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A simple, highly sensitive stability indicating reverse phase high-performance liquid chromatographic (RP-HPLC) method was developed and validated for the determination of sumatriptan succinate in bulk and tablet dosage form. The analysis was performed on reverse phase C18 ODS Inertsil (250×4.6mm, 5μm) column, with a mobile phase containing buffer: aetonitrile: methanol (80:10:10 v/v/v), pH was adjusted to 2.5 with orthophosphoric acid (OPA) at 221nm, by an isocratic elution mode with 1ml/min flow rate using photo diode array (PDA) detector at ambient temperature. The injection volume and retention time was found 20 μl and 4.4 minutes respectively. The method produced linear responses in the concentration range of 5-150 μg/ml, with a correlation coefficient of 0.999. The limit of detection (LOD) and limit of quantification (LOQ) values for HPLC method were found to be 1.967 and 5.961 μg/ml respectively. The recovery of the method was 98% of the labelled value. This method was validated for accuracy, precision, linearity and robustness. Sumatriptan subjected to different ICH prescribed stress conditions of acid, alkali, peroxide, reduction, thermal, photolytic and humidity degradation. This method can easily and conveniently take up for routine quantitative analysis of sumatriptan in bulk and pharmaceutical dosage form by easily available materials with low cost.
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Background: HbA1c can be measured by different methods. Enzymatic, boronate affinity chromatographic and cation-exchange high performance liquid chromatographic (HPLC) methods are considered as gold standard methods. To make the test cost-effective many laboratories use the immunological method installed in a chemistry analyzer. Objective: To compare the values of HbA1c measured by high performance liquid chromatographic method and immunological method in two laboratory settings. Materials and Methods: This observational and comparative study was conducted in Bangladesh Institute of Health Sciences (BIHS) and Enam Medical College, Savar, Dhaka. HbA1c levels measured by HPLC in BIHS were compared with that measured by immunological method in Enam Medical College, Savar, Dhaka. p values <0.05 were considered significant. Results: Statistically no difference was observed in mean HbA1c% between two methods in <7.0% HbA1c group and 7.1-10.0% HbA1c group. Significant statistical difference was found in mean HbA1c >10.0% group, but it was within acceptable limit. Conclusion: HbA1c can be measured by immunological method installed in an automated chemistry analyzer to make the test costeffective. But HPLC method is preferable.
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1ug/ml),chromatographing ona 300?3.9mm 1.D.colomn packcd with u Bondapak C_(18)(10um),and detecting at UV254nm.The mobile phase was MeOH-H_2O-TEMED-HAC(65:35:0.3:0.52)The average recovery of the whole procedure were 99.9?4.1(SD)%.CV=4.1%for clozapine)98.5?4.0(SD)%,CV=4.2% for chlopromazine.The Minimum detetionlimit was 10ng/ml serum.The developed method was applied to clinical monitoring of serum levels from11 patients who wereco administered with multiple oral doses of clozapine and chlor-promazine.The serum concentrations of 0.150-0.445?g/ml and 0.014-0.086?g/ml werefound.Futhermore,one case of suicide was encountered.
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An isocratic high-performance liquid-chromatographic method is-described for the simultaneously determining carbamazepine and its biologically active metabolite, carbamazepine-10, 11-epoxide. Serum samples containing an internal standard (10-methoxycarba-mazepine) are extracted with dichlor-methane and 4 mol ? L-1 sodium hydroxide. The organic extract are evaporated at ambient temperature under a stream of nitrogen. The residues are reconstituted in mobile phase and injected on to a re-versed-phase C18 Column (150?4. 6mm I. D). The mobile phase consists of ace-tontrile/methanol/water (50/210/260 by vol) . The UV detector is operated at 214nm. The elution times of all com-pounds are within 7 min.The least detectable concentrations of carbamazepine and carbamazepine-10, 11-epoxide are 0. 08mg ? L-1 and 0.1mg ? L-1, respectively. The average absolute recovery for carbamazepine is 96.0% and for carbamazepine-10,11-epoxide is 97.3%. Within-run CV is 3. 3%~5.7%. and between-run CV is 4.3%~9.0%. The standard curve is linear at least within 40mg ? L-1 for carbamazepine and within 20mg ? L-1 for carbamazepine-10, 11-epoxide.