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酰胺基亲水作用色谱-高效液相色谱-紫外法测定DHA颗粒中的磷脂酰丝氨酸
Quantification of phosphatidylserine in DHA granules by amide-HPLC-UV
【摘要】 目的:建立酰胺基亲水作用色谱-高效液相色谱-紫外法测定DHA颗粒中磷脂酰丝氨酸的含量。方法:以正己烷-异丙醇为提取溶剂对样品进行超声提取;选用Waters XBridge Amide(4.6 mm×250 mm,3.5μm)色谱柱,以乙腈-异丙醇(7∶3)为流动相,流速1.0 m L·min-1,柱温45℃,进样量20μL,紫外检测波长203 nm,单次运行时间10 min。结果:样品中磷脂酰丝氨酸获得很好的分离,在0.11.0mg·m L-1线性关系良好(r=0.999 9);在高、低浓度的回收率(n=6)分别为101.2%和95.8%,RSD分别为1.3%和2.6%;3批样品中磷脂酰丝氨酸含量分别为10.5、10.3、10.6 mg·g-1。结论:本方法操作简捷、环保、高效,经方法学验证,本法专属性、重复性好,准确度高,适应性强,为含磷脂酰丝氨酸功能食品的全面质量控制提供一种新的方法。
【Abstract】 Objective:To establish an Amide-HPLC-UV method for the determination of phosphatidylserine in DHA granules.Methods:The sample was extracted with n-hexane-isopropanol as the extraction solvent.The chromatographic separation was achieved on a Waters XBridge Amide(4.6 mm×250 mm,3.5μm)column using acetonitrile-isopropanol(7∶3)as the mobile phase at a flow rate of 1.0 m L·min-1.The column temperature was45℃,the injection volume was 20μL,the detection wavelength was set at 203 nm,and the single run time was 10min.Results:Phosphatidylserine in the sample was well separated.The calibration curves of phosphatidylserine showed good linearity in the range of 0.1-1.0 mg·m L-1(r=0.999 9).The average recoveries(n=6)at high and low concentrations were 101.2%and 95.8%,respectively;and RSD were 1.3%and 2.6%,respectively.The contents of phosphatidylserine in three batches were 10.5,10.3,10.6 mg·g-1,respectively.Conclusion:This method is simple,environmental and efficient.The established method is proved by methodology validation which is specific,reproducible,accurate and adaptable,that can be applied to overall quality control of phosphatidylserine in functional food.
【Key words】 phosphatidylserine; DHA granules; Amide; HPLC; UV;
- 【文献出处】 药物分析杂志 ,Chinese Journal of Pharmaceutical Analysis , 编辑部邮箱 ,2017年11期
- 【分类号】O657;TS218
- 【被引频次】6
- 【下载频次】223