19 research outputs found

    Monitoring crystallization processes in confined porous materials by dynamic nuclear polarization solid-state nuclear magnetic resonance

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    Establishing mechanistic understanding of crystallization processes at the molecular level is challenging, as it requires both the detection of transient solid phases and monitoring the evolution of both liquid and solid phases as a function of time. Here, we demonstrate the application of dynamic nuclear polarization (DNP) enhanced NMR spectroscopy to study crystallization under nanoscopic confinement, revealing a viable approach to interrogate different stages of crystallization processes. We focus on crystallization of glycine within the nanometric pores (7–8 nm) of a tailored mesoporous SBA-15 silica material with wall-embedded TEMPO radicals. The results show that the early stages of crystallization, characterized by the transition from the solution phase to the first crystalline phase, are straightforwardly observed using this experimental strategy. Importantly, the NMR sensitivity enhancement provided by DNP allows the detection of intermediate phases that would not be observable using standard solid-state NMR experiments. Our results also show that the metastable β polymorph of glycine, which has only transient existence under bulk crystallization conditions, remains trapped within the pores of the mesoporous SBA-15 silica material for more than 200 days

    Efficacité et tolérance des anti-inflammatoires non stéroïdiens et des glucocorticoïdes dans la lombosciatique aigüe par hernie discale : TéAGS : résultats d’un essai thérapeutique randomisé contrôlé

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    Objective. Sciatica is a critical burden for public health. Data regarding therapeutic strategies are scarce and controversial. We aimed to assess the efficacy and the tolerance of intravenous injections of ketoprofen and methylprednisolone on acute discogenic sciatica. Methods. Multicentric, double-blinded randomized controlled trial with an intent-to-treat analysis. Patients with acute sciatica (<8 weeks) of radiologically confirmed discogenic origin, without neurologic deficit were randomized in 3 arms. Besides oral analgesics, they received intravenous injections of Methylprednisolone (60mg/day) or ketoprofen (200mg/day) or placebo during 5 days. Clinical evaluation was performed on days 1, 3, 5. We evaluated radicular pain scale defined by clinical relevant or major response defined respectively by a decrease ≥20mm/100 and ≥30mm/100 on visual analogic. The primary outcome measure was clinical relevant response at day 5; secondary outcomes were the clinical relevant and major responses at day 3, major response at day 5, medians of radicular and lumbar pains, Lasegue’s sign and Schober’s index, analgesic consumption and realization of spinal injections and surgery at day 5. Results. 54 patients were randomized and 50 completed the study. There was no significant difference on the clinical relevant and major responses at day 5. In the Methylprednisolone group, there were more clinical relevant and major responses at day 3. No difference was observed on others secondary outcomes and adverse events. Conclusion. Even though there is no improvement of the clinical relevant response at day 5, our study suggests that more patients are relieved if the analgesics are associated with intravenous methylprednisolone in the 72 first hours.Objectif. Les données sur la prise en charge de la lombosciatique sont controversées. Le but était de comparer efficacité et tolérance des injections intra veineuses de kétoprofène et méthylprednisolone dans la lombosciatique aigue. Méthodes. Essai thérapeutique contrôlé, randomisé, multicentrique, en double aveugle, avec analyse en intention de traiter. Les patients présentaient une lombosciatique aigue sans déficit neurologique avec confirmation radiologique du conflit disco-radiculaire. Randomisation en 3 bras. En plus d’un protocole d’antalgiques, ils recevaient durant 5 jours des injections de méthylprednisolone ou de kétoprofène ou de placebo. Une amélioration d’au moins 20/100 de la douleur radiculaire était définie comme cliniquement pertinente, au delà de 30/100 la réponse était majeure. Critère de jugement principal : proportion de réponses cliniquement pertinentes à J5. Critères de jugement secondaires : proportion de réponses cliniquement pertinentes ou majeures à J3, de réponses majeures à J5, EVA radiculaire et lombaire médianes, consommation d’antalgiques et réalisation d’infiltration ou de chirurgie à J5. Résultats. 54 patients. Pas de différence sur la proportion de réponses cliniquement pertinentes ou majeures à J5. Dans le groupe méthylprednisolone, significativement plus de réponses cliniquement pertinentes et de réponses majeures à J3. Aucune différence sur les autres critères de jugement ou sur la tolérance. Conclusion. Pas de différences de réponses cliniquement pertinentes à J5 mais notre étude suggère que plus de patients sont soulagés si les antalgiques sont associés à des perfusions de méthylprednisolone dans les 72 premières heures
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