SIMPLE AND FAST RP-HPLC METHOD FOR THE DETERMINATION OF PREDNISOLONE SODIUM PHOSPHATE, PREDNISOLONE, ATROPINE, AND HOMATROPINE AS RESIDUALS IN CLEANING VALIDATION OF INDUSTRIAL PHARMACEUTICAL EQUIPMENT

Abstract

Determining traces of pharmaceuticals in equipment is an important step for controlling cross-contamination during the production cycle. Time-consuming analysis is not applicable because it of incremental costs, especially in evaluating residuals as steroids and alkaloids that require a fast and specific technique. Here, an isocratic reversed-phase HPLC method was developed for the trace analysis of Prednisolone Sodium Phosphate (PSP), Homatropine (HOM), Atropine (ATR), and Prednisolone (PRE) in cleaning samples from pharmaceutical equipment. For this, a mobile phase mixture of 35/65 (V/V) acetonitrile/potassium dibasic phosphate 10 m mol L⁻¹, pH 6.9 at 1.0 mL min⁻¹, with a phenyl-hexyl column, were used. These parameters enabled quantifying the analytes within 7.0 min, detecting ATR and HOM at 210 nm, while PSP and PRE were monitored at 240 nm, being lineal between 1–100 µg mL⁻¹ in all cases. The quantification and detection limits were 0.04 and 0.02 µg mL⁻¹ for PSP, ATR, and HOM and 0.02 and 0.01 µg mL⁻¹ for PRE. The method proved its worth and specificity even in presence of other formulation components of the final dosage forms without extraction or concentration procedures.

Keywords:

• atropine
• cleaning validation
• homatropine
• HPLC
• prednisolone
• prednisolone sodium phosphate
• trace analysis

Notes

Y = Area of standard. X = Concentration (µg mL⁻¹).

^a (SD of amount detected = mean of amount detected) × 100 (n = 3).

^b (SD of amount detected = mean of amount detected) × 100 (n = 5).