1. Solid-phase extraction followed by liquid chromatography–time-of-ﬂight–mass spectrometry to evaluate pharmaceuticals in eﬄuents. A pilot monitoring study
Marıa Jose Gomez, Octavio Malato, Imma Ferrer, Ana Aguera and Amadeo R. Fernandez-Alba. J. Environ. Monit., 2007, 9, 718–729
The pharmaceuticals considered in this investigation were selected using the following criteria: (i) the consumption data provided by the hospital, (ii) previous information about occurrences in wastewater and surface water and (iii) persistence and poor removal eﬃciencies along the municipal WWTPs. A list including the most consumed drugs during the year 2004 was provided by the hospital pharmacy. The pharmaceuticals dipyrone, omeprazole, ketorolac, methyl-prednisolone, acetaminophen, mepivacaine, cefotaxime and ranitidine were among the top forty in the list. It was of special relevance that the highly consumed analgesic and antipyretic dipyrone (also known as metamizole), was more than two times higher than the second pharmaceutical in the list, omeprazole. Use of dipyrone as an analgesic is controversial and it has been banned in some countries (e.g. USA, UK, Sweden) because of a potential side eﬀect, agranulocytosis. However, in other countries (e.g. Germany, Italy and Spain), it represents one of the most frequently used nonopioids for postoperative pain, colic pain, cancer pain and migraine. In Spain, it is freely available over-the-counter and is one of the most popular non-opioid ﬁrst line analgesics. Use at hospitals is also very important, where the parenteral application of this drug is very common.
2. Toponomics: studying protein–protein interactions and protein networks in intact tissue
Sandra Pierre and Klaus Scholich*. Mol. BioSyst., 2010, 6, 641–647
Due to the fact that drug eﬀects are often not reﬂected by proteomic changes, the sensitive detection of alterations in the toponome presents now an alternative for the identiﬁcation of unknown mode of actions of drugs as well as oﬀ-target eﬀects. In a recent approach toponomics changes were detected after treatment of mice with the analgesic drug dipyrone. Here, eﬀects of the analgesic drug dipyrone on protein network proﬁles associated with arachidonic acid-dependent signaling pathways were studied. MELC analysis with 31 diﬀerent ﬂuorescence-labelled tags was used to compare the eﬀect of dipyrone on the toponome in spinal cords of mice with inﬂammatory pain. The number of motifs describing the co-localization of 5-lipoxygenase (5-LO) or 12-LO with other proteins increased strongly after dipyrone-treatment. Notably, activation of 5-LO and 12-LO induces their translocation to membrane compartments which was reﬂected in MELC results by an increased frequency of CMPs containing 5-LO or 12-LO and membrane compartment markers.
3. Fe3O4@TiO2 preparation and catalytic activity in heterogeneous photocatalytic and ozonation processes
L. Ciccotti, L. A. S. do Vale, T. L. R. Hewer and R. S. Freire*.Catal. Sci. Technol.,2015, 5,1143–1152
Dipyrone is an analgesic broadly used in Brazil and many other countries. Dipyrone is easily hydrolyzed into 4-methylaminoantipyrine (4-MAA). This and other dipyrone metabolites are not completely eliminated by biological treatment, and although little is known about their behavior and persistence in the environment, they have already been detected in surface water at high concentrations. In this paper, the preparation of Fe3O4 magnetic nanoparticles under different experimental conditions and the effect on the particle hydrodynamic diameter and size distribution were evaluated. The magnetic nanoparticles were used to prepare the hybrid catalyst Fe3O4@TiO2.Thismaterial was applied in the degradation of 4-MAA, the major dipyrone metabolite, by heterogeneous catalytic ozonation and photocatalysis treatment processes.
4. Determination of cocaine and its main adulterants in seized drugs from Rio Grande do Sul, Brazil, by a Doehlert optimized LC-DAD method
M. C. A. Marcelo,* T. R. Fiorentin, K. C. Mariotti, R. S. Ortiz, R. P. Limberger and M. F. Ferrao. Anal. Methods,2016, 8, 5212–5217
The linearity result for each adulterant indicates a good regression model. The calibration curve showed a good determination coefficient (r2) above 0.99 for all analytes. The LOD range is between 0.11 and 0.67 mgL-1 and suitable for the analysis. These results are summarized in Table 2. Table 3 depicts the accuracy and precision for cocaine analysis. The within-day and between-day precision as well as the accuracy were satisfactory for all analytes, with the worst RSD of 7.5% for between-days for dipyrone. All analytes’ recoveries were adequate, between 95.3% for cocaine and 116.2% for dipyrone. The conditions optimized by the Doehlert matrix were considered appropriate for the seized cocaine and its main adulterants’ analysis. A more detailed LC-DAD validation for cocaine was conducted by Floriani et al. However, our method optimized by Doehlert matrices suggests that using an isocratic mode with a basic pH also achieves good results for cocaine analysis. Moreover, our proposition conrms that levamisole is the most common salt cocaine adulterant in Brazil.