Setting cleaning validation acceptance limits and developing an HPLC method for determination of risperidone residues on manufacturing equipment

Introduction. Risperidone is a potent atypical antipsychotic; residual carryover therefore requires stringent control. Cleaning validation protects product quality by preventing cross-contamination between manufacturing campaigns. Materials and methods. Sampling was performed using Textwipe 714A swabs with direct sampling of manufacturing-equipment surfaces. Risperidone certified reference material (CRM) was used. The HPLC system was Shimadzu Nexera XR UPLC with a LiChrospher RP Select B column (125 × 4.0 mm, 5 µm). The mobile phase was ACN / 0.25% KH2PO4 = 34:66 (v/v) at pH 3.0. Elution was isocratic at 1.0 mL/min and 35 °C. Detection was at 235 nm with injection volume 50 µL. Diluent was methanol / 0.08% H3PO4 = 7:3 (v/v). Validation design included selectivity, accuracy, linearity, precision, and quantification limit. Results. The method met the reported sensitivity, linearity, and precision criteria for routine residue monitoring. Linearity showed R² = 0.9990 over seven concentration levels ranging 0.12–3.6 µg/mL. Limit of quantification was 0.12 µg/mL, precision RSD < 5% at LOQ. Selectivity was demonstrated by chromatographic traces distinguishing risperidone response from matrix and solvent contributions. Acceptance limits were established using the Permitted Daily Exposure (PDE) approach to control cross-contamination risk. Conclusion. The validated RP-HPLC method is suitable for monitoring risperidone in equipment-surface swab samples. PDE-based limits were described as realistic and attainable, supporting routine cleaning validation and cross-contamination control. Key messages. Risperidone residues require stringent cleaning validation to prevent cross-contamination. A sensitive RP-HPLC method was developed and validated for risperidone residue detection on equipment surfaces. PDE-based acceptance limits provide a practical approach for cleaning validation and risk control.

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Publication Details

Journal
DOAJ (DOAJ: Directory of Open Access Journals)
Published
2026-11-02
DOI
https://doi.org/10.5281/zenodo.23887564
Primary Topic
Analytical Methods in Pharmaceuticals
Type
article
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article

Setting cleaning validation acceptance limits and developing an HPLC method for determination of risperidone residues on manufacturing equipment

Milena Prculovska, Irena Slaveska Spirevska, Angela Nikolovska, Kateřina Kochová et al.
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DOAJ (DOAJ: Directory of Open Access Journals)
Analytical Methods in Pharmaceuticals
article

Setting cleaning validation acceptance limits and developing an HPLC method for determination of risperidone residues on manufacturing equipment

Milena Prculovska, Irena Slaveska Spirevska, Angela Nikolovska, Kateřina Kochová, Monika Jakovleska Ruseska, Elena Petrovska Kostadinoska
article en

Abstract

Introduction. Risperidone is a potent atypical antipsychotic; residual carryover therefore requires stringent control. Cleaning validation protects product quality by preventing cross-contamination between manufacturing campaigns. Materials and methods. Sampling was performed using Textwipe 714A swabs with direct sampling of manufacturing-equipment surfaces. Risperidone certified reference material (CRM) was used. The HPLC system was Shimadzu Nexera XR UPLC with a LiChrospher RP Select B column (125 × 4.0 mm, 5 µm). The mobile phase was ACN / 0.25% KH2PO4 = 34:66 (v/v) at pH 3.0. Elution was isocratic at 1.0 mL/min and 35 °C. Detection was at 235 nm with injection volume 50 µL. Diluent was methanol / 0.08% H3PO4 = 7:3 (v/v). Validation design included selectivity, accuracy, linearity, precision, and quantification limit. Results. The method met the reported sensitivity, linearity, and precision criteria for routine residue monitoring. Linearity showed R² = 0.9990 over seven concentration levels ranging 0.12–3.6 µg/mL. Limit of quantification was 0.12 µg/mL, precision RSD < 5% at LOQ. Selectivity was demonstrated by chromatographic traces distinguishing risperidone response from matrix and solvent contributions. Acceptance limits were established using the Permitted Daily Exposure (PDE) approach to control cross-contamination risk. Conclusion. The validated RP-HPLC method is suitable for monitoring risperidone in equipment-surface swab samples. PDE-based limits were described as realistic and attainable, supporting routine cleaning validation and cross-contamination control. Key messages. Risperidone residues require stringent cleaning validation to prevent cross-contamination. A sensitive RP-HPLC method was developed and validated for risperidone residue detection on equipment surfaces. PDE-based acceptance limits provide a practical approach for cleaning validation and risk control.

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Analytical Methods in Pharmaceuticals
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Setting cleaning validation acceptance limits and developing an HPLC method for determination of risperidone residues on manufacturing equipment — Milena Prculovska, Irena Slaveska Spirevska, et al. · DOAJ (DOAJ: Directory of Open Access Journals) (2026) | TGRS Research Map | TGRS