Cleaning Validation for Estimation of Vincamine Residues on the Pharmaceutical Equipment Surfaces

Imeda Rubashvili, Validation Department, Aversi-Rational Ltd, Tbilisi, Georgia
Natela Karukhnishvili, Quality Control Laboratory, Aversi-rational Ltd, Tbilisi, Georgia
Nino Dvali, Quality Control Laboratory, Aversi-rational Ltd, Tbilisi, Georgia

Cleaning validation is a critical analytical responsibility of quality assurance system in pharmaceutical industry and ensures the efficiency of the cleaning routine procedure used in production which means that it effectively removes active pharmaceutical ingredient residues from the manufacturing equipment surfaces below a predetermined level and to prevent cross-contamination of next product.

The aim of this study was to demonstrate the applicability of developed HPLC method for quantitative estimation of vincamine residues in cleaning control swab samples taken from stainless steel surfaces after manufacturing of Glatan (vincamine 30 mg) uncoated tablets and the efficiency of the developed cleaning procedure. Vincamine is practically insoluble in water and adherent to surfaces. The swab sampling method was developed in order to obtain a suitable recovery (>90 %). The selected surface (sampling area - 5 × 5 cm²) was successively wiped with one micro polyester swab (3×2.5×10 mm) moistened with diluent – methanol.

The method was developed using LC system “Ag 1260 Infinity” and  Luna C18(2) 150 × 4.6 mm, 5 µm column with a mobile phase - a mixture of 0.1 M ammonium acetate solution and acetonitrile (40 : 60); The flow rate – 1.0 ml/min; The detector wavelength - 280 nm; The injection volume – 50 μL. The method was validated with respect to robustness, system suitability test, specificity, linearity-range, accuracy, precision (intra-day and inter day), limit of detection (LOD) and quantitation (LOQ). The stability of solutions of vincamine was also studied. These studies were performed in accordance with established guidelines.

The calibration curve is linear r²=1.00000 over a concentration range 0.025 – 150 µg/mL; LOD - 0.005 µg/mL and LOQ - 0.025 µg/mL; The determined concentration of vincamine residues in swab sample solutions varies from 0.0069 - 11.60 µg/mL which is well below the limit of cross-contamination (123 µg/mL) of next product.