气相色谱法分析生物润滑油三羟甲基丙烷脂肪酸三酯的研究

Analysis of Trimethylolpropane Fatty Acid Triester as Biolubricant by Gas Chromatography

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 high temperature gas chromatography method was developed for analyzing trimethylolpropane triester obtained by the transesterifieation of palm oil fatty acid methyl esters （FAME） with trimethylolpropane. The composition of TMP esters was analyzed using a GC equipped with a capillary column DB - 1ht（ 15m×250μm×0.1μm）. The oven temperature was set initially at 50℃ ,increased by 50 ℃/min to 220 ℃, and then increased by 30 ℃/min to 290 ℃ ,increased by 40 ℃/min to 330 ℃ ,held for 2 rain,then increased by 30 ℃/min to 370 ℃ ,and held for another 3 rain. Nitrogen was used as the carrier gas. The injector and detector temperatures were at 380 and 400 ℃ ,respectively ,the split ratio was set at 20：1 and the injection volume was 1 μL. Trimethylolpropane fatty acid triester （TFATE） standard was prepared and verified. The calibration curve of TFATE built by the gas chromatography showed a good linear correlation at concentration range of 0.5 - 20.0 mg/mL. Recovery experiments showed the average recoveries of samples were in range of 96.64%-98.06% with RSD in range of 0.20%-0.45%. The method had good precision and reproducibility for TFATE analysis.