毛细管气相色谱法测定中药蝉花中角鲨烯的含量

目的: 建立毛细管气相色谱法测定蝉花中角鲨烯的含量,确定蝉花中角鲨烯含量测定的最佳溶剂. 方法: 采用毛细管气相色谱法研究了8种不同提取溶剂对蝉花中角鲨烯含量的影响.色谱条件:HP-5毛细管色谱柱(柱长30 m,内径0.32 mm,涂布厚度0.25 μm,Agilent Technologies);FID检测器,载气为N₂,纯度99.999%,空气流速300 mL·min^-1,氢气流速30 mL·min^-1,程序升温(初始温度180 ℃,以20 ℃·min^-1升温至210 ℃,保持3 min,然后以20 ℃·min^-1升温至250 ℃,保持5 min,最后以5 ℃·min^-1升温至280 ℃,保持5 min);分流进样(10:1);进样口温度为280 ℃,检测口温度为290 ℃. 结果: 角鲨烯的检测浓度在42.90~171.6 μg·mL^-1 范围内线性关系良好(r=0.9999),方法精密度良好(RSD=1.1%),加标回收率为99.08%~100.7%,平均回收率(n=9)为99.70%.正己烷是蝉花中角鲨烯含量测定的最好溶剂,角鲨烯的含量为(74.36±0.24)μg·g^-1. 结论: 经方法学验证本方法可用于蝉花角鲨烯的含量测定.

Objective: To determine the content of squalene in Cordyceps cicadae and the optimum solvent for determination by capillary gas chromatography(GC). Methods: GC method was applied to determine the influence of 8 different extraction solvents on the content of squalene.Chromatography conditions included the HP-5 capillary column(250 mm×0.32 mm,0.25 μm)with FID detector,the nitrogen carrier gas(purity 99.999%),the air velocity of flow at 300 mL·min^-1,and the hydrogen at 30 mL·min^-1.The programmed temperature was started at 180 ℃,then increased to 210 ℃ at a rate of 20 ℃·min^-1,and kept for 3 min,then increased to 250 ℃ at a rate of 20 ℃·min^-1,kept for 5 min,and finally increased to 280 ℃ at a rate of 5 ℃·min^-1 held for 5 min.The split injection was adopted with the split ratio 10:1,the injector temperature at 280 ℃,and the detector temperature at 290 ℃. Results: The results showed that a good linear relationship for the mass concentration of squalene from 42.90 μg·mL^-1 to 171.6 μg·mL^-1 with the correlation coefficient of 0.9999.The recovery rates of squalene in Cordyceps cicadae were 99.08%-100.7%,and their average value(n=9)was 99.70%. n-hexane was the best solvent for determination of squalene content in Cordyceps cicadae,by which,the content of squalene extracted with n-hexane was(74.36±0.24)μg·g^-1 in Cordyceps cicadae. Conclusion: By the methodology the method is suitable for the determination of squalene in Cordyceps cicadae.