Determination of Pentachloronitrobenzene and Its Metabolites in Ginseng by Matrix Solid-Phase Dispersion and GC-MS-MS
2009
Li, Jing | Dong, Fengshou | Liu, Xingang | Zheng, Yongquan | Yao, Jianren | Zhang, Changpeng
A rapid method was developed for the determination of pentachloronitrobenzene (PCNB) and its metabolites pentachloroaniline, pentachlorothioanisole residues in ginseng. Extraction and clean-up were carried out in a single step and analysis was accomplished by gas chromatography-mass spectrometry with multiple reaction monitoring. The main parameters affecting extraction yield and selectivity, such as type and amount of dispersant material, clean-up co-sorbent and extraction solvent were evaluated. The best results were obtained using 1 g ginseng, 2 g florisil as dispersant sorbent, 0.5 g neutral alumina as clean-up co-sorbent, and subsequent extraction with 10 mL acetone-n-hexane (5:5, v/v) with assisted sonication and repeated with another 5 mL of the same solvent mixture. The method was validated by analysis of ginseng samples fortified at different concentration levels (0.01-0.10 mg kg⁻¹). Average recoveries (n = 5) ranged from 85 to 95% with relative standard deviation between 2.5 and 11.2%. Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. The detection limits ranged from 0.2 to 0.9 μg kg⁻¹ in ginseng. The method was applied to the analysis of PCNB and its metabolite residues in commercial ginseng samples.
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