The analysis of regulated contaminants in fruit drinks often requires suitable validated and rapid analytical methods for cost-effective food control, and is of considerable interest among the fruit beverage industry. This study demonstrated a rapid and sensitive high-performance liquid chromatography approach for the simultaneous determination of ochratoxin A (OTA), patulin (PAT), 5-hydroxymethylfurfural (HMF), and bisphenol A (BPA) in various fruit drinks. The separations were achieved using a C18 core-shell column with both photo-diode array and fluorimetric detections connected in series. A gradient system consisting of methanol and 0.1% formic acid at a flow rate of 1.2 mL min−1, thermostated at 35 °C, provided fast elution with run time <9 min. Sample pretreatment was optimised to enable extraction of all analytes from fruit drink matrices. The optimised method was validated. Correlation coefficients of R > 0.99 were achieved with detection limits of 0.5 ng mL−1 (OTA), 1.1 ng mL−1 (PAT), 7.9 ng mL−1 (HMF), and 1.0 ng mL−1 (BPA). Recoveries ranged from 82% to 99%. Good relative standard deviations for intraday retention times (≤3.54%) and peak area (≤3.5%) were achieved. The developed multi-contaminants analysis method was successfully applied to determine OTA, PAT, HMF, and BPA in various fruit drinks.
Over the last decades, comprehensive two-dimensional gas chromatography (GC×GC) has emerged as a significant separation tool for high-resolution analysis of disease-associated metabolites and pharmaceutically relevant molecules. This review highlights recent advances of GC×GC with different detection modalities for drug discovery and analysis, which ideally improve the screening and identification of disease biomarkers, as well as monitoring of therapeutic responses to treatment in complex biological matrixes. Selected recent GC×GC applications that focus on such biomarkers and metabolite profiling of the effects of drug administration are covered. In particular, the technical overview of recent GC×GC implementation with hyphenation to the key mass spectrometry (MS) technologies that provide the benefit of enhanced separation dimension analysis with MS domain differentiation is discussed. We conclude by highlighting the challenges in GC×GC for drug discovery and development with perspectives on future trends.
Background:
Polyaromatic hydrocarbons (PAHs) are a class of toxic compounds commonly found in edible vegetable oils as a result of contamination through food processing. Among the wide variety of PAHs existing in edible oils, benzo(a)pyrene (BAP), benzo(a)anthracene (BAA), benzo(b)fluoranthene (BBF) and chrysene (CHR) are commonly monitored due to their toxicity, carcinogenic and teratogenic properties.
Materials and Methods:
In this context, we described a combination of liquid-liquid extraction and dual cartridge solid-phase extraction (dSPE) system for the extraction of BAP, BAA, BBF, and CHR in palm oil derived tocotrienol rich fraction (T3RF), followed by their analysis using GC-MS operating in selected ion monitoring mode (SIM).
Results:
The separation was effected using a DB-5HT column (30 m × 0.250 mm × 0.25 µm) that can operate at a high temperature limit of 400 °C, which enables the separation of the PAHs in < 28 min. The calibration curves were correlated within the range of 1.5–25 µg/ L, with detection limits (S/N: 3) of 0.48–1.35 µg/L, and relative standard deviations of ≤ 0.07% and ≤ 6.85% were achieved for intra-day retention times and peak areas.
Conclusion:
The proposed sample preparation and GC-SIM workflow greatly reduces interference caused by tocotrienol homologues and enables the quantitative determination of BAP, BAA, BBF, and CHR in T3RF and palm fatty acid distillates.
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