A Validated Stability-Indicating HPLC Method for Routine Analysis of an Injectable Lincomycin and Spectinomycin Formulation

Abstract

Lincomycin and spectinomycin combination therapy is widely used in veterinary medicine for the treatment of gastrointestinal and respiratory infections caused by lincomycin- and spectinomycin-sensitive microorganisms. A simple, reverse phase HPLC method for the analysis of samples of an injectable lincomycin and spectinomycin preparation containing a mixture of inactive excipients has been developed. The HPLC was carried out using the RP-C18 (250 mm × 4.0 mm, 5 μm) column, with the gradient mobile phase consisting of an acetonitrile and phosphate buffer at pH 6; the flow rate of 1 mL/min and ultraviolet detection at 220 nm. This method was validated in accordance with both FDA and ICH guidelines and showed good linearity, accuracy, precision, selectivity, and system suitability results within the acceptance criteria. A stability-indicating study was also carried out and indicated that this method can also be used for purity and degradation evaluation of these formulations.

RP-HPLC Method Development and Validation of Synthesized Codrug in Combination with Indomethacin, Paracetamol, and Famotidine

“…The robustness of the developed method was performed by doing minor modifications on the method parameters, including detection wavelength, different mobile phase pH, and flow rate [ 30 ]. The studied robustness parameters were the pH effect of the mobile phase (4.9, 5.0, and 5.1), the detection wavelength (273, 275, and 277 nm), and the effect of the mobile phase flow rate (1.2, and 1.4 mL/min).…”

Development of sensitive benzofurazan‐based spectrometric methods for analysis of spectinomycin in vials and human biological samples

“…[1][2][3] SPEC is listed in the US Pharmacopeia and characterized using gas chromatography with a flame ionization detector. [4] In addition, various other methods have been used to determine SPEC, such as spectrophotometry, [5] high performance liquid chromatography (HPLC), [1,[6][7][8] gas chromatography [9] and electrophoresis. [10,11] Several drawbacks have been reported for these methods, such as lack of sensitivity, [5] the need for expensive instrumentation and the use of organic solvents.…”

“…[10,11] Several drawbacks have been reported for these methods, such as lack of sensitivity, [5] the need for expensive instrumentation and the use of organic solvents. [1,[6][7][8] 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) is a chemical reagent that reacts with amine moietycontaining drugs forming fluorogenic and chromogenic products under alkaline conditions. [12][13][14][15] The methods presented here represent the first use of NBD-Cl to derivatize SPEC, firstly measuring the product spectrophotometrically at 410 nm and secondly measuring the product spectrofluorimetrically at 530 nm (λ ex at 460 nm).…”

Comparison of an Enzyme-Linked Immunosorbent Assay with an Immunochromatographic Assay for Detection of Lincomycin in Milk and Honey

“…Microbiological tests are both time-consuming and nonspecific (Gaudin et al, 2013). Even though GC (Luo et al, 1996;Tao et al, 2011), LC, and HPLC (Abualhasan et al, 2012;Dousa et al, 2006) are highly efficient, these methods contribute to significant waste of sample and require extensive cleanup. Fluorescent (Kamenik et al, 2009;Zhou et al, 2014) and UV-based (Olsovska et al, 2007) LIN detection methods require complicated derivatization steps due to the absence of a chromophore or a conjugated compound.…”