Monitoring Residual Solvents in Pharmaceutical Products using a Portable Pre-Concentration Gc-Pid

Abstract

Pharmaceutical manufacturing utilizes solvents at different stages of production. Some of the harmful solvent residuals may be retained in the final product; therefore, they need to be monitored for quality control and to meet the regulation requirement. Here, a novel method capable of rapidly analyzing residual solvents in pharmaceutical products was developed using a compact-portable gas chromatography with a photoionization detector (GC-PID). The method consists of modified Tedlar® bag sampling, online pre-concentration, separation of volatiles by miniaturized GC, and micro-PID detection. The method detection limits of selected residual solvents were in the range of 26.00 – 52.03 pg/mL which is much lower than the pharmaceutical compliance concentration limits. Limits of detection > 520 pg of analyte per grams of sample was also determined for the over-the-counter drugs. The method performance showed rapid speed (5 min), linear calibration (r2 < 0.99), and repeatable retention time (RSD < 0.4 %). Direct analysis of residual solvents in solid samples was conducted without the need for complex sample preparation. The method validation using over-the-counter pharmaceutical products yielded excellent accuracy (recovery > 91.2 %) and precision (RSD < 6.5 %) for the selected residual solvents, including 1,4-dioxane, benzene, chlorobenzene, cyclohexane, xylenes, and toluene. This portable and rapid method could be deployed during the pharmaceutical drug manufacturing processes for quality control.

Department(s)

Chemistry

Keywords and Phrases

On-line pre-concentration; Pharmaceutical products; Portable GC with photoionization detector; Volatile residual solvents

International Standard Serial Number (ISSN)

1873-264X; 0731-7085

Document Type

Article - Journal

Document Version

Citation

File Type

text

Language(s)

English

Rights

© 2024 Elsevier; American Association of Pharmaceutical Scientists, All rights reserved.

Publication Date

15 Oct 2024

PubMed ID

39089199

Link to Full Text

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