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建立了高温气相色谱快速分析棕榈油脂肪酸甲酯(fatty acid methyl ester,FAME)酯交换反应样品中三羟甲基丙烷脂肪酸三酯(trimethylolpropane fatty acid trimester,TFATE)的方法。采用DB-1ht型毛细管柱(15 m×250μm×0.1μm),柱温条件为:起始温度50℃,以50℃/min升至220℃,以30℃/min升至290℃,以40℃/min升至330℃保留2 min,以30℃/min升至370℃保留3 min;载气为高纯氮气,进样口380℃,FID检测器400℃,分流比20∶1,进样量为1μL。制备了TFATE的标准样品,并验证了标准样品的纯度,建立了TFATE的标准曲线,在质量浓度范围0.5～20.0 mg/mL内峰面积与被测物质量浓度线性关系良好。加样回收试验表明,平均加样回收率在96.64%～98.06%之间,RSD在0.20%～0.45%之间,该方法有较好的精密度和重复性。
A method for the rapid analysis of trimethylolpropane fatty acid trimester (TFATE) in the transesterification reaction of fatty acid methyl ester (FAME) by high temperature gas chromatography was established. DB-1ht capillary column (15 m × 250μm × 0.1μm) was used. The column temperature was 50 ℃, raised to 220 ℃ at 50 ℃ / min, raised to 290 ℃ at 30 ℃ / ℃ / min to 330 ℃ for 2 min and 30 ℃ / min to 370 ℃ for 3 min. The carrier gas is high purity nitrogen, the inlet is 380 ℃, the FID detector is 400 ℃ and the split ratio is 20: 1 The sample volume is 1μL. The standard sample of TFATE was prepared, and the purity of standard sample was verified. The standard curve of TFATE was established. The peak area of 0.5 ~ 20.0 mg / mL in mass concentration range was linear with the concentration of analyte. The recovery tests showed that the average recovery was between 96.64% and 98.06%, and the RSD ranged from 0.20% to 0.45%. This method has good precision and repeatability.