This study evaluates the application of Cr(VI) adsorption from the prepared synthetic solution by black sesame (Sesamum indicum L.) seed pulp (BSSP) and chitosan (Cts)-coated black sesame seed pulp beads (Cts-BSSP). BSSP and Cts-BSSP were used as an adsorbent without any chemical or physical treatment to remove Cr(VI) from an aqueous medium. The results indicated that the Cr(VI) removal was pH-dependent and reached an optimum at pH 2.0. It has been observed that the percentage of adsorption increased from 62% to 95% when the amount of Cts-BSSP increased from 0.0125 g to 0.0250 g. The required adsorbent amount for the maximum removal was 0.05 g and 0.1 g for Cst-BSSP and BSSP, respectively. The contact time for the adsorption was 120 min and 90 min for BSSP and Cst-BSSP, respectively. Scanning electron microscopy and Fourier transform infrared spectroscopy were used to explore the possible adsorption mechanism for Cr(VI). The equilibrium data for the BSSP and Cts-BSSP were used with the Langmuir and Freundlich adsorption isotherm models to assess the adsorption capacity and relevant mechanism. The adsorption capacity of the Cts-BSSP for Cr(VI) is relatively high compared to BSSP. The monolayer maximum adsorption capacities for Cr(VI) ions were 31.44 and 18.32 mg/g for Cts-BSSP and BSSP, respectively.
A new method based on fluorescence derivatization with 5-(dimethylamino) naphthalene-1-sulfonyl chloride (dansyl chloride) was developed for the quantitative determination of galantamine in human plasma and urine using high-performance liquid chromatography. The reaction between galantamine and dansyl chloride was optimally realized in 30 min at room temperature and pH 10.5, with a reagent to galantamine molar ratio of 2.13. The derivative was extracted with dichloromethane, and the extract was dried under a nitrogen stream and dissolved in the mobile phase. Chromatographic analysis was performed with an Inertsil C column and a mobile phase comprising 40% acetonitrile and 60% 10 mM o-phosphoric acid, 1.2 ml/min. The injection volume was 20 μl. The derivatives were detected with a fluorescence detector (excitation 375 nm/emission 537 nm). The retention time for the dansyl derivative of galantamine was 16.8 min. Linearity was observed between 125 and 2000 ng/ml in water, urine and plasma. The limit of detection and limit of quantification for the developed method were 6.27-70.99 and 18.81-212.97 ng/ml, respectively. Per cent recovery was calculated as 95.15 for urine and 95.78 for plasma. Interday repeatability values for urine and plasma samples (n = 6) at three different concentrations were calculated as a per cent relative standard deviation of 0.24-0.59 and 0.35-0.56. The corresponding per cent relative standard deviation values for intraday repeatability were 0.13-0.51 and 0.04-0.15, respectively.
Background and Aims: A new sensitive and selective method for the determination of sultamicillin in bulk and pharmaceutical preparations has been developed. Methods: The developed method is based on the derivatization of sultamicillin with 4-chloro-7-nitrobenzofurazan in pH 9.0 borate buffer at 70ºC for 60 min. The derivative was measured spectrophotometrically at 432 nm after extraction with chloroform. Results: The method was validated by linearity, LOD, LOQ, accuracy, precision and recovery parameters. The linear range for sultamicillin was 10-50 µg.mL-1 with a correlation coefficient of 0.9999. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 1.47 and 4.41 µg/mL-1 , respectively. Conclusion: The suggested method was validated, and can be applied for routine sultamicillin analysis in dosage formsfor industrial analysis.
Background and Aims: An HPLC method with photodiode array detector on a chiral column was proposed for enantioselective determination of chlorpheniramine (CLP) enantiomers in dosage forms. Methods: The enantioselective determination was achieved on amylose tris(3,5-dimethylphenylcarbamate) column, using n-hexane-(propan-2-ol)-diethylamine (97.5:2.5:0.025, v/v/v) mobile phase. The peaks were detected at 258 nm. Diphenhydramine was used as an internal standard (IS). A new sample preparation procedure was developed to avoid the interference of the other ingredients present in the formulations. Results: Limit of quantification of the proposed method was 0.88 and 1.31 µg/mL for S-(+)-CLP and R-(-)-CLP, respectively. Conclusion: The method is linear, sensitive, specific and can be used for the enantioselective assay of CLP enantiomers in pharmaceutical formulations.
In the present study, two new methods were developed and validated for the determination of rilmenidine in bulk and pharmaceutical preparation. Both methods are based on a derivatization reaction using 4-chloro-7-nitro-1,2,3-benzoxadiazole (NBD-Cl) as a fluorogenic substance. The drug reagent derivatives were formed by the reaction of rilmenidine with NBD-Cl at pH 9.0 at 70°C for 40 min. The reaction mixtures were analyzed by spectrofluorimetry in the first method and high performance liquid chromatography (HPLC) in the second method. Derivatives were determined at λex 493 nm and at λem 536 nm in the spectrofluorimetric method. The separation was performed place on a Phenomenex, C18 column (250 × 4.6 mm, 5 μm i.d) using a mobile phase comprising 0.2% formic acid and acetonitrile gradient elution mode in the HPLC method. Analytes were detected by a fluorescence detector at the same wavelength. The methods were validated for limit of quantitation, linearity, robustness, recovery, limit of detection, precision and accuracy. Calibration curves for the first and second methods were found to be linear in the range of 2.0–12.0 and 250–2000 ng/mL, respectively. Detection limits for the spectrofluorimetric and HPLC methods were calculated as 0.16 and 18.28 ng/mL, respectively. The validated methods were applied successfully to the determination of rilmenidine in bulk and pharmaceutical preparation.
Araştırmanın amacı, İstanbul ilinde bir kamu hastanesindeki Ocak-Aralık 2016 tarihleri arasındaki hasta şikâyet başvuru içeriklerinin incelenmesi ve elde edilen sonuçları tanımlayıcı istatistiksel yöntemler çerçevesinde analiz ederek değerlendirmektir. Sağlık kurumlarının temel odak noktası hastaların ihtiyaçlarını karşılamaktır. Hastaların ihtiyaçlarının karşılanarak memnuniyet düzeylerinin yüksek tutulması ise son derece zor bir durumdur. Bu çerçevede araştırmada hasta şikâyet başvurularının nedenleri ve bunların nasıl çözüleceği çalışmanın temel gerecidir. Çalışmada İstanbul ilindeki bir devlet hastanesinin hasta şikâyet başvuru içerikleri ele alınmış olup, veriler frekans, yüzde gibi tanımlayıcı istatistiksel yöntemler kullanılarak değerlendirilmiştir. Hasta hakları birimine birinci (% 60,12) ve ikinci (% 43,45) altı ayda en fazla başvuru poliklinik hizmetlerine yapılmıştır. Hastaların hangi konu ile ilgili olarak yaptıkları başvurular incelendiğinde, birinci (% 43,35) ve ikinci (%38,08) altı ayda en fazla şikayet hizmetten faydalanamama sorunu olmuştur. Kurula en fazla, şikâyet konusu olan meslek grubu ile ilgili veriler incelendiğinde, birinci (% 35,27) ve ikinci (% 43,46) altı ayda en fazla şikayete konu olan meslek grubu hekimlerdir. Sağlık sisteminin gelişmesi, etkili bir sağlık hizmet sunumu ve hasta memnuniyetinin sağlanması için hastalar tarafından olumlu ve olumsuz eleştirilerin dikkate alınarak, bu doğrultuda çalışmaların yapılması gerektiği düşünülmektedir.
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