University of the basque country UPV/EHU
Science and technology faculty
Bº Sarriena, s/n 48940 Leioa (Vizcaya)
Dr. Juan Carlos Raposo (service technician)
Phone: 94 601 5443
Dra. Beatriz Abad (service technician)
Phone: 94 601 3197
Dr. Luis Bartolomé (service technician)
Phone: 94 601 3473
Dr. Isabel Collado
Phone: 94 601 5432
Dr. Patricia Navarro Villaverde
Phone: 94 601 3197
Access to the unit of Central Analysis Service Bizkaia involves meeting the requirements set forth in the Protocol for access to SGIker and the services it provides.
The use of analytical techniques by numerous research groups from the University of the Basque Country (UPV/EHU), and by different companies and technology centres from the milieu is becoming more and more common, with growing requirements in terms of precision, accuracy and sensitivity, etc. Numerous areas of industry, services and public institutions are warning about the need to carry out analytical determinations with totally different aims and objectives. Thus, these companies and institutions are making major financial investment with this in mind, either by purchasing the necessary instrumentation or by outsourcing the relevant chemical analyses.
Within the university milieu, the use of analytical techniques is demanded by numerous research groups from different areas of knowledge. The use of a General Service significantly facilitates the management and use of the analytical techniques available. This General Service emerged with the aim of providing back-up for research, being at the disposal of the University itself, public institutions and companies. The infrastructure it possesses enables a great variety of problems to be dealt with in the field of research and technological development. Attention should also be drawn to the fact that this Central Analysis Service improves the use of existing infrastructures, which contributes towards better returns on resources and, therefore, towards a reduction in expenditure in this area by the University of the Basque Country / EHU.
Range of services offered
The Analysis Service attempts to cover very diverse fields within applied chemical analysis, ranging from the analysis of water, soils, sediments and foods, etc. to the development of analytical methods applied to clinical or toxicological fields.
In this respect, different types of service are offered that could be grouped into three categories:
Fine-tuning of a familiar analytical methodology
For those cases in which the customer is aware of a suitable analytical method or is considering using an already-established standard or method.
Development of different analytical methodologies for unknown compounds
In these cases, since the substance to be determined is unknown, the service will ask the customer for all the information required to start checking different analytical techniques in order to deal with the problem being taken into consideration, in the sense of characterizing the unknown compound or compounds with the help of the most suitable techniques - including, where necessary, a confirmation technique, possibly with the help of combined techniques that may include mass spectrometry.
Research work and/or studies
In these cases, the Service will take part in the research considered by one or more groups by clearly defining the objectives to be attained in such research and the work plan to be developed.
By way of example, some of the fields and analyses offered by the Service are summarised below:
Analysis of drugs in pharmaceutical formulations
Analytical methods will be fine-tuned or developed for determining drugs in their formulations which do not require very high sensitivity. However, these may require great selectivity, as the active component may contain impurities that could give rise to major side effects. The pharmaceutical company increasingly needs not only the active component to be analysed, but also these impurities.
Analysis of drugs in biological fluids (plasma, urine, faeces, etc.)
Highly sensitive analytical methods will be put into practice to monitor levels of concentration in the biological fluid of pharmaceutical compounds. This type of determination requires the fine-tuning of a method for treating the biological method which will include liquid-liquid or solid-liquid extraction methods. This type of analysis is, generally speaking, carried out using chromatographic and electrophoretic methods.
Determining levels of plasma concentration in compounds of pharmaceutical interest tends to involve trying to establish the relevant pharmacokinetic profiles. Liquid chromatography with different types of detection is the most commonly-used technique.
The current trend in the field of Metabolomics is to have a bearing on the monitoring not only of the active component, but also on determining its metabolites. In this respect, the recent purchase of liquid chromatography-mass spectrometry equipment will enable this type of analysis to be carried out that has been requested both by pharmaceutical industries and research groups in bioanalytics.
In the food area, the control not only of raw materials is of vital importance, but also of end products. The type of analysis offered covers the following:
Determining metal ions in foods
Analysis of toxic substances in foods
Spectroscopic and chromatographic techniques will be applied when carrying put these analyses, following prior treatment of the sample.
Different analyses are offered within this area, among which are included the following:
Tracing analysis in underground water
Given the type of tracer used in hydrogeology (fluorescein, rhodamine, iodide, lithium, etc.,), techniques are used such as fluorometry, capillary electrophoresis and atomic absorption spectrometry.
Analysis of rocks, minerals and metal ores.
The metal ions in this type of matrix are determined, mainly via emission spectroscopy with inductively-coupled plasma (ICP-AES), given that a multi-elemental analysis is generally required and in very varied levels of concentration.
Area of the Environment
Analysis of urban and industrial atmospheres
Persistence of insecticides
Analysis of organic compounds in contaminated soils
Analysis of organic compounds in sentry organisms
Analysis of ink in documents
Isotopic analysis in different matrices (biological and environmental)
Determining pigments in works of art
In the field of artistic heritage conservation, in which the sample is of crucial importance, non-destructive techniques are required or those that require a very small size of sample. Capillary electrophoresis offers the advantages of being a technique that requires a volume of picoliters and possesses separation power which is greater than that of liquid chromatography. Thus, this technique will be applied to this type of analysis.
Determining liquid and protein agglutinants
In a painting, the pigments are accompanied by agglulitants that need to be analysed. Chromatographic methods (HPLC and gaseous chromatography) are the ones used in this type of determination.
Industry requires monitoring of its processes and also the characterization of its end products. The commercialisation of these products requires a series of standards with regard to specifications, which make it necessary to analyse such products. The Service attempts to provide the following two types of analysis:
Characterization of new materials
Monitoring of industrial processes which will require the use of different analytical methodologies, according to the type of industry.
This technique provides the content of carbon, hydrogen, nitrogen and sulphur which are present in a sample. The analytical method is based on the complete and instantaneous oxidation of the sample via combustion with oxygen at an approximate temperature of 1020° C. The combustion products are transported by the gas carrier to a chromatographic column where separation is carried out. A thermal conductivity detector provides the signal for each element which is then translated to a percentage content.
This equipment consists of a computer-controlled atomic absorption system which enables automated multi-elemental analysis to be carried out in a sequential way. Its control software (Winlab) makes it very versatile under numerous working conditions. This equipment enables other types of accessory to be incorporated such as automatic injection systems, diluters and injections systems, etc.
This atomic emission spectrometer (ICP-AES) is equipped with a glass and Teflon nebulizer system, which enables samples from acidic digestion to be determined using HF. This equipment also provides the option of coupling a hydride generation system which enables elements such as As, Hg and Sb,.etc. to be determined, in very low levels of concentration (ppb).
The equipment is controlled by a control computer with Activa Analyst 5.4 software, which enables it to interact with the equipment at all times.
This equipment is used for identification and structural eludation. It consists of electronic impact and chemical ionization probes, enabling work to be carried out in both positive and negative mode, and a flight-of-time analyzer capable of analysing molecular weight samples.
The equipment consists of a chromatograph coupled to a mass spectrometer with ion lens with ionization by electronic impact. The quadrupole makes it possible to analyse samples with molecular weight.
This equipment in turn possesses an automatic sampler (HP 6890 series) which permits the injection of up to 100 samples.
This equipment consists of a high-resolution chromatograph for the management and control of elluents and samples, together with a photodiode detector and a mass analyzer in tandem, triple-type quadrupole and ESI and APcI interfaces with "Z-spray" design. This enables work to be carried simultaneously both in positive and negative ion mode, as well as in several scanning modes (Full San, SIR, MRM, precursor ions, product ions, neutral losses, etc.) within a mass interval from 2 to 2000 u.
This capillary electrophoresis system is equipped with a photometric detector with fixed wave length, variable via filters, which enables it to detect from 185 and 254 nm. It possesses a carrousel with 20 positions for samples and electrolyte, hydrostatic injection mode, injection time and programmable analysis, separation voltage between 0-30kV, positive and negative power supplies and isomigration technique. It is coupled to a PC personal computer and controlled by Chemstation software (Agilent).
Desiccation technique for solutions, suspensions and animal or plant tissues that have been previously solidified by freezing, capable of removing around 6 litres of water in 24 hours. It enables lyophilization ramps to be programmed in addition to the monitoring of what occurs during lyophilization by computer. It also consists of lyophilization nozzles and three trays for lyophilization inside the chamber.
This equipment consists of an ultra-fast liquid chromatography (UPLC) coupled to a photodiode array detector (DAD) and a tandem mass spectrometer (QTOF) mass and high resolution accurate ionization with ESI sources, ESCI, APCI and MALDI. It is designed to provide high resolution of 40000 FWHM, mass accuracy around 1 ppm, high sensitivity and scan speed and versatility in the ways of scanning through the cell Triwave: MS, MSE, MS2, MS3.
It also has the following software:
Stable isotopes are commonly used for light elements (hydrogen, carbon, nitrogen and oxygen), which are precisely the most abundant in the environment. These elements are characterized by the largest natural variations in isotope ratios (abundance ratio between heavy and light isotope) due to be suffering greater isotopic fractionation in a wide range of physical and chemical processes.
In many cases the accurate determination of these relationships opens the possibility of differentiating materials or compounds that are chemically indistinguishable.