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目的:建立超临界流体色谱法分离并测定蛋黄卵磷脂中的三棕榈酸甘油酯(TG)、胆固醇(CH)、磷脂酰乙醇胺(PE)、溶血磷脂酰乙醇胺(LPE)、磷脂酰肌醇(PI)、磷脂酰胆碱(PC)、鞘磷脂(SM)、溶血磷脂酰胆碱(LPC)8种磷脂组分。方法:采用Zorbax Silica色谱柱(250 mm×4.6 mm,5μm)与Li Chrosphere 100 Diol色谱柱(250 mm×4 mm,5μm)串联,以二氧化碳为流动相A,甲醇-氨水(100∶0.5)为流动相B,进行梯度洗脱,流速为2.3 m L·min~(-1),柱温为30℃,进样量为5μL,二氧化碳补偿液(甲醇)流速为0.2 m L·min~(-1),蒸发光散射检测器检测,漂移管温度为90℃,雾化气流速为1.2 L·min~(-1)。结果:8种磷脂组分分离完全,且峰面积与浓度的双对数线性关系良好,日内精密度RSD为0.2%~2.0%,日间精密度RSD为0.5%~2.0%,检测限为0.137~0.584μg,定量限为0.273~1.169μg,加样回收率为97.1%~100.6%,RSD为1.1%~2.7%,测得3批蛋黄卵磷脂中的TG为1.6%~1.8%,CH为0.4%~0.5%,PE为7.8%~8.9%,LPE为0.7%~0.9%,PI为0.9%~1.1%,PC为79.1%~83.0%,SM为1.4%~1.5%,LPC为1.6%~1.7%。结论:本文建立的方法可用于蛋黄卵磷脂的质量控制。
OBJECTIVE: To establish a method for the separation and determination of triglyceride (TG), cholesterol (CH), phosphatidylethanolamine (PE), lysophosphatidylethanolamine (LPE) and phosphatidylinositol in egg yolk lecithin by supercritical fluid chromatography PI, phosphatidylcholine (PC), sphingomyelin (SM) and lysophosphatidylcholine (LPC). Methods: The chromatographic separation was performed on a Li Chrosphere 100 Diol column (250 mm × 4 mm, 5 μm) using a Zorbax Silica column (250 mm × 4.6 mm, 5 μm) with carbon dioxide as mobile phase A and methanol- The mobile phase B was eluted with gradient elution at a flow rate of 2.3 m L · min -1 with a column temperature of 30 ° C and an injection volume of 5 μL. The flow rate of the CO2 compensation solution (methanol) was 0.2 mL · min ~ (- 1), detected by evaporative light scattering detector, the drift tube temperature was 90 ℃ and the atomization gas flow rate was 1.2 L · min ~ (-1). Results: The components of eight phospholipids were separated completely, and the logarithm of peak area and concentration had a good linear relationship. The intra-day RSD was 0.2% ~ 2.0%, intraday RSD was 0.5% ~ 2.0%, and the detection limit was 0.137 ~ 0.584μg, the limit of quantification was 0.273 ~ 1.169μg, the recoveries were 97.1% ~ 100.6% and the RSD was 1.1% ~ 2.7%. The TG in three batches of yolk lecithin was 1.6% ~ 1.8% 0.4% -0.5%, PE 7.8% -8.9%, LPE 0.7% -0.9%, PI 0.9% -1.1%, PC 79.1% -83.0%, SM 1.4% -1.5%, LPC 1.6% ~ 1.7%. Conclusion: The method established in this paper can be used for the quality control of egg yolk lecithin.