalide disinfection by-products determination in water by ion chromatography and ion chromatography-mass spectrometry

This paper is a review of ion chromatographic (IC) separations of inorganic oxyhalide disinfection by-products (DBPs) in water and beverages. The review outlines the chemical mechanisms of formation, regulation of maximum allowable levels, chromatographic column selection and speciation. In addition, this review highlights the application of IC coupled to mass spectrometry (MS) for trace and elemental composition analysis of oxyhalides, along with the analytical considerations associated to enable sensitive analysis. Furthermore, a review of literature concerning IC determination of inorganic oxyhalide DBPs in environmental matrices, including water, published since 2005 is presented, with a focus on MS detection, and a discussion on the relative performance of the methods. Finally some prospective areas for future research, including fast, selective, multi-analyte analysis, for this application are highlighted and discussed