Impurities profiling of brands of ceftriaxone sodium injection marketed in Ibadan, Southwest Nigeria
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Abstract
Background: Several factors can affect the effectiveness of a drug in therapy. One of such is the presence of impurities.
Objectives: Based on the current useful utility status of ceftriaxone injection as an antibacterial agent, a comprehensive impurity profiling of thirteen brands was carried out in order to provide a basis for specifying appropriate storage conditions.
Methods: The profiling was carried out by developing a new liquid chromatographic method with UV detection. Factors that could affect the separation method such as elution mode, pH, flow rate, detection wavelength and type of organic modifier were studied. Validation studies comprising calibration curve, LOD and LOQ determination, accuracy and repeatability were determined. The method was successfully applied to the determination of ceftriaxone and impurities in 13 brands of ceftriaxone injections.
Results: The developed method involved separation of ceftriaxone and major impurities within 15 minutes using gradient elution with KH2PO4 (pH 7.5) and methanol (flow rate, 1 mL/min). Separation was achieved on 2 a C-18 column at 220 nm. Linearity was obtained within the range 7.8–250 μg/mL (r = 0.9996) with LOD and LOQ as 74.56 and 225.9 ng/mL respectively. Relative errors from the intra- and inter-day assessment were generally less than 2%. All the brands complied with the content BP specification of 92-108% of ceftriaxone. However, the impurities content in all the 13 brands were far higher than the 0.2% specified by ICH for the dose of the drug.
Conclusion: There is need for measures to adequately control storage conditions of the injection in order to limit impurities content.
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