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1.
Cureus ; 14(8): e27660, 2022 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-36072179

RESUMEN

Intertrochanteric fracture is a prevalent condition among older adults, and it is becoming more so as the population is aging. A 52-year-old man was reported to the hospital with symptoms of pain and swelling in the right hip since the morning. The patient reported a history of unexpected slips and falls in the morning. An X-ray was taken of both hips, and an intertrochanteric fracture was identified. After one month post-fracture, a dynamic hip screw (DHS) was used to perform open reduction internal fixation (ORIF). Early mobility, appropriate lower limb strength, pain reduction, and quality of life are all significant determinants. As evidenced by statistically significant improvements in exercise capacity and well-being, the intertrochanteric fracture rehabilitation program is beneficial. This case study represents a comprehensive rehabilitation program for people who have had post-fracture surgery.

2.
J Orthop Case Rep ; 11(8): 107-110, 2021 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-35004388

RESUMEN

INTRODUCTION: Scurvy is a rarely seen in pediatric patients nowadays, seen more in those with developmental delay, autism or those who are severely malnourished. Epiphyseal separations are known to occur in scurvy, but only a few such cases have been reported in children with cerebral palsy. The diagnosis is often misleading since other morbidities as trauma, malignancies, coagulopathies, septic arthritis, osteomyelitis, or rheumatologic disorders are often considered at first. We report the case of 4-year-old female child with cerebral palsy in whom the initial concern was septic arthritis/osteomyelitis based upon clinical presentation, ultrasonic and magnetic resonance imaging, led to a surgery revealing subperiosteal hematomas. CASE REPORT: A 4-year-old girl was admitted in the pediatrics department for fever and bilateral knee joint pain for 3 days. She was a diagnosed case of with cerebral palsy, psyco-developmental delay, and epileptogenic disorder put under valproic acid. She was toxic and febrile. Within 4 h after admission, both knees developed tense shiny intense swelling associated with pain, redness, and local rise of temperature with limited active range of motion. Near-complete passive range of motion was noted. There were no abnormal findings on the rest of the musculoskeletal examination. Aspiration of the knee revealed subperiosteal hematoma diagnostic of scurvy. CONCLUSION: Scurvy is exceedingly rare in children nowadays; however, its presentation among risky populations should not be forgotten. Musculoskeletal revelations, mostly subperiosteal hematoma, are the main manifestation of scurvy in the pediatric population. Scurvy as a differential diagnosis for trauma, osteomyelitis, septic arthritis will always be a bane for orthopedic surgeons. A heightened awareness is needed to avoid unnecessary surgery, unnecessary tests, and procedures and to be able to start treatment for a potentially fatal but easily curable disease.

3.
Talanta ; 72(1): 80-8, 2007 Apr 15.
Artículo en Inglés | MEDLINE | ID: mdl-19071585

RESUMEN

A high throughput liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for the determination of valproic acid, an antiepileptic drug, in human plasma is described. It is a rapid and sensitive isocratic reversed-phase liquid chromatography-tandem mass spectrometric method equipped with turbo ion spray (TIS) source, operating in the negative ion and pseudo selective reaction monitoring (SRM) acquisition mode to quantify valproic acid. The extraction of valproic acid and hydrochlorothiazide (IS) from the plasma involved sample treatment with phosphoric acid followed by solid-phase extraction using Waters hydrophilic-lipophilic balance (HLB) cartridge giving extracts free from endogenous interferences. Sample preparation by this method yielded very good and consistent mean recoveries of 99.73 and 74.47% for valproic acid and IS, respectively. The method was linear over the dynamic range of 2.0-200.0mug/ml (covering entire therapeutic range) with a correlation coefficient r>/=0.9989. The coefficient of variance (CV, %) was 7.03% at 2.0mug/ml (LLOQ). This method was fully validated for its accuracy, precision, recovery and matrix effect especially because the pattern of elution of all the analytes may appear as flow injection type. The analyte stability was examined under conditions mimicking the sample storage, handling and analysis procedures. The method was successfully applied for bioequivalence studies in human subject samples after oral administration of 500mg formulations.

4.
Biomed Chromatogr ; 21(1): 67-78, 2007 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-17080507

RESUMEN

A rapid, specific and sensitive LC-MS/MS assay using solid-phase extraction (SPE) for the determination of pravastatin, in human plasma is described. The plasma filtrate obtained after SPE, using a polymer base, a hydrophilic-lipophilic balance (HLB) cartridge, was submitted directly to short-column liquid chromatography-tandem mass spectrometric (LC-MS/MS) assay, with negligible matrix effect on the analysis. For validation of the method, the recovery of the free analytes was compared with that from an optimized extraction method, and the analyte stability was examined under conditions mimicking the sample storage, handling, and analysis procedures. The extraction procedure yielded extremely clean extracts with a recovery of 107.44 and 98.93% for pravastatin and IS, respectively. The intra-assay and inter-assay precisions for the samples at the LLOQ were 3.30 and 7.31% respectively. The calibration curves were linear for the dynamic range 0.5-200 ng/mL with correlation coefficient r > or = 0.9988. The intra- and inter-assay accuracy ranged from 95.87 to 112.40%. The method is simple and reliable with a total run time of 3 min. This novel validated method was applied to the pharmacokinetic (PK) study in human volunteers receiving a single oral dose of 40 mg immediate release (IR) formulation.


Asunto(s)
Pravastatina/sangre , Administración Oral , Anticolesterolemiantes/administración & dosificación , Anticolesterolemiantes/sangre , Calibración , Cromatografía Liquida , Humanos , Hidroclorotiazida/sangre , Espectrometría de Masas , Estructura Molecular , Pravastatina/administración & dosificación , Unión Proteica , Proteínas/química , Estándares de Referencia , Reproducibilidad de los Resultados , Sensibilidad y Especificidad , Extracción en Fase Sólida , Factores de Tiempo
5.
Rapid Commun Mass Spectrom ; 20(23): 3509-21, 2006.
Artículo en Inglés | MEDLINE | ID: mdl-17072906

RESUMEN

A high-throughput and sensitive bioanalytical method using liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) has been developed for the estimation of sibutramine and its two metabolites (M1 and M2). The extraction of sibutramine, its metabolites and imipramine (internal standard (IS)) from the plasma involved treatment with phosphoric acid followed by solid-phase extraction (SPE) using a hydrophilic-lipophilic balanced HLB cartridge. The SPE eluate without drying and reconstitution was analyzed by LC/MS/MS, equipped with a with turbo ion spray (TIS) source, operating in the positive and multiple reaction monitoring (MRM) acquisition mode. Sample preparation by this method yielded extremely clean extracts with quantitative and consistent mean recoveries; 95.12% for sibutramine, 92.74% for M1, 95.97% for M2 and 96.60% for the IS. The total chromatographic run time was 3.0 min with retention times of 2.51, 2.13, 2.09 min for sibutramine, M1, M2 and imipramine, respectively. The developed method was validated in human plasma matrix, with a sensitivity of 0.1 ng/mL (coefficient of variance (CV), 2.07%) for sibutramine, 0.1 ng/mL (CV, 3.59%) for M1 and 0.2 ng/mL (CV, 4.93%) for M2. Validation of the method for its accuracy, precision, recovery, matrix effect and stability was carried out especially with regard to real subject sample analysis. The response was linear over the dynamic range 0.1 to 8.0 ng/mL for sibutramine and M1, and 0.2 to 16.0 ng/mL for M2 with correlation coefficients of r > or = 0.9959 (sibutramine), 0.9935 (M1) and 0.9943 (M2). The method was successfully applied for bioequivalence studies in 40 human subjects with 15 mg capsule formulations.


Asunto(s)
Aminas/sangre , Aminas/farmacocinética , Análisis Químico de la Sangre/métodos , Cromatografía Liquida/métodos , Ciclobutanos/sangre , Ciclobutanos/farmacocinética , Espectrometría de Masa por Ionización de Electrospray/métodos , Humanos , Equivalencia Terapéutica
6.
Rapid Commun Mass Spectrom ; 20(17): 2539-47, 2006.
Artículo en Inglés | MEDLINE | ID: mdl-16878346

RESUMEN

The first liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for the determination of levetiracetam, an antiepileptic drug, in human plasma is described. The plasma filtrate obtained after solid-phase extraction (SPE), using a polymer-based, hydrophilic-lipophilic balanced (HLB) cartridge, was submitted directly to a short column LC/MS/MS assay. There was no significant matrix effect on the analysis. For validation of the method, the recovery of the free analytes was compared to that from an optimized extraction method, and the analyte stability was examined under conditions mimicking sample storage, handling, and analytical procedures. The extraction procedure yielded extremely clean extracts with a recovery of 79.95% and 89.02% for levetiracetam and the internal standard (IS), respectively. The intra-assay and inter-assay precision for the samples at the lower limit of quantitation (LLOQ) were 6.33 and 6.82%, respectively. The calibration curves were linear for the dynamic range of 0.5 to 50 microg/mL with a correlation coefficient r >/= 0.9971. The intra-assay accuracy at LLOQ, LQC, MQC, and HQC levels ranged from 81.60 to 95.40, 93.00 to 103.47, 95.97 to 104.09, and 91.15 to 95.18%, respectively, while the inter-assay accuracy at LLOQ, LQC, MQC and HQC levels varied from 80.20 to 95.40, 88.53 to 107.53, 95.97 to 108.45, and 91.15 to 112.70%, respectively. The method is rugged and fast with a total instrumental run time of 2 min. The method was successfully applied for bioequivalence studies in human subject samples after oral administration of 1000 mg immediate release (IR) formulations.


Asunto(s)
Anticonvulsivantes/sangre , Anticonvulsivantes/farmacocinética , Cromatografía Líquida de Alta Presión/métodos , Piracetam/análogos & derivados , Espectrometría de Masa por Ionización de Electrospray/métodos , Espectrometría de Masas en Tándem/métodos , Relación Dosis-Respuesta a Droga , Humanos , Levetiracetam , Piracetam/sangre , Piracetam/farmacocinética , Reproducibilidad de los Resultados , Extracción en Fase Sólida/métodos , Equivalencia Terapéutica
7.
Rapid Commun Mass Spectrom ; 20(19): 2921-31, 2006.
Artículo en Inglés | MEDLINE | ID: mdl-16941726

RESUMEN

A rapid and sensitive liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) method for the determination of isosorbide-5-mononitrate (5-ISMN), used in the treatment of angina pectoris, in human plasma is described. The quantification of 5-ISMN was performed via stable acetate adduct formation with a high relative abundance. The plasma filtrate obtained after solid-phase extraction (SPE), using a polymer based, hydrophilic-lipophilic balanced (HLB) cartridge, was submitted directly to reversed-phase high-performance liquid chromatography separation followed by ESI and detection of the resulting ions using triple-quadrupole mass spectrometry in selected reaction monitoring (SRM) mode. There was no significant matrix effect on the analysis. For validation of the method, the recovery of the free analyte response was compared to that obtained from an optimized extraction method. The analyte stability was examined under conditions mimicking the sample storage, handling, and analytical procedures. The extraction procedure yielded extremely clean extracts with a recovery of 95.51% and 93.98% for iossorbide-5-mononitrate and topiramate (internal standard (IS)), respectively. The calibration curves were linear for the dynamic range of 10.0 to 1000.0 ng/mL with a correlation coefficient r > or = 0.9985. The intra-assay and inter-assay precision for the samples at the lower limit of quantification (LLOQ) were 9.02 and 13.30%, respectively. The intra-assay accuracies at LLOQ, LQC, MQC and HQC levels varied from 98.13 to 118.15, 102.34 to 105.21, 100.69 to 109.68, and 95.76 to 102.92%, respectively, while the inter-assay accuracies ranged from 93.10 to 118.15, 93.03 to 107.04, 86.97 to 109.68 and 86.18 to 105.85%, respectively, at these levels. The method is rugged and fast with a total run time of 2 min. The method was successfully applied for a bioequivalence study in 24 human subject samples after oral administration of 60 mg extended release (ER) formulations.


Asunto(s)
Cromatografía Líquida de Alta Presión , Preparaciones de Acción Retardada , Dinitrato de Isosorbide/análogos & derivados , Donantes de Óxido Nítrico/sangre , Espectrometría de Masa por Ionización de Electrospray/métodos , Acetilación , Administración Oral , Humanos , Dinitrato de Isosorbide/sangre , Dinitrato de Isosorbide/química , Dinitrato de Isosorbide/farmacocinética , Donantes de Óxido Nítrico/química , Donantes de Óxido Nítrico/farmacocinética , Reproducibilidad de los Resultados , Extracción en Fase Sólida , Equivalencia Terapéutica
8.
J Chromatogr B Analyt Technol Biomed Life Sci ; 837(1-2): 92-100, 2006 Jun 06.
Artículo en Inglés | MEDLINE | ID: mdl-16709467

RESUMEN

A high throughput bioanalytical method based on solid phase extraction and liquid chromatography-tandem mass spectrometry (LC-MS/MS), has been developed for the estimation of perindopril and its metabolite perindoprilat, an angiotensin-converting enzyme inhibitor in human plasma. Ramipril was used as internal standard (IS). The extraction of perindopril, perindoprilat and ramipril from the plasma involved treatment with phosphoric acid followed by solid phase extraction (SPE) using hydrophilic lipophilic balance HLB cartridge. The SPE eluate without drying were analyzed by LC-MS/MS, equipped with turbo ion spray (TIS) source, operating in the negative ion and selective reaction monitoring (SRM) acquisition mode to quantify perindopril and perindoprilat in human plasma. The total chromatographic run time was 1.5 min with retention time for perindopril, perindoprilat and ramipril at 0.33, 0.35 and 0.30 min. The developed method was validated in human plasma matrix, with a sensitivity of 0.5 ng/ml (CV, 7.67%) for perindopril and 0.3 ng/ml (CV, 4.94%) for perindoprilat. This method was extensively validated for its accuracy, precision, recovery, stability studies and matrix effect especially because the pattern of elution of all the analytes appears as flow injection elution. Sample preparation by this method yielded extremely clean extracts with very good and consistent mean recoveries; 78.29% for perindopril, 76.32% for perindoprilat and 77.72% for IS. The response of the LC-MS/MS method for perindopril and perindoprilat was linear over the range 0.5-350.0 ng/ml for perindopril and 0.3-40 ng/ml for perindoprilat with correlation coefficient, r>/=0.9998 and 0.9996, respectively. The method was successfully applied for bioequivalence studies in human subjects samples with 4 mg immediate release (IR) formulations.


Asunto(s)
Inhibidores de la Enzima Convertidora de Angiotensina/sangre , Indoles/sangre , Perindopril/sangre , Espectrometría de Masa por Ionización de Electrospray/métodos , Inhibidores de la Enzima Convertidora de Angiotensina/farmacocinética , Humanos , Indoles/farmacocinética , Perindopril/farmacocinética , Reproducibilidad de los Resultados , Sensibilidad y Especificidad , Equivalencia Terapéutica
9.
J Chromatogr B Analyt Technol Biomed Life Sci ; 834(1-2): 149-54, 2006 Apr 13.
Artículo en Inglés | MEDLINE | ID: mdl-16531130

RESUMEN

A highly precise and sensitive method for the estimation of indapamide in human whole blood using high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) is described. The method developed is validated in human whole-blood matrix, with a sensitivity of 0.5 ng/ml as lower limit of quantification. The procedure for the extraction of indapamide and glimepiride as internal standard (IS) involves haemolysis and deprotienation of whole blood using ZnSO(4) followed by liquid-liquid extraction using ethyl acetate. The sample extracts after drying were reconstituted and analysed by LC-MS/MS, equipped with turbo ion spray (TIS) source, operating in the positive ion and selective reaction monitoring (SRM) acquisition mode to quantify indapamide in human whole blood. The mean recovery for indapamide was 82.40 and 93.23% for IS. The total run time was 2.5 min to monitor both indapamide and the IS. The response of the LC-MS/MS method for indapamide was linear over the range of 0.5-80.0 ng/ml with correlation coefficient, r>or=0.9991. The coefficient of variance (% CV) at 0.5 ng/ml was 4.02% and the accuracy was well within the accepted limit of +/-20% at 0.5 ng/ml and +/-15% at all other concentrations in the linear range. This method is fully validated for the accuracy, precision and stability studies and also applied to subject-sample analysis of bioequivalence study for 1.5mg sustained-release (SR) formulations.


Asunto(s)
Antihipertensivos/sangre , Cromatografía Líquida de Alta Presión/métodos , Diuréticos/sangre , Indapamida/sangre , Espectrometría de Masas/métodos , Antihipertensivos/farmacocinética , Disponibilidad Biológica , Humanos , Indapamida/farmacocinética , Reproducibilidad de los Resultados
10.
J Chromatogr B Analyt Technol Biomed Life Sci ; 829(1-2): 69-74, 2005 Dec 27.
Artículo en Inglés | MEDLINE | ID: mdl-16233994

RESUMEN

A method for the determination of sertraline, a new antidepressant drug and a selective serotonin reuptake inhibitor (SSRI), in human plasma is described. Therapeutic drug monitoring (TDM) necessitates efficient, fast and reliable analytical methods validated by external quality control. We therefore devised a simple, rapid and sensitive isocratic reversed-phase liquid chromatographic-tandem mass spectrometric method equipped with Turbo Ion spray (TIS) source, operating in the positive ion and selective reaction monitoring (SRM) acquisition mode to quantify sertraline in human plasma. A new and superior procedure of solid-phase extraction (SPE) (compared to liquid-liquid extraction) was followed to extract sertraline and imipramine as internal standard (IS) from the human plasma. Sample preparation was performed using waters hydrophilic-lipophilic balance (HLB) cartridge and this method yielded extremely clean extracts with very good recovery, 81.47 and 85.79% for sertraline and IS, respectively. Both were analyzed by combined reverse phase liquid chromatography and tandem mass spectrometry (LC-MS/MS) with positive ion TIS ionization using SRM acquisition mode. The response of the LC-MS/MS method for sertraline was linear over the dynamic range of 0.5-60.0 ng/ml with correlation coefficient r>or=0.9996. The coefficient of variance (%CV) was 8.53% at 0.5 ng/ml and the accuracy was well within the accepted limit of +/-20% at lower limit of quantification (LLOQ) and +/-15% at all the other concentrations in the linear range. This method was fully validated for the accuracy, precision and stability studies. The above findings indicate that the method is very much accurate and precise and can be successfully applied for bioequivalence studies in human subjects.


Asunto(s)
Cromatografía Liquida/métodos , Espectrometría de Masas/métodos , Inhibidores Selectivos de la Recaptación de Serotonina/sangre , Sertralina/sangre , Estabilidad de Medicamentos , Humanos , Estándares de Referencia , Reproducibilidad de los Resultados , Sensibilidad y Especificidad
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