GC法同时测定北葶苈子中四种脂肪酸的含量

Simultaneous Determination of Four Fatty Acid Components in the Seeds of Semen Lepidii by GC

目的:建立气相色谱法同时测定北葶苈子中棕榈酸、亚油酸、顺-11-二十碳烯酸、芥酸4种脂肪酸的含量。方法:采用超声提取法用石油醚提取样品,对样品进行衍生化处理,使用Agilent DB-5毛细管柱(30 mm×0.32 mm, 0.50μm),程序升温,气化室温度为280℃,FID检测器温度为290℃,载气为高纯氮气,流速为5 ml·min^(-1),进样量为1.0μl,分流比10∶1。结果:棕榈酸、亚麻酸、顺-11-二十碳烯酸、芥酸质量浓度分别在0.425~2.125 mg·ml^(-1)(r=0.999 6)、3.650~18.250 mg·ml^(-1)(r=0.999 4)、0.833~4.166 mg·ml^(-1)(r=0.999 6)、0.453~2.265 mg·ml^(-1)(r=0.999 6)内呈良好线性关系,平均回收率分别为96.88%,96.92%,97.29%,95.66%(RSD≤2.0%,n=9)。结论:首次建立了北葶苈子中4种主要脂肪酸含量的测定方法,对北葶苈子的进一步研究和质量控制有一定的参考意义。

Objective: To establish a method for the simultaneous determination of the contents of palmitoic acid, linolenic acid, cis-11-eicosaenoic acid and erucic acid in the seeds of Lepidium apetalum Willd. by GC. Methods: The samples were ultrasonically extracted by petroleum ether. The GC separation was achieved on an Agilent DB-5(30 m×0.32 mm, 0.50 μm) column with a temperature program at the flow rate of 5 ml·min;after the derivatization of samples. The carrier gas was high purity nitrogen. The flame-ionization detector temperature was 290 ℃ and the injection port temperature was 280 ℃.The injection volume was 1.0 μl. The split ratio was 10∶1.Results: The linear ranges of palmitic acid, linolenic acid, cis-11-eicosenoic acid and erucic acid were 0.425-2.125(r=0.999 6), 3.650-18.250(r=0.999 4), 0.833-4.166(r=0.999 6) and 0.453-2.265(r=0.999 6) mg·ml^(-1), and the average recoveries were 96.88%,96.92%,97.29%,95.66%(RSD≤2.0%, n=9), respectively. Conclusion: The determination method for the four fatty acids was established for the first time, which has certain reference significance for further study and quality control for the seeds of L. apetalum Willd.