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<p>This study presents a green, near-solvent-free method for quantifying residual BTEX solvents (benzene, toluene, ethylbenzene, and xylene) in injectable antibiotic vials using gas chromatography with flame ionization detection (GC-FID) coupled with solid-phase microextraction (SPME).&#xa0;Among five fabricated functionalized carbon fibers, the fiber coated with a graphene oxide/pyrrole/aniline nanocomposite (Fiber 4) demonstrated superior adsorption capacity. Optimized extraction parameters were established as follows: fiber length 1.5&#xa0;cm, sample temperature 50&#xa0;°C, extraction time 15&#xa0;min, stirring speed 500&#xa0;rpm,&#xa0;and 20% w/v NaCl (0.5&#xa0;g per 2&#xa0;mL sample).&#xa0;Method validation confirmed excellent sensitivity, with limits of detection (LODs) and quantification (LOQs) in the ranges of 0.02–0.15&#xa0;µg/L and 0.09–0.45&#xa0;µg/L, respectively.&#xa0;All concentrations refer to standard solution levels; for solid antibiotic samples (100&#xa0;mg in 2&#xa0;mL), these correspond to LODs of 0.001–0.0075&#xa0;µg/g and LOQs of 0.0045–0.0225&#xa0;µg/g.&#xa0;The method exhibited linearity from&#xa0;0.1 to 500&#xa0;µg/L&#xa0;(R<sup>2</sup> &gt; 0.999) and good precision, with relative standard deviations (RSDs) of 4.8–7.3% at 25&#xa0;µg/L (n = 6). Successful application to real ampicillin and penicillin vials from two manufacturers yielded well-resolved chromatograms with minimal matrix interference.&#xa0;The method achieves detection limits well below ICH Q3C regulatory thresholds, uses minimal methanol (only for stock standards, &lt; 100 µL per batch), and offers a reproducible, economical, and environmentally friendly solution for monitoring Class 1 and 2 residual solvents in critical pharmaceutical products. Quantitative greenness assessment gave an Analytical Eco-Scale score of 85, an AGREE score of 0.78, and a favourable GAPI pictogram.</p> Graphical Abstract <p></p>

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Green Monitoring of Residual BTEX Solvents in Injectable Antibiotics via Functionalized Carbon Fiber Microextraction and GC-FID: Optimization and Validation

  • 期刊论文

  • 发表日期：

    2026年5月18日

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  • Mohammad Reza Vardast,
  • Arezu Fasihi Agbolagh

摘要

This study presents a green, near-solvent-free method for quantifying residual BTEX solvents (benzene, toluene, ethylbenzene, and xylene) in injectable antibiotic vials using gas chromatography with flame ionization detection (GC-FID) coupled with solid-phase microextraction (SPME). Among five fabricated functionalized carbon fibers, the fiber coated with a graphene oxide/pyrrole/aniline nanocomposite (Fiber 4) demonstrated superior adsorption capacity. Optimized extraction parameters were established as follows: fiber length 1.5 cm, sample temperature 50 °C, extraction time 15 min, stirring speed 500 rpm, and 20% w/v NaCl (0.5 g per 2 mL sample). Method validation confirmed excellent sensitivity, with limits of detection (LODs) and quantification (LOQs) in the ranges of 0.02–0.15 µg/L and 0.09–0.45 µg/L, respectively. All concentrations refer to standard solution levels; for solid antibiotic samples (100 mg in 2 mL), these correspond to LODs of 0.001–0.0075 µg/g and LOQs of 0.0045–0.0225 µg/g. The method exhibited linearity from 0.1 to 500 µg/L (R2 > 0.999) and good precision, with relative standard deviations (RSDs) of 4.8–7.3% at 25 µg/L (n = 6). Successful application to real ampicillin and penicillin vials from two manufacturers yielded well-resolved chromatograms with minimal matrix interference. The method achieves detection limits well below ICH Q3C regulatory thresholds, uses minimal methanol (only for stock standards, < 100 µL per batch), and offers a reproducible, economical, and environmentally friendly solution for monitoring Class 1 and 2 residual solvents in critical pharmaceutical products. Quantitative greenness assessment gave an Analytical Eco-Scale score of 85, an AGREE score of 0.78, and a favourable GAPI pictogram.

Graphical Abstract