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Rapid determination of nosiheptide in feed based on dispersive SPE coupled with HPLC
Author(s) -
Xie Jingmeng,
Song Xuqin,
Zhang Yingxia,
Zhang Meiyu,
Li Xuezhi,
He Limin
Publication year - 2019
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201801036
Subject(s) - chromatography , formic acid , chemistry , elution , solid phase extraction , extraction (chemistry) , acetonitrile , high performance liquid chromatography , ammonium acetate , sorbent , aqueous solution , calibration curve , detection limit , adsorption , organic chemistry
A novel, simple, and reliable method based on high‐performance liquid chromatography coupled with fluorescence detection has been developed for the determination of nosiheptide in feed. The feed samples were extracted with acetonitrile 0.1% formic acid aqueous solution and then purified via a dispersive solid‐phase extraction procedure using silica gel powder as the sorbent. Using a mixture of acetonitrile and 5 mM ammonium acetate solution (containing 0.1% formic acid) as the mobile phase, good separation and peak shape were obtained for nosiheptide on a Poroshell C 8 column (250 × 4.6 mm id, 4 μm) via the isocratic elution program. The resulting calibration curve shows high levels of linearity ( r 2 > 0.999) for nosiheptide concentrations of 50–1000 μg/L. At three spiked levels, i.e., 0.500, 2.50 and 5.00 mg/kg, the intra‐ and interday recoveries of nosiheptide in five types of feed ranged from 78.5–96.8 and 84.9–94.2%, respectively. The intra‐ and interday relative standard deviations were less than 10.8%. The limits of quantification for nosiheptide in complete feed and premixes were measured as 50 and 100 μg/kg, respectively. Compared with other common adsorbents, silica gel presents stronger recovery and purification results for feed samples during the dispersive solid‐phase extraction process.