- Bar adsorptive microextraction technique - application for the determination of pharmaceuticals in real matrices. [Journal Article]
- ABAnal Bioanal Chem 2017 Jan 16
- In the present work, bar adsorptive microextraction using miniaturized devices (7.5 × 3.0 mm) coated with suitable sorbent phases, combined with microliquid desorption (100 μL) followed by high-perfo...
In the present work, bar adsorptive microextraction using miniaturized devices (7.5 × 3.0 mm) coated with suitable sorbent phases, combined with microliquid desorption (100 μL) followed by high-performance liquid chromatography with diode array detection (BAμE-μLD/HPLC-DAD), is proposed for the determination of trace level of six pharmaceuticals (furosemide, mebeverine, ketoprofen, naproxen, diclofenac and mefenamic acid) in environmental water and urine matrices. By comparing ten distinct sorbent materials (five polymeric and five activated carbons), the polymer P5 proved to be the most suitable to achieve the best selectivity and efficiency. The solvent volume minimization in the liquid desorption stage demonstrated remarkable effectiveness, being more environmentally friendly, and simultaneously increased the microextraction enrichment factor two-fold. Assays performed through BAμE(P5, 0.9 mg)-μLD(100 μL)/HPLC-DAD on 25 mL of ultrapure water samples spiked at the 4.0 μg/L level yielded average recoveries ranging from 91.4% (furosemide) to 101.0% (ketoprofen) with good precision (RSD < 10.6%), under optimized experimental conditions. The analytical performance showed convenient detection limits (25.0 - 120.0 ng/L), good linear dynamic ranges (0.1 to 24.0 μg/L), appropriate determination coefficients (r (2) > 0.9983), and excellent repeatability through intraday (RSD < 10.4%)) and interday (RSD < 10.0%) assays. By using the standard addition methodology, the application of the present analytical approach on environmental waters and urine samples revealed the occurrence of trace levels of some pharmaceuticals. The solvent minimization during the back-extraction step associated with the miniaturization of BAμE devices proved to be a very promising analytical technology for static microextraction analysis. Graphical abstract BAμE operating under the floating sampling technology for the determination of pharmaceuticals in aqueous media.
- Magnesium sulphate attenuates acute postoperative pain and increased pain intensity after surgical injury in staged bilateral total knee arthroplasty: a randomized, double-blinded, placebo-controlled trial. [Journal Article]
- BJBr J Anaesth 2016; 117(4):497-503
- CONCLUSIONS: Magnesium sulphate administration significantly reduced postoperative pain and minimized the difference in pain intensity between the first and second operations.
- Compacted Multiparticulate Systems for Colon-Specific Delivery of Ketoprofen. [Journal Article]
- APAAPS PharmSciTech 2017 Jan 10
- Pellet-containing tablets for colon-specific drug delivery present higher targeting efficiency and lower costs when compared with monolithic tablets and pellet-filled capsules, respectively. In this ...
Pellet-containing tablets for colon-specific drug delivery present higher targeting efficiency and lower costs when compared with monolithic tablets and pellet-filled capsules, respectively. In this study, pellets containing ketoprofen were coated with different acrylic polymers and submitted to compaction. The influence of formulation and process factors on film integrity was then evaluated. Pellets were prepared via extrusion-spheronization and coated using two acrylic polymers (Eudragit® FS 30 D and Opadry® 94 k28327, PMMA and PMA, respectively). The resulting pellets were mixed with placebo granules and compressed in a hydraulic press. Multiple regression showed that ketoprofen release from pellet-containing tablets is predominantly influenced by pellet content, hardness, friability, and disintegration time. PMA-containing tablets prepared under low compaction force or with low pellet content showed rapid disintegration (<1 min) and ketoprofen release similar to those of uncompressed coated pellets (∼30% at 360 min of experiment). On the other hand, PMMA-containing tablets showed a higher rupture level, and those prepared with higher pellet content gave rise to a non-disintegrating matrix. Coated pellets were shown to be able to target ketoprofen to the colonic region. Targeting capacity was dependent on the physicochemical characteristics of the tablets.
- Adsorption of non-steroidal anti-inflammatory drugs from aqueous solution using activated carbons: Review. [Review]
- JEJ Environ Manage 2017 Apr 01; 190:274-282
- Pharmaceutical pollutants are of significant effect on the environment, so that their treatments have been addressed in many studies. Activated carbon (AC) adsorbent shows best attraction for these c...
Pharmaceutical pollutants are of significant effect on the environment, so that their treatments have been addressed in many studies. Activated carbon (AC) adsorbent shows best attraction for these compounds due to its unique characteristics represented by high capacity and porosity. In this article, the adsorption performance of AC towards non-steroidal anti-inflammatory drugs (NSAIDs) such as ibuprofen, ketoprofen, naproxen, and diclofenac were reviewed. According to collected data, maximum adsorption capacities of 417, 25, 290, and 372 mg/g were obtained from Langmuir isotherm for these drugs, respectively. The values of 1/n for Freundlich isotherm were lower than unity for all studied drugs, confirming the nonlinear and favorable adsorption. In addition, kinetics data were well represented by the pseudo-second-order model and mechanism was not controlled by the pore diffusion step alone. AC adsorption demonstrated superior performance for all selected NSAIDs, thus being efficient technology for treatment of these pharmaceutical pollutants.
- Simultaneous enantiomeric analysis of pharmacologically active compounds in environmental samples by chiral LC-MS/MS with a macrocyclic antibiotic stationary phase. [Journal Article]
- JMJ Mass Spectrom 2017 Jan 06
- This paper presents a multi-residue method for direct enantioselective separation of chiral pharmacologically active compounds in environmental matrices. The method is based on chiral liquid chromato...
This paper presents a multi-residue method for direct enantioselective separation of chiral pharmacologically active compounds in environmental matrices. The method is based on chiral liquid chromatography and tandem mass spectrometry detection. Simultaneous chiral discrimination was achieved with a macrocyclic glycopeptide-based column with antibiotic teicoplanin as a chiral selector working under reverse phase mode. For the first time, enantioresolution was reported for metabolites of ibuprofen: carboxyibuprofen and 2-hydroxyibuprofen with this chiral stationary phase. Moreover, enantiomers of chloramphenicol, ibuprofen, ifosfamide, indoprofen, ketoprofen, naproxen and praziquantel were also resolved. The overall performance of the method was satisfactory in terms of linearity, precision, accuracy and limits of detection. The method was successfully applied for monitoring of pharmacologically active compounds at enantiomeric level in influent and effluent wastewater and in river water. In addition, the chiral recognition and analytical performance of the teicoplanin-based column was critically compared with that of the α1 -acid glycoprotein chiral stationary phase.
- Distribution of Animal Drugs among Curd, Whey, and Milk Protein Fractions in Spiked Skim Milk and Whey. [Journal Article]
- JAJ Agric Food Chem 2017 Jan 17
- It is important to understand the partitioning of drugs in processed milk and milk products, when drugs are present in raw milk, in order to estimate the potential consumer exposure. Radioisotopicall...
It is important to understand the partitioning of drugs in processed milk and milk products, when drugs are present in raw milk, in order to estimate the potential consumer exposure. Radioisotopically labeled erythromycin, ivermectin, ketoprofen, oxytetracycline, penicillin G, sulfadimethoxine, and thiabendazole were used to evaluate the distribution of animal drugs among rennet curd, whey, and protein fractions from skim cow milk. Our previous work reported the distribution of these same drugs between skim and fat fractions of milk. Drug distribution between curd and whey was significantly correlated (R(2) = 0.70) to the drug's lipophilicity (log P), with improved correlation using log D (R(2) = 0.95). Distribution of drugs was concentration independent over the range tested (20-2000 nM). With the exception of thiabendazole and ivermectin, more drug was associated with whey protein than casein on a nmol/g protein basis (oxytetracycline experiment not performed). These results provide insights into the distribution of animal drug residues, if present in cow milk, among milk fractions, with possible extrapolation to milk products.
- High-Quality Metal-Organic Framework ZIF-8 Membrane Supported on Electrodeposited ZnO/2-methylimidazole Nanocomposite: Efficient Adsorbent for the Enrichment of Acidic Drugs. [Journal Article]
- SRSci Rep 2017 Jan 04; 7:39778
- Metal-organic framework (MOF) membranes have received increasing attention as adsorbents, yet the defects in most membrane structures greatly thwart their capacity performance. In this work, we fabri...
Metal-organic framework (MOF) membranes have received increasing attention as adsorbents, yet the defects in most membrane structures greatly thwart their capacity performance. In this work, we fabricated a novel ZnO/2-methylimidazole nanocomposite with multiple morphology by electrochemical method. The nanocomposite provided sufficient and strong anchorages for the zeolitic imidazolate frameworks-8 (ZIF-8) membrane. Thus, a crack-free and uniform MOF membrane with high performance was successfully obtained. In this case, 2-methylimidazole was believed to react with ZnO to form uniform ZIF nuclei, which induced and guided the growth of ZIF-8 membrane. The as-prepared ZIF-8 membrane had large surface area and good thermal stability. As expected, it displayed high adsorption capacity for acidic drugs (e.g., ibuprofen, ketoprofen and acetylsalicylic acid) as they could interact through hydrophobic, hydrogen bonding and π-π stacking interaction. Accordingly, by coupling with gas chromatography the ZIF-8 membrane was successfully applied to the real-time dynamic monitoring of ibuprofen in patient's urine.
- Development of Diagnostic Techniques for Early Rheumatoid Arthritis Using Positron Emission Tomography with [(11)C]PK11195 and [(11)C]Ketoprofen Tracers. [Journal Article]
- MIMol Imaging Biol 2017 Jan 03
- CONCLUSIONS: With [(11)C]PK11195 and [(11)C]ketoprofen tracers, non-invasive in vivo PET imaging for rheumatoid synovitis can provide diagnostic evidence of early synovitis and allow monitoring inflammatory cell activity during treatment.
- Pain alleviation during castration of piglets: a comparative study of different farm options. [Journal Article]
- JAJ Anim Sci 2016; 94(12):5077-5088
- Pain alleviation associated with castration of piglets is an important welfare issue. The present study compares the effect of different approaches and products suitable for farmer use, with the aim ...
Pain alleviation associated with castration of piglets is an important welfare issue. The present study compares the effect of different approaches and products suitable for farmer use, with the aim to alleviate pain due to castration in piglets. A randomized within-litter design, with 28 replicate litters, compared 7 treatments: handling () restraint of the piglet and manipulation of the scrotum, castration without pain relief (), 2 treatments (, ) with different concentrations of tetracaine (2 and 6%) applied topically 10 min before and immediately post-surgery, and 3 treatments with i.m. injection of different nonsteroidal anti-inflammatory drugs () 10 min prior to surgery (-meloxicam, -ketoprofen, -tolfenamic acid). Efficacy of pain relief was assessed during a 300 min period after castration by serum cortisol, behavior (walking, lying, suckling, in the nest, isolated and pain related: tremors, rubbing the rear, hunching, wagging of the tail), facial expression and scrotal skin pressure sensitivity. C pigs had greater serum cortisol concentration than all other groups at 60 min post-surgery ( < 0.001), while H pigs had lower concentrations than pigs given topical anesthesia ( < 0.001) though not injected analgesia. No treatment differences were significant at 180 min, but at 300 min cortisol concentration was greater in T2 and T6 piglets than those given NSAIDs ( = 0.03). These treatment differences were mirrored by the pressure sensitivity of the scrotum; in comparison with C piglets, those given NSAIDs showed a reduced sensitivity ( 0.003) but those given local anesthesia did not ( = 0.15). C pigs showed increased frequency of pain-related behavior in the first 30 min in comparison with all other treatments, more time isolated than H or NSAID treatments, and more time standing inactive than H or K treatments. No behavioral differences were apparent after 60 min. No differences in facial expressions were observed among treatments. In conclusion, on-farm methods for pain relief can provide some, though not complete, pain alleviation in the hours after castration. The use of topical anesthesia gave only minor benefit in comparison to NSAID agents injected prior to castration. Since the main differences in indicators of pain between positive and negative controls were observed within the first h after castration, it is important to select drugs that act quickly after administration to facilitate practical processing schedules on farm.
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- Intracellular Enzymes Contribution to the Biocatalytic Removal of Pharmaceuticals by Trametes hirsuta. [Journal Article]
- ESEnviron Sci Technol 2017 Jan 17; 51(2):897-904
- The use of white rot fungi (WRF) for bioremediation of recalcitrant trace organic contaminants (TrOCs) is becoming greatly popular. Biosorption and lignin modifying enzymes (LMEs) are the most often ...
The use of white rot fungi (WRF) for bioremediation of recalcitrant trace organic contaminants (TrOCs) is becoming greatly popular. Biosorption and lignin modifying enzymes (LMEs) are the most often reported mechanisms of action. Intracellular enzymes, such as cytochrome P450 (CYP450), have also been suggested to contribute. However, direct evidence of TrOCs uptake and intracellular transformation is lacking. The aim of this study was to evaluate the relative contribution of biosorption, extracellular LMEs activity, TrOCs uptake, and intracellular CYP450 on the removal of six nonsteroidal anti-inflammatories (NSAIs) by Trametes hirsuta. Results show that for most tested NSAIs, LMEs activity and biosorption failed to explain the observed removal. Most tested TrOCs are quickly taken up and intracellularly transformed. Fine characterization of intracellular transformation using ketoprofen showed that CYP450 is not the sole intracellular enzyme responsible for intracellular transformation. The contribution of CYP450 in further transformation of ketoprofen byproducts is also reported. These results illustrate that TrOCs transformation by WRF is a more complex process than previously reported. Rapid uptake of TrOCs and intracellular transformation through diverse enzymatic systems appears to be important components of WRF efficiency toward TrOCs.