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利用电喷雾质谱(ESI-MS)及高效液相色谱-蒸发光散射检测器(HPLC-ELSD)法分析聚甘油酯的组成及含量。以聚甘油与脂肪酸乙酯为原料,先采用碱催化酯交换法制备聚甘油酯,然后再用ESI-MS法在正离子模式下定性分析,最后通过HPLC-ELSD法进行定量分析及HPLC-ESI-MS法对所建立的分析方法进行验证。所建立的色谱条件为:C8色谱柱,以甲醇-水为流动相进行梯度洗脱,流速为1.0m L/min,柱温为30℃,漂移管温度为75℃,气体流速为2.0L/min,增益为1,按峰面积归一化法计算各组分的相对含量。结果表明,精制后的样品主要由单酯、二酯、三酯和四酯组成;当原料摩尔比为1∶1时,单酯为主要组分,其含量占56.47%~80.79%;当原料摩尔比为1∶2时,二酯为主要组分,其含量占51.63%~68.21%;所建立的方法简便、灵敏度高、准确、重现性好。
The composition and content of polyglycerol ester were analyzed by electrospray ionization mass spectrometry (ESI-MS) and high performance liquid chromatography-evaporative light scattering detector (HPLC-ELSD). Polyglycerol and fatty acid ethyl ester were used as raw materials. Polyglyceryl ester was first prepared by ester-catalyzed transesterification. The polyglycerol ester was then qualitatively analyzed by ESI-MS in positive mode. The quantitative analysis by HPLC-ELSD and HPLC-ESI -MS method to verify the established analytical method. The established chromatographic conditions were as follows: C8 column, gradient elution with methanol-water as mobile phase at a flow rate of 1.0 mL / min, a column temperature of 30 ℃, a drift tube temperature of 75 ℃ and a gas flow rate of 2.0 L / min, gain of 1, according to the peak area normalization method to calculate the relative content of each component. The results showed that the purified samples mainly consisted of monoester, diester, triester and tetraester. When the molar ratio of the raw materials was 1: 1, the monoester was the main component, accounting for 56.47% ~ 80.79% The molar ratio of 1: 2, the diester as the main component, its content accounted for 51.63% ~ 68.21%; The established method is simple, high sensitivity, accurate, reproducible.