Search

A simple, rapid, specific and precise liquid chromatography--tandem mass spectrophotometric (LC-MS/MS) method was developed and validated for quantification of Erlotinib, in human plasma. Erlotinib d6 was used as internal standard, added to plasma sample prior to extraction using acetonitrile as a precipitating agent. Chromatographic separation was achieved on Phenomenex Luna C18 column (50 mm x 1 mm, 5 µm) with acteonitrile: 10 mM ammonium formate buffer (80 : 20, v/v) as an isocratic mobile phase with a flow rate of 0.5 mL/min. Quantitation was performed by transition of 394.0 → 278.0 (m/z) for Erlotinib and 400.0 → 278.0 (m/z) for Erlotinib d6. The lower limit of quantitation was 10 ng/mL with a 100 mL plasma sample. The concentrations of nine working standards showed linearity between 10 and 5000 ng/mL ([r.sup.2] ≥ 0.9992). Chromatographic separation was achieved within 3.50 min. The average extraction recoveries of 3 quality control concentrations were 94.25% for Erlotinib and 93.55% for Erlotinib d6. The coefficient of variation was ≤ 15% for intra- and inter-batch assays. The developed method was successfully applied to the determination of Erlotinib pharmacokinetics after oral administration. Keywords: LC-MS/MS, Erlotinib, Erlotinib d6, validation, human plasma DOI: 10.1134/S1061934815120151, Erlotinib hydrochloride is used to treat non-small lung cancer, pancreatic cancer and several other types of cancer. It is a reversible tyrosine kinase inhibitor, which acts on the epidermal growth [...]

Stability study for dolutegravir bulk drug was performed and the degradation products formed were identified by chromatography (HPLC, LCMS) and spectroscopy (ESI-MS, FTIR, 1H and 13C NMR) techniques. Degradation of the drug in acidic and peroxide environment yielded one common major degradant f ((2,4-difluorophenyl) methanamine) with a mass peak at m/z = 182.44. In addition to this, five more minor degradation products (a, b, c, d and e) were formed. The structure interpretation showed that the drug degraded to its synthetic precursor and no extra structures were formed. Hence, it was suggested that drug dolutegravir should be kept away from acidic and oxygen rich conditions. [ABSTRACT FROM AUTHOR]

Saroglitazar is a newly approved oral hypoglycemic drug by FDA. Although the drug entered the market, there are no reports on its degradation products till date. To identify the degradation products of saroglitazar during the stability studies, a RP-HPLC method was developed and validated as per ICH guidelines. The samples were eluted using acetonitrile and phosphate buffer (pH 7.4, 50:50 v/v) as a mobile phase over Kromasil 100- 5C18 (250×4.6 mm, 5μm) column. The analytes were monitored by UV detector at 294 nm with isocratic mode of elution at a flow rate of 1.0 mL/min. The stability studies were conducted under stressed conditions of acidic, basic, neutral (peroxide), photolytic studies at room temperature and thermal at 60oC for 48 hours. The stressed samples were analyzed for their degradation products by RP-HPLC. The degradant products obtained were characterized using UPLC with tandem mass spectroscopy (LC/MS/MS) and FTIR. Major degradation products were observed with m/z at 365, 247 and 294. The drug is found to be comparatively stable under photo and thermal stress. Peroxide stress has degraded the drug completely. The drug has to be stored away from oxidation during transport and storage. [ABSTRACT FROM AUTHOR]

ABSTRACT Objective To study the role of epidural steroid injection (ESI) in patients with lumbar disc herniation (LDH) and lumbar canal stenosis (LCS). ESIs are regularly used to support non-operative treatment for LBP, and our anecdotal impression is that a considerable proportion of patients report substantial pain relief after ESI. Methods One thousand consecutive patients (645 patients with LDH and 355 patients with LCS) who required ESI from January-August 2018 were included. All were given the same ESI, prepared with triamcinolone (80 mg), bupivacaine (0.25%, 4 ml) and normal saline (4 ml). Patients were evaluated using the numerical rating scale (NRS) immediately after the injection, after 7 days, and after 3 months. Results The mean NRS back-pain score of the LDH-group was reduced from 5 (range: 4-8) to 4 (range: 2-7) immediately after injection, 2 (range: 1-7) after 7 days and 2 (range: 1-7) after 3 months (p-value