Development of an HPLC-PDA Method for the Simultaneous Estimation of Three Antibiotics in Pharmaceutical Formulations and Bovine Milk and Health Risk Assessment
Mohammad Nasir Uddin , Asif Hasnaine , Md. Sajedul Haque , Suman Das , Monir Uddin , Dipankar Chakraborty , Mohammad Mostafa
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引用次数: 0
Abstract
A simple new, rapid, sensitive, and cost-effective HPLC–PDA method was developed and validated for the determination of tetracycline (TC), oxytetracycline (OTC), and ciprofloxacin (CIP) simultaneously. Chromatographic separations were carried out using a reversed-phase Shim-pack GIS C18 column (4.60 × 250.00 mm; 5.00 µm) at 30°C. Oxalic acid (0.05 M), acetonitrile, and methanol were used as mobile phase under gradient elution conditions at the flow rate of 1.50 mL min−1. Detection wavelength was set at 330 nm. An aliquot of 20.00 µL solution was injected, and three drugs were eluted within 7.39 ± 0.05 min. As per ICH guidelines linearity, recovery, accuracy, precision, selectivity, specificity, sensitivity, stability, column efficiency, system suitability, and robustness were determined for the validation of the proposed method. Calibration curves were linear over a studied concentration range of 8.00 µg mL−1 with a correlation coefficient (r) of 0.999 for all drugs. Relative standard deviation (RSD) for intra− and interday precision was found less than 2.87% and 3.22%, respectively, indicating the method to be reproducible. The proposed method has been suitably applied for the estimation of TC, OTC, and CIP in pharmaceutical formulation and milk samples collected from local market in Bangladesh. Among 15 milk samples analyzed, most of the cases (more than 50%) TC, OTC, and CIP were detected above maximum residue levels (MRLs) though no significant toxicological effect on the health of consumers in the study area was identified.
期刊介绍:
The Journal of Food Protection® (JFP) is an international, monthly scientific journal in the English language published by the International Association for Food Protection (IAFP). JFP publishes research and review articles on all aspects of food protection and safety. Major emphases of JFP are placed on studies dealing with:
Tracking, detecting (including traditional, molecular, and real-time), inactivating, and controlling food-related hazards, including microorganisms (including antibiotic resistance), microbial (mycotoxins, seafood toxins) and non-microbial toxins (heavy metals, pesticides, veterinary drug residues, migrants from food packaging, and processing contaminants), allergens and pests (insects, rodents) in human food, pet food and animal feed throughout the food chain;
Microbiological food quality and traditional/novel methods to assay microbiological food quality;
Prevention of food-related hazards and food spoilage through food preservatives and thermal/non-thermal processes, including process validation;
Food fermentations and food-related probiotics;
Safe food handling practices during pre-harvest, harvest, post-harvest, distribution and consumption, including food safety education for retailers, foodservice, and consumers;
Risk assessments for food-related hazards;
Economic impact of food-related hazards, foodborne illness, food loss, food spoilage, and adulterated foods;
Food fraud, food authentication, food defense, and foodborne disease outbreak investigations.