Maraschiello C, García Regueiro J A
IRTA, Meat Technology Center, Monells, Girona, Spain.
J Chromatogr A. 1998 Aug 28;818(1):109-21. doi: 10.1016/s0021-9673(98)00531-7.
A procedure designed for the determination of retinol (vitamin A) and alpha-tocopherol (vitamin E) in poultry tissues has been developed. The procedure involves lipid extraction, saponification, solid-phase clean-up and capillary gas chromatography (cGC). Retinol and alpha-tocopherol were determined separately by cGC-flame ionisation detection using a fused-silica open tubular capillary column, 30 m x 0.25 mm I.D. coated with 5% phenylmethylsilicone and with a film thickness of 0.25 micron. Solvent extraction followed by saponification were sufficient to provide a purified extract which was directly analyzed for retinol by cGC in the solvent venting mode. However, in order to accurately determine alpha-tocopherol by cGC, further purification of the extract by solid-phase extraction was necessary. A silica SPE column was used to remove interfering cholesterol from the extract. alpha-Tocopherol was analyzed in its derivatized form. Absolute and relative recoveries for both vitamins from spiked samples were evaluated. Absolute and relative recoveries ranging from 80 to 95% were obtained for both compounds. 5 alpha-Cholestane and alpha-tocopheryl acetate were used as internal standards. Poultry muscle meat and liver tissue were analyzed for their retinol and alpha-tocopherol content and the peaks detected by cGC were confirmed by cGC-mass spectrometry.
已开发出一种用于测定家禽组织中视黄醇（维生素A）和α-生育酚（维生素E）的方法。该方法包括脂质提取、皂化、固相净化和毛细管气相色谱法（cGC）。使用内径为0.25mm、长30m、涂有5%苯基甲基硅氧烷且膜厚为0.25微米的熔融石英开管毛细管柱，通过cGC-火焰离子化检测分别测定视黄醇和α-生育酚。溶剂萃取后进行皂化足以提供纯化提取物，该提取物可通过cGC在溶剂放空模式下直接分析视黄醇。然而，为了通过cGC准确测定α-生育酚，需要通过固相萃取对提取物进行进一步纯化。使用硅胶固相萃取柱从提取物中去除干扰性胆固醇。α-生育酚以其衍生化形式进行分析。评估了加标样品中两种维生素的绝对回收率和相对回收率。两种化合物的绝对回收率和相对回收率均在80%至95%之间。使用5α-胆甾烷和α-生育酚乙酸酯作为内标。分析了家禽肌肉和肝脏组织中的视黄醇和α-生育酚含量，并通过cGC-质谱法对cGC检测到的峰进行了确认。
