GC法同时测定蜂房药材中5个脂肪酸的含量

目的: 建立衍生化气相色谱法同时测定蜂房药材中脂肪酸类含量的方法,比较不同产地的蜂房中5个脂肪酸的含量. 方法: 采用AB-INOWAX毛细管色谱柱(30 m×0.25 mm,0.25 μm);程序升温,起始温度150℃,以5℃·min^-1速率升至190℃,保持2 min;再以5℃·min^-1速率升至240℃,保持9 min.进样口温度250℃;FID检测器,检测器温度250℃;载气为氮气,流速1.83 mL·min^-1;分流比为80: 1. 结果: 棕榈酸甲酯、硬脂酸甲酯、油酸甲酯、亚油酸甲酯、α-亚麻酸甲酯质量浓度分别在0.08~0.77、0.02~0.23、0.17~2.70、0.11~1.12、0.08~0.82 mg·mL^-1范围内呈现良好的线性关系,相关系数分别为0.999 9、0.999 7、0.999 3、0.999 8、0.999 8;平均回收率(n=6)分别为102.4%、103.3%、98.0%、100.2%、97.7%,RSD均≤2.5%.按脂肪酸甲酯标准曲线计算,并换算为脂肪酸含量,12批样品中棕榈酸、硬脂酸、油酸、亚油酸、α-亚麻酸的含量测定结果分别为1.42~24.79、0.48~2.72、1.89~34.48、0.78~4.81、1.26~19.55 mg·g^-1. 结论: 该方法可作为蜂房中脂肪酸的含量测定及鉴别方法.

Objective: To establish an assay method of multiple components of fatty acids,for comparing the quality of Nidus Vespae collected from different areas. Methods: A capillary column AB-INOWAX (30 m×0.25 mm,0.25 μm) was used,and the heating program was 150℃ programmed to 190℃ at 5℃·min^-1 and kept for 2 min, and then risen to 240℃ and kept for 9 min;the injector temperature was 250℃; the detector temperature was 250℃; the flow rate was 1.83 mL·min^-1;the split injection was conducted with split radio of 80: 1.Nitrogen was used as carrier gas. Results: Good liner relationships were observed between the masses and the peak areas of methyl palmitoleate,methyl stearate,methyl oleate,methyl linoleate,α-methyl linolenate in the ranges of 0.08-0.77 mg ·mL^-1(r=0.999 9),0.02-0.23 mg·mL^-1(r=0.999 7), 0.17-2.70 mg·mL^-1(r=0.999 3),0.11-1.12 mg·mL^-1 (r=0.999 8),0.08-0.82 mg·mL^-1(r=0.999 8),respectively.The average recovery rates (n=6) were 102.4%,103.3%,98.0%,100.2% and 97.7% respectively and RSD≤2.5%.In the 12 batches of samples,fatty acid contents were calculated by fatty acid methyl ester standard curve,and the contents of palmitic acid,stearic acid, oleic acid,linoleic acid,α-linolenic acid were in the ranges of 1.42-24.79 mg·g^-1,0.48-2.72 mg·g^-1,1.89-34.48 mg·g^-1,0.78-4.81 mg·g^-1,1.26-19.55 mg·g^-1. Conclusion: The GC method can be used for the determination and identification of fatty acids in Nidus Vespae.