摘要
目的建立加校正因子GC内标法测定鱼肝油中EPA和DHA含量。方法样品经皂化、甲酯化、异辛烷提取,采用DB-23(30 m×0.25 mm,0.25μm)毛细管柱,FID检测器,程序升温(起始温度170℃,以1℃·min^(-1)的速率升温至225℃,保持5 min),进样口温度为250℃,检测器温度为280℃,高纯N2为载气,流速为1.0 mL·min^(-1),分流比为100∶1,二十三烷酸(C23∶0)甲酯为内标物。结果 EPA、DHA的峰面积比和浓度比分别在0.048 7~9.740 mg·mL^(-1),0.051 0~10.206 mg·mL^(-1)内呈良好的线性关系(r=1.000 0),EPA、DHA的平均回收率分别为98.7%(RSD=0.98%),99.4%(RSD=1.34%)。结论该方法简便、准确、重复性好,可用于鱼肝油的质量控制和掺假鉴定。
OBJECTIVE To establish a method for the determination of EPA and DHA in cod-liver oil by gas chromatography internal standard method with relative correction factor. METHODS The samples were saponified, methyl esterified and extracted with isooctane. The sample was chromatographed on a DB-23(30 m×0.25 mm, 0.25 μm) capillary column with a FID detector. The column temperature was raised by program(the initial temperature was 170 ℃ and the temperature was raised to 225 ℃ at a rate of 1 ℃·min(-1) for 5 min). The injector temperature was 250 ℃, detector temperature was 280 ℃, high purity nitrogen was used as carrier gas, flow rate was 1.0 mL·min(-1), split flow was 100∶1, methyl ester(C23∶0) was used as an internal standard. RESULTS EPA and DHA showed good linear relationships(r=1.000 0) with the peak area ratio and concentration ratio at the range of 0.048 7-9.740 mg·mL(-1), 0.051 0-10.206 mg·mL(-1), respectively. The average recoveries of EPA and DHA were 98.7%(RSD=0.98%), 99.4%(RSD=1.34%). CONCLUSION The method is sample, accurate and reproducible. It can be used for the quality control and adulteration identification of cod-liver oil.
作者
王琼芬
刘婷
郑平安
徐虹
WANG Qiongfen;LIU Ting;ZHENG Pingan;XU Hong(Zhoushan Institute for Food and Drug Control,Dinghai 316021,China;Hailisheng Group Co.,Ltd.,Dinghai 316021,China)
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2018年第9期1322-1326,共5页
Chinese Journal of Modern Applied Pharmacy
基金
浙江省食品药品监管系统科技计划项目(SP201627)