高效液相色谱-蒸发光散射法测定保健食品中 磷脂酰丝氨酸的方法优化

Optimization of determination of phosphatidylserine in health foods by high performance liquid chromatography-evaporative light scattering detection

中文关键词:  磷脂酰丝氨酸  旋涡混合辅助超声提取法  高效液相色谱法  蒸发光散射检测器

英文关键词:phosphatidylserine  vortex mixing coupled with ultrasonic extraction  high performance liquid chromatography  evaporative light scattering detector

中文摘要:

      目的 优化高效液相色谱-蒸发光散射法测定保健食品中磷脂酰丝氨酸含量的分析方法。方法 以氯仿-甲醇溶液(9:1, V:V)为提取剂, 样品经旋涡混合辅助超声提取后高效液相色谱仪测定。以硅胶柱(4.6 mm×250 mm, 5 μm)作为分离柱, 流动相为异丙醇:水:乙酸:三乙胺(84:16:1.5:0.08, V:V: V:V), 流速1.0 mL/min, 等度洗脱, 柱温40 ℃。蒸发光散射检测器选择不分流模式, 漂移管温度100 ℃, 载气(氮气)流速为2.0 L/min, 增益值为200。结果 磷脂酰丝氨酸在20~320 mg/L浓度范围内现呈良好线性关系, 相关系数为0.9999, 加标回收率为95.7%~100.7%, 检出限为4.0 mg/100 g, 定量限为11 mg/100 g。采用该方法对14种保健食品中磷脂酰丝氨酸的含量进行测定, 结果符合产品质量标准。结论 该方法适用范围广, 有机溶剂用量少, 数据准确可靠和重现性好, 可满足实验要求。

英文摘要:

      Objective To optimize the method for determination of phosphatidylserine in health foods by high performance liquid chromatography-evaporative light scattering detection (ELSD). Methods The samples were extracted with chloroform-methanol mixture (9:1, V:V) by vortex mix-assisted ultrasound and determined by high performance liquid chromatography. The separation was conducted on a silica gel column (4.6 mm×250 mm, 5 μm) with a mobile phase of isopropanol:water:acetic acid:triethylamine (84:16:1.5:0.08, V:V:V:V). The flow rate was 1.0 mL/min with a isocratic elution system and the column temperature was set at 40 ℃. The ELSD parameters were non-distributary mode, drift tube temperature of 100 ℃, flow rate of nebulizing gas (N2) of 2.0 L/min, and gain of 200, respectively. Results Phosphatidylserine had good linearity in the concentration range of 20-320 mg/L with the correlation coefficient of 0.9999. The recoveries were between 95.7% and 100.7%. The limit of detection was 4.0 mg/100 g and the limit of quantitation was 11 mg/100 g. The method was used to determine the content of PS in 14 kinds of health foods and the results were consistent with the product quality standard. Conclusion This method has the advantages of wide applicability, less solvent consumption, good accuracy and reproducibility, which can meet the requirements of experiment.