摘要
用苯-石油醚(1:1)混合溶剂溶解鱼油,加入2mL0.4mol/L氢氧化钾-甲醇溶液,室温静置10min。加入蒸馏水使全部有机层升至瓶径上部,上清液注入气相色谱仪分析。分离柱采用交联PC-WAX-57CB(50m×0.25mmID×0.2mmDF)毛细管色谱柱;分流进样,载气:He,线速度80cm/min;分流进样,分流比:1:40:汽化室温度:220℃;柱室温度:40℃恒温 2min;以 20℃/min升温至 160℃;再以 2℃/min升温至 200℃恒温 15min;以 1℃/min升温至 225℃。检测器:FID,250℃;C-R4A色谱专用数据处理打印机进行数据处理。采用内标法定量,以C21:0脂肪酸甲酯为内标;EPA和DHA甲酯对内标C21:0甲酯的RRF分别为1.165±0.018和1.187±0.023;重复性试验:SD<5％。经对 12份实际样品测定,结果可靠。
Fish lipid sample 50mg was dissolved in 2ml benzene - petroleum ether(1:1) and added in 2ml 0. 4mol/L KOH methyl alcohol solution, static state in room temperature for 10min after mixed. Added in stilled water until organic layer was risen up to top of the bottom. The higher solution was injected into gas chromatographic system with capillary column coasted PC - WAX -57CB stationary phase. Carrier gas was He at 80cm/s of linear gas velocity, Injector temperature was 220℃ and split ratio was 1: 40. Column temperature program was isothermal at 40℃ for 2min, followed by a temperature gradient to 160℃ at 20℃/min and second gradient to 200℃ at 2℃/min and then hold 200℃ for 15min and followed by third gradient to 225℃ at 1℃/min. C21:0 fat acid methyl ester was used as inner standard and the RRF of methyl ester of EPA and DHA related it were 1.16 ± 0.018 and 1.187 ± 0.023. The result of repeat test was SD< 5 % . The method was good by determination of 12 samples.
出处
《中国国境卫生检疫杂志》
CAS
1998年第6期328-331,383-384,共4页
Chinese Journal of Frontier Health and Quarantine
