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目的采用顶空气相色谱法测定结构甘油三酯中残留的溶剂甲醇和石油醚。方法采用DB-624毛细管色谱柱,程序升温,氢火焰离子化检测器,以DMF为溶剂,顶空平衡温度为80℃。结果在选定的条件下,各组分分离良好;甲醇、正戊烷、正己烷和正庚烷的定量限分别为3.53、0.14、0.24、0.53μg·m L-1;3.5~118.4μg·m L-1甲醇、0.14~195.8μg·m L-1正戊烷、0.24~11.6μg·m L-1正己烷、0.53~199.0μg·m L-1正庚烷与峰面积呈良好的线性关系;甲醇、正戊烷、正己烷和正庚烷的平均回收率分别为100.8%、100.4%、99.5%、99.7%,RSD分别为1.2%、0.9%、0.9%、0.3%。结论所用方法专属、简便,结果准确可靠,可用于结构甘油三酯中残留溶剂的检测。
Objective To determine the residual solvents methanol and petroleum ether in structural triglycerides by headspace gas chromatography. Methods DB-624 capillary column, programmed temperature and flame ionization detector were used. DMF was used as the solvent. The equilibrium temperature at the headspace was 80 ℃. Results Under the selected conditions, the components were well separated. The quantification limits of methanol, n-pentane, n-hexane and n-heptane were 3.53,0.14,0.24 and 0.53μg · m L-1, respectively. L-1 methanol, 0.14 ~ 195.8μg · m L-1 n-pentane, 0.24 ~ 11.6μg · m L-1 n-hexane and 0.53 ~ 199.0μg · m L-1 n-heptane showed a good linear relationship with the peak area The average recoveries of methanol, n-pentane, n-hexane and n-heptane were 100.8%, 100.4%, 99.5% and 99.7%, respectively. The RSDs were 1.2%, 0.9%, 0.9% and 0.3% respectively. Conclusion The method is simple, accurate and reliable, and can be used for the determination of residual solvents in structural triglycerides.