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高效液相色谱-蒸发光散射检测法测定蛋黄卵磷脂的含量

Determination of Egg-Yolk Phosphatidylcholine by Normal-Phase High Performance Liquid Chromatography with Evaporative Light Scattering Detection

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【作者】 龚雁王巧娥杨屹丁明玉

【Author】 GONG Yan~1,WANG Qiao’e~2,YANG Yi~1,DING Mingyu~2(1.Department of Science,Beijing University of Chemical Technology,Beijing 100029,China;2.Key Lab of Bioorganic Phosphorous Chemistry & Chemical Biology,Ministry of Education,Department of Chemistry,Tsinghua University,Beijing 100084,China)

【机构】 北京化工大学理学院清华大学化学系生命有机磷化学及化学生物学教育部重点实验室清华大学化学系生命有机磷化学及化学生物学教育部重点实验室 北京100029北京100084北京100029

【摘要】 建立了蛋黄磷脂中卵磷脂(即磷脂酰胆碱,PC)的高效液相色谱-蒸发光散射检测(HPLC-ELSD)的测定方法。以N ova-Pak S ilica60A硅胶柱(3.9mm i.d.×150mm,4μm)为分离柱,正己烷-异丙醇-3%冰醋酸水溶液(体积比为35∶65∶8)为流动相,等度洗脱,流速1.0m L/m in,柱温30℃。蒸发光散射检测器漂移管温度50℃,雾化气(空气)压力350kPa。在上述条件下测得PC在0.16~1.61g/L范围内线性关系良好(r2=0.997 9),检测限为0.64μg,方法的精密度为3.2%(n=5),回收率为98.2%~128.2%。将该方法用于实际样品的测定,获得了令人满意的结果。该方法预处理简单,分析速度快,可用于蛋黄磷脂中卵磷脂的测定。

【Abstract】 A method for the determination of egg-yolk phosphatidylcholine by normal-phase high performance liquid chromatography(NP-HPLC) with evaporative light scattering detection(ELSD) was developed.Yolk phosphatidylcholine was successfully separated on a Nova-Pak Silica 60A column(3.9 mm i.d.×150 mm,4 μm),using hexane-isopropanol-water containing 3% acetic acid(35∶65∶8,v/v/v) as mobile phase at a flow rate of 1.0 mL/min.The drift tube temperature and air carrier gas pressure of the ELSD were set at 50 ℃ and 350 kPa,respectively.The linear detection range was 0.16-1.61 g/L(r~2=0.9979) and the limit of detection(LOD) was 0.64 μg with excellent relative standard deviation(RSD) of 3.2%(n=5).The recovery was in the range of 98.2%-128.2%.The results indicated that this method is accurate,rapid,simple and reproducible,and thus suitable for the analysis of egg-yolk phosphatidylcholine in real samples.

  • 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,2006年04期
  • 【分类号】O657.72;TQ423
  • 【被引频次】34
  • 【下载频次】676
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