This study describes a comparison between LC-UV and LC-MS method for the simultaneous analyses of a few disease-modifying agents of multiple sclerosis. Quantitative determination of fampridine (FAM), teriflunomide (TFM) and dimethyl fumarate (DMF) was performed in human plasma with the recovery values in the range of 85-115%. A reversed-phase high-performance liquid chromatography (HPLC) with UV as well as MS detection is used. The method utilizes an XBridge C18 silica column and a gradient elution with mobile phase consisting of ammonium formate and acetonitrile at a flow rate of 0.5 mL min(-1) . The method adequately resolves FAM, TFM and DMF within a run time of 15 min. Owing to low molecular weights, the estimation of DMF and FAM is more versatile in UV than MS detection. With LC-UV, the detection limits of FAM, TFM and DMF were 0.1, 0.05, 0.05 μg and the quantification limit for all the analytes was 1 μg. With LC-MS, the detection and quantification limits for all of the analytes were 1 and 5 ng, respectively. The two techniques were completely validated and shown to be reproducible and sensitive. They were applied to a pharmacokinetic study in rats by a single oral dose. Copyright © 2016 John Wiley & Sons, Ltd.

Saksagliptin ve dapagliflozinin sabit doz kombinasyonu antidiyabetik ilaç tedavisi için onaylanmıştır ve Qtern markası ile pazarda yer almaktadır. Bu çalışmada amaç, insan plazmasındaki saksagliptin ve dapagliflozinin eş zamanlı tayini için Avrupa Gıda ve İlaç İdaresi kılavuzlarına uygun şekilde linagliptin iç standardı kullanarak ve basit, hızlı, hassas ve validasyonu yapılmış izokroatik ters faz-yüksek performanslı sıvı kromatografi (RP-HPLC) yöntemi geliştirmektir. Gereç ve Yöntemler: Method 4'lü akış pompasına sahip Waters 2695 marka HPLC cihazı ile gerçekleştirilmiştir. Analitin ayrılmasında Eclipse XDB C18 kolon (150 × 4.6 mm × 5 μm) kullanılmıştır. Kullanılan mobil fazın bileşimi ise pH 5.0 ayarlanmış %0.1 orto fosforik asit ve asetonitril (50:50) şeklinde olup akış hızı analiz süresince 1 mL/dk'dır. Bulgular: Analit 254 nm'de tayin edilmiştir. İç standart, saksagliptin ve dapagliflozinin alıkonma zamanları sırasıyla 2.746, 5.173 ve 7.218 dk olarak tespit edilmiştir. Pikler interferanslar gözlenmeden elde edilmiştir. Metot validasyonu saksagliptin ve dapagliflozin için sırasıyla 0.01 ile 0.5 μg/mL ve 0.05 ile 2 μg/mL doğrusal derişim aralığında 0.998 korelasyon katsayısı ile gerçekleştirilmiştir. Numunlere ait 6 ölçüme ait kesinlik ve doğruluk tayin sınırları içerisinde bulunmuştur. Analitlerin insan plazması içinde-28°C sıcaklıkta 37 gün boyunca kararlı halde kaldığı belirlenmiştir.

A rapid, sensitive, and accurate high performance liquid chromatography for the determination of axitinib (AN) in rabbit plasma is developed using crizotinibe as an internal standard (IS). Axitinib is a tyrosine kinase inhibitor, used in the treatment of advanced kidney cancer, which works by slowing or stopping the growth of cancer cells. The chromatographic separation was performed on a Waters 2695, Kromosil (150 mm × 4.6 mm, 5 µm) column using a mobile phase containing buffer (pH 4.6) and acetonitrile in the ratio of 65:35 v/v with a flow rate of1 mL/min. The analyte and internal standard were extracted using liquid-liquid extraction with acetonitrile. The elution was detected by photo diode array detector at 320 nm.The total chromatographic runtime is 10.0 min with a retention time for axitinib and IS of 5.685, and 3.606 min, respectively. The method was validated over a dynamic linear range of 0.002-0.2µg/mL for axitinib with a correlation coefficient of r 2 0.999.

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The present method describes the development of a validated RP-HPLC method for determination of Tigecycline. Separation was carried out on a Kromasil ODS C-18 column (150×4.6mm, 5µ) using Buffer: Acetonitrile 83: 17 as mobile phase at a flow rate of 1.2 ml/min. UV detection was performed at 247nm. The method was validated with respect to specificity, selectivity, linearity, accuracy, precision and robustness. The assay method was found to be linear in the range of 80 to 120 µg/ml with a correlation coefficient of 0.9999.The percentage recovery of active pharmaceutical ingredient from parenteral dosage form ranged from 99.5 to 100.2%. The results showed that the developed RP-HPLC method is suitable for determination of Tigecycline in bulk as well as stability samples of pharmaceutical dosage forms containing various excipients.

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To develop and validate a simple, selective, rapid and stability indicating reverse phase high performance liquid chromatographic (RP-HPLC) method for the analysis of Lurasidone HCl in bulk and its tablet dosage forms. Method: Several trials were made by changing the mobile phase composition and nally the drug was resolved on a Thermo ODS, C18, (150 X 4.6 mm, 5µ) column, using the mobile phase consisting of sodium dihydrogen ortho phosphate buffer (pH 6.5) and acetonitrile in 60 : 40 ratio and pumped at a ow rate of 0.8 ml/min at ambient temperature. Studies were performed on Waters HPLC system equipped with PDA detector, the response was monitored at 230 nm. The developed method was validated as per ICH guidelines. Results: The retention time of Lurasidone HCl was found to be 3.33±0.02 minutes. The calibration curve 2 was linear over the concentration range of 10-60 μg/ml (r =0.9999). The limit of detection for Lurasidone HCl was found to be 0.25 μg/ml and the quantication limit was about 0.75 μg/ml. The accuracy of the method was established based on the recovery studies and the percentage recovery was in the range of 99.95 to 100.01. The drug was degraded in all the conditions like acid, alkali, oxidative, thermal and photolytic conditions by proposed RP-HPLC method. Research Value: The proposed method can be applied for the routine analysis of Lurasidone HCl in bulk and its pharmaceutical dosage forms in quality control laboratory.

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