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单双甘油酯定量分析方法的研究

潘广坤

(广州市糖匠食品有限公司,广东广州511300)

摘要:建立一种高效液相色谱-蒸发光散射检测法定量单双甘酯含量的方法。单双甘酯样品用异丙醇直接溶解,经过0.22滋m 微滤膜过滤处理,色谱柱为C18 反相色谱柱,以异丙醇/ 乙腈为流动相,进行梯度洗脱,洗脱流率为0.5mL/min,漂移管温度:45℃,雾化器温度:36℃,载气压力:25psi。实验结果显示:棕榈酸单甘酯、硬脂酸单甘酯、1,3- 棕榈酸二酯、1,2-棕榈酸二酯、1,2- 硬脂酸二酯和1,3-硬脂酸二酯组分可完全分离,各组分峰面积的常用对数与其进样浓度的常用对数呈现良好线性关系(R2>0.996),检出限(S/N=3)为:0.01~0.02滋g,定量限(S/N=10)为:0.03~0.04μ g,单双甘酯样品中各组分的加标回收率平均值在94.62%~103.70%范围内,RSD<5%。此方法不需要对样品进行衍生化处理,且能够简单、快速、有效地定量单双甘酯样品中单酯含量和甘二酯含量。

关键词:高效液相色谱;蒸发光散射检测器;单双甘油酯;定量

Study on the Quantitative Analysis Method ofMonoglyceryl Ester

PAN Guang-kun

(Guangzhou Sugar Food Co.,Ltd.,Guangzhou 511300,China)

Abstract: A high performance liquid chromatography with evaporative light-scatter detector (HPLC-ELSD)quantitativemethod for monoglyceryl ester was established. The monoglyceryl ester was directly dissolved by isopropyl alcohol,andfiltered by 0.22μm microfiltration membrane. Using C18 reverse phase chromatography column,acetonitrile and isopropylalcohol were used as mobile phase,to gradient elution,with a flow rate of 0.5mL/min. The drift tube temperature wascontrolled at 45℃ and atomizer temperature at 36℃. The pressure of carrier gas was controlled at 25psi. Experimental resultsshowed that the components can be separated completely among monoglyceride palmitate,monoglyceric stearate,1,3-Dipalmitin,1,2-Dipalmitin,1,2-Distearin,1,3-Distearin. The common logarithm for peak area and concentrationshowed good linear relationship(R2 >0.996). The limit of detection(S/N=3)of the method was 0.01~0.02μg and the limitof quantitation(S/N=10)was 0.03~0.04μg. The average standardized recycling ranged from 94.62% to 103.70%and therelative standard deviation (RSD)was less than 5%. The method is simple and rapid for quantifying monoester anddiglyceride contents in monoglyceryl ester without derivatization.

Key words: HPLC;ELSD;monoglyceryl ester;quantification

(2018年第21卷第4期)

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