Search

A novel method for hierarchical screening of illegal adulterants in Fur seal ginseng pills products was developed by multi‐dimensional fingerprint profiling analysis. Fingerprint feature of the samples was acquired by high‐performance liquid chromatography analysis of 11 batches of samples with diode array detector and fluorescence detector, and then potential illegal adulterants including phosphodiesterase type‐5 inhibitors, androgens, α receptor antagonists and yohimbine, were further separated at multiple wavelengths to reduce or remove interferences from sample matrix for highlight their chromatographic characteristics. Accordingly, a hierarchical screening strategy was designed by first‐order and second‐order fingerprints combined with spectral examination to achieve high accuracy and reliability. The method was successfully applied to screening of illegal adulterants in real samples, and it also exhibited good quantification performance through validation tests. From 16 batches of samples, three suspected samples were confirmed to be positive, containing 9.37μg/g of testosterone, 18.8 μg/g of tadalafil, and 48.5 μg/g of sildenafil, respectively. The recoveries and relative standard deviations were in the range of 83.6–103.1% and 4.2–6.8%, respectively. The proposed method provided a simple, efficient and promising alternative to monitoring functional foods. [ABSTRACT FROM AUTHOR]

• Enantioseparation and determination of triazole fungicides was developed by ATPE coupled to 2D-LC. • ATPE extraction of triazole fungicides were optimized by single-factor experiments and SRM. • 2D-LC chromatographic conditions of racemates and enantiomers were investigated respectively. • Simultaneous determination of racemates and enantiomers was validated by online heart-cutting 2D-LC. • The approach was successfully used in analysis of triazole fungicides in vegetables and fruits. A novel method for determination of triazole fungicides and their enantiomers in foods was developed by aqueous two-phase extraction (ATPE) coupled with two-dimensional liquid chromatography (2D-LC). With an aqueous two-phase system (ATPS) of ethanol/K 2 HPO 4 as biphasic extractant, the effects of the ATPS composition, extraction temperature and time on extraction yields of triazole fungicides were investigated. Optimum conditions were concluded as follows: ethanol concentration 31% (w/w) and K 2 HPO 4 concentration 21% (w/w), extraction temperature 60 °C, extraction time 21 min. Based on reversed-phase separation systems, a 2D-LC was constructed by optimizing chromatographic conditions and online heart-cutting procedures. As a result, eight triazole fungicides and their enantiomers were separated respectively on C18 and cellulose-tris (3,5-dimethylphenylcarbamate) stationary phases, revealing good linear relationship in the range of 0.1218–30.06 μg/mL (R2 ≥ 0.9984). The detection limits and recoveries were 0.03113–0.3525 μg/mL and 71.57–107.8%, respectively. The ATPE–2D-LC method was successfully applied to chiral analysis of triazole fungicides in fruits and vegetables. [ABSTRACT FROM AUTHOR]