Cleaning verification assays for highly potent compounds by high performance liquid chromatography mass spectrometry: Strategy, validation, and long-term performance

Liu, Li; Pack, Brian W.

doi:10.1016/j.jpba.2006.10.008

Cited by 20 publications

(10 citation statements)

References 9 publications

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“…Finally, sample collection and analysis are time-consuming. For example, swabbing and a high-performance liquid chromatography (HPLC) analysis, which is most commonly used for detection in cleaning studies [7], can take several hours. Hence, the verification of the cleaning procedure following each cleaning step is cumbersome, while the FDA requires continued process verification [8].…”

Section: Introductionmentioning

confidence: 99%

Novel Cleaning-in-Place Strategies for Pharmaceutical Hot Melt Extrusion

et al. 2020

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To avoid any type of cross-contamination, residue-free production equipment is of utmost importance in the pharmaceutical industry. The equipment cleaning for continuous processes such as hot melt extrusion (HME), which has recently gained popularity in pharmaceutical applications, necessitates extensive manual labour and costs. The present work tackles the HME cleaning issue by investigating two cleaning strategies following the extrusion of polymeric formulations of a hormonal drug and for a sustained release formulation of a poorly soluble drug. First, an in-line quantification by means of UV–Vis spectroscopy was successfully implemented to assess very low active pharmaceutical ingredient (API) concentrations in the extrudates during a cleaning procedure for the first time. Secondly, a novel in-situ solvent-based cleaning approach was developed and its usability was evaluated and compared to a polymer-based cleaning sequence. Comparing the in-line data to typical swab and rinse tests of the process equipment indicated that inaccessible parts of the equipment were still contaminated after the polymer-based cleaning procedure, although no API was detected in the extrudate. Nevertheless, the novel solvent-based cleaning approach proved to be suitable for removing API residue from the majority of problematic equipment parts and can potentially enable a full API cleaning-in-place of a pharmaceutical extruder for the first time.

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Section: Introductionmentioning

confidence: 99%

Novel Cleaning-in-Place Strategies for Pharmaceutical Hot Melt Extrusion

et al. 2020

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“…The process of cleaning verification is typically conducted by swabbing the spoiled manufacturing equipment, extracting residue from the swab and then subjecting the extract to analysis. High performance liquid chromatography (HPLC) is typically used for analysis of residues [1–3] . The principal disadvantage associated with HPLC analysis is the length of time involved in running the necessary samples.…”

Section: Introductionmentioning

confidence: 99%

“…High performance liquid chromatography (HPLC) is typically used for analysis of residues. [1][2][3] The principal disadvantage associated with HPLC analysis is the length of time involved in running the necessary samples. Adequately representing the cleanliness of the equipment train can result in the analysis of 70-80 swabs.…”

Section: Introductionmentioning

confidence: 99%

Towards the development of a rapid, portable, surface enhanced Raman spectroscopy based cleaning verification system for the drug nelarabine

Corrigan

Salton

Preston³

et al. 2010

Journal of Pharmacy and Pharmacology

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“…The conventional analytical method employed by the pharmaceutical industry for cleaning validation involves sampling of the manufacturing equipment followed by highperformance liquid chromatography (HPLC). 1,[4][5][6][7][8][9] Product Introduction L. Alvarez-Jubete et al, J. Near Infrared Spectrosc.…”

mentioning

confidence: 99%

“…21, 173-182 (2013) Received: 8 January 2013 n Revised: 21 June 2013 n Accepted: 24 June 2013 n Publication: 9 July 2013 contact surfaces on the manufacturing equipment are typically sampled for residual mass quantitation by swab or rinse sampling. 1,[4][5][6][7][8][9] An important disadvantage of the use of HPLC analysis for cleaning validation is the length of time required for the analysis. 1,[10][11][12][13] Presently, cleaning validation of manufacturing equipment involving collection and preparation of samples for HPLC analysis, data acquisition and processing results in a time requirement of up to two days with associated loss of production time.…”

mentioning

confidence: 99%

Feasibility of near Infrared Chemical Imaging for Pharmaceutical Cleaning Verification

Alvarez‐Jubete¹,

Mishra²,

Jones

et al. 2013

Journal of Near Infrared Spectroscopy

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In conformity with the 2011 Food and Drug Administration guidance for industry, Process Validation: General Principles and Practices, there is a requirement for new methodologies that support continued cleaning verification of manufacturing equipment. Near infrared chemical imaging (NIR-CI) represents an attractive alternative to the current methodologies for cleaning verification since it represents a direct, rapid and sensitive technology. The aim of this study was to test the feasibility of NIR-CI for cleaning verification. Stainless steel, glass and Perspex surfaces were soiled with selected active pharmaceutical ingredients (APIs) with the resulting hyperspectral data employed to identify and quantify the dried residues. Correlations to high-performance liquid chromatography (HPLC) swab analysis were also made. Linear models were obtained for the number of API classified pixels and applied soil concentration with R 2 values of 0.90 and 0.98 for caffeine and sulfathiazole sodium salt, respectively, on stainless steel coupons. In the case of caffeine soils on borosilicate glass and Perspex coupons, the obtained R 2 values were 0.95 and 0.96, respectively. These R 2 values suggest a linear relationship between the number of API classified pixels and applied soil concentration. The calculated detection limits for caffeine and sulfathiazole sodium salt soils on stainless steel coupons were 48 µg and 18 µg 50 mm −2 , respectively. For caffeine soils on borosilicate glass and Perspex coupons the calculated detection limits were 33 µg and 27 µg 50 mm −2 , respectively. However, visual inspection of the NIR-CI following the classification function point to limits of detection closer to 1 µg 50 mm −2 or lower. High correlations (R 2 of 0.91 and 0.93 for caffeine and sulfathiazole sodium salt, respectively) were also obtained between NIR-CI API soil quantification and swabbing/ HPLC analysis. This research points to possible future use of portable CI systems for continued cleaning verification of pharmaceutical residues.

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Cleaning verification assays for highly potent compounds by high performance liquid chromatography mass spectrometry: Strategy, validation, and long-term performance

Cited by 20 publications

References 9 publications

Novel Cleaning-in-Place Strategies for Pharmaceutical Hot Melt Extrusion

Novel Cleaning-in-Place Strategies for Pharmaceutical Hot Melt Extrusion

Towards the development of a rapid, portable, surface enhanced Raman spectroscopy based cleaning verification system for the drug nelarabine

Feasibility of near Infrared Chemical Imaging for Pharmaceutical Cleaning Verification

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