Eczacılık Fakültesi / Faculty of Pharmacy
Permanent URI for this collectionhttps://hdl.handle.net/11727/5700
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Item Green Hplc Method For Simultaneous Determination Of N-Acetylcysteine And L-Ascorbic Acid In Co-Formulated Pharmaceutical Products(JOURNAL OF RESEARCH IN PHARMACY, 2024-10-02) Ozen, Gurkan; Nemutlu, EmirhanIt is difficult to analyze different concentrations of pharmaceutical active substances in dosage forms simultaneously, especially in formulations containing high amounts of excipients, on environmentally friendly principles without the need for any intervention. This study proposes a powerful analytical method for the simultaneous determination of L-ascorbic Acid and N- Acetyl Cysteine in an effervescent tablet using high performance liquid chromatography technique. In the study, it was aimed to reduce the use of toxic solvents/chemicals and waste emissions, to increase efficiency and to reduce the negative environmental consequences that may arise from them. The method was developed using a C18 (ACE-121-2546, 4.6 x 250 mm, 5 mu m) column and a sodium dihydrogen phosphate buffer mobile phase. Detection wavelengths were taken as 210 and 240 nm while the flow rate was 1 mL/min. The linearity, accuracy and precision, selectivity, sensitivity, and robustness of the proposed method were validated using International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use Q2R criteria and its green assessment was validated by AGREE and AGREEprep applications. The linear range was taken as 0.1-100 mu g/mL for both compounds analyzed in the developed method. The detection limit of the method was 0.02 and 0.04 mu g/mL respectively for L-ascorbic Acid and N- Acetyl Cysteine. The recovery of the method was between 98.75%102.20% and the accuracy and precision of the method for all compounds were 0.17% and 0.11% respectively. This new environmentally friendly method can be easily used by the chemical and pharmaceutical industries for regular analysis without any restrictions.Item Analysis of 3-hydroxyisovaleric acid and 3-hydroxybutyric acid in plasma samples by LC-MS/MS(2022) Recber, Tuba; Ozkan, Ece; Nemutlu, Emirhan; Beksac, Mehmet Sinan; Kir, SedefDown syndrome is a common genetic disorder that results from the presence of an extra chromosome in the 21st chromosome pair of humans. Metabolomics is an alternative method in discovery of new biomarkers for the screening and diagnosis of Down syndrome. In this study, quantitative analyzes of 3-hydroxybutyric acid and 3hydroxyisovaleric acid, selected as possible markers for prenatal diagnosis of Down syndrome were performed. LCMS/MS analyzes were performed on a Phenomenex Luna NH2(100 x 4.6 mm, 3 mu m) column using a mobile phase mixture of 0.1% formic acid and acetonitrile containing 0.1% formic acid at a flow rate of 0.35 mL/minute. The MRM transitions were 103.0 -> 59.0 for 3-hydroxybutyric acid and 117.1 -> 59.0 for 3-hydroxyisovaleric acid. Under these conditions, the retention times of 3-hydroxyisovaleric acid 3-hydroxybutyric acid were 2.7 and 3.1 minute, respectively. The method was found linear from 0.1 to 10.0 mu g/mL for both metabolites. The limit of detection (LOD) was 0.017 mu g/mL for 3-hydroxybutyric acid and 0.003 mu g/mL for 3-hydroxyisovaleric acid. The lower limit quantification (LLOQ) was 0.045 mu g/mL for 3-hydroxybutyric acid and 0.008 mu g/mL for 3-hydroxyisovaleric acid. The method has been proven to be selective, precise, accurate, sensitive, and robust based on the validation studies results. Finally, the method was applied to plasma samples of the pregnant women with healthy fetus (n = 30) and with Down syndrome fetus (n = 17). As a result of the analysis, a statistically significant increase (p <0.01) was observed in the 3-hydroxybutyric acid level of the group with Down syndrome compared to the healthy group. This result strengthens the use of 3-hydroxybutyric acid as an important biomarker in the prenatal screening/diagnosis of Down syndrome.