A spectrophotometric procedure was developed for determination of cefepime depending on the complexation of the drug with Hg 2 (NO 3) 2 in acid medium (pH 3.5) and measuring the absorbance at 263 nm. Different variables affecting the reaction were studied and optimized. Under the optimized conditions, linear relationship with good correlation coefficient (0.999) was found between the absorbance and the concentration in the range of 3.65-40 µg ml-1. The limits of detection and quantitation were 1.20 and 3.65 µg ml-1 respectively. The stoichiometry of the reaction was studied using Yoe and Jones method and was found to be 1:2 ratio for cefepime : Hg (I). The method was successfully applied for determination of cefepime in its vial with average percentage recovery of 98.95±1.079. The results were favorably compared with those of reference method. The IR study of the formed complex was done and different probabilities of the formed complexes were suggested.
A highly sensitive and selective HPLC method with UV detection was developed for the determination of cefepime in goat plasma and milk. The proposed method was based on the complexation of cefepime with Hg(I) ions that imparts the high selectivity of the proposed method with enhancement of the sensitivity which enabled the analysis of cefepime in complex matrices such as plasma and milk. Detection was performed at 263 nm, using cefuroxime sodium as an internal standard. Chromatographic separation of cefepime and the internal standard was achieved with Aqua RP-C(18) column using methanol/triethylamine-acetate buffer, pH 3.5 (18:82, v/v) as mobile phase at a flow rate of 1 mL/min. Linear detector responses were observed spanning the range of 1.3-20 μg/mL. The LOD for standard cefepime was 0.43 μg/mL, whereas the LOD for cefepime in goat plasma was 0.84 μg/mL and the corresponding value in goat milk was 1.1 μg/mL. No interference from endogenous substances in plasma and milk was observed. The developed HPLC method has been successfully applied for the pharmacokinetic study of cefepime in goat plasma and milk, for the first time, after a single intramuscular injection of 50 mg cefepime/kg body weight.
An innovative quality by design-integrated VA-SALLME-core–shell chromatographic method was developed for the simultaneous determination of DOR and TIM in plasma.
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