Development and Validation of a Stability Indicating RP-UPLC Method for Analysis of Imipramine Hydrochloride in Pharmaceuticals

Abstract

The objective of the current study was the development of a simple, rapid, and accurate isocratic reverse-phase ultra-performance liquid chromatographic (RP-UPLC) method for the routine control analysis of imipramine hydrochloride (IMH) in bulk drug and in pharmaceutical formulations. This work was carried out in order to reduce analysis time and maintaining good efficiency which in turn is focused on high-speed chromatographic separations. The method was developed using Waters Acquity BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with mobile phase consisting of a mixture of acetonitrile and ammonium acetate buffer of pH-5 (80 : 20, v/v/v). UV detection was performed at 220 nm for eluted compound. An excellent linearity was observed in the concentration range 0.2–3 µg/mL IMH with a regression coefficient () value of 0.9999. The method developed was validated and forced degradation was performed as per ICH guidelines. The limit of detection () was 0.2532 ng/mL and the limit of quantitation () was found to be 0.7672 ng/mL. The drug IMH was subjected to hydrolytic, acidic, basic, thermal, photolytic, and oxidative stress conditions according to ICH regulations. IMH was found to be stable in basic, thermal, and photolytic conditions and degrades in acidic, hydrolytic, and oxidative stress conditions.

Simultaneous colorimetric detection of four drugs in their pharmaceutical formulations using unmodified gold nanoparticles as a probe

“…Table 1 shows the analytical data of the present method for simultaneous colorimetric detection of four drugs using unmodied Au NPs as a probe. Compared with the performance of chromatographic [7][8][9][10][11][12][13][14] and spectrophotometric [16][17][18][19] methods for detection of four drugs, the present method demonstrated a lowered detection limit and a simplied procedure (without the any sample pretreatment at minimal volume of samples) (Table 2). Although LC-MS is an efficient tool for separation and determination of four drugs independently, the unmodied Au NPs-based colorimetric method is particularly attractive for simultaneous detection of four drugs because the color changes can be easily discerned with the naked-eye and then quantied by UV-visible spectrometry, which avoids tedious sample preparations and complicated instrumentation.…”

“…[1][2][3][4][5][6] Identication and quantication of four drugs (venlafaxine; imipramine; amlodipine; alfuzosin) require a simple, specic and sensitive method for routine analysis of individual drug in biological samples. So far, various analytical techniques including high performance liquid chromatography (HPLC), [7][8][9][10] liquid chromatography with mass spectrometry (LC-MS), 14 capillary electrophoresis, 15 uorescence 16 and UV-visible spectrometry [17][18][19] have been used for the analysis of four drugs independently in pharmaceutical and biological samples. However, some of these methods are expensive, somewhat time consuming, they require derivatization steps and expensive instruments, which makes it unavailable in many laboratories for the analysis of four drugs in biological samples.…”

Kinetic Modeling of API Oxidation: (2) Imipramine Stress Testing

“…Here, we demonstrate the value and potential of ab initio kinetic modeling for API degradation via a case study of imipramine (Figure ), an API used in the treatment of depression, diabetic neuropathy, and panic disorder . Imipramine is an ideal compound for initial studies that employ new technologies because its modest size is computationally tractable for high-level QM methods and its intrinsic susceptibility toward oxidative degradation is an active area of research. − The goal of the present work is to build a quantitative kinetic model for the radical-initiated oxidation ( i.e. , autoxidation) of imipramine in the azobis­(isobutyronitrile) (AIBN)/H 2 O/CH 3 OH “forced degradation” system .…”