气相色谱法测定中药蝉花中角鲨烯的含量

 Tengzhou City Xiangying Analysis Technology Co., Ltd. to establish a capillary gas phase chromatography determination of Cordyceps cicadae squalene content, determine the optimum solvent for the determination of Cordyceps cicadae squalene content.            The heating heating heating, heating, XiangyingGC7990plus methods: using capillary gas chromatography method was used to study the 8 kinds of different extraction solvents on Cordyceps cicadae squalene content. Chromatographic conditions: capillary chromatographic column (column length of 30 m diameter 0.32 mm, coating thickness of 0.25 m; FID detector, carrier gas N2, purity of 99.999%, air flow rate of 300 ml min-1, hydrogen flow rate of 30 ml / min, the program (initial temperature of 180 DEG to 20 DEG min-1 to 210 DEG C and kept for 3 min, then to 20 DEG min-1 to 250 DEG C and maintained for 5 min, and finally to 5 DEG C min-1 to 280 DEG C and maintained for 5 min); shunt injection (10:1); sampling outlet temperature of 280 DEG C to detect temperature of 290 degrees centigrade.          Results: the squalene concentration detected in 42.90~171.6 [mu] g-kg – ml-1 linear relations of good (r = 0.9999). The method precision good (RSD was 1.1%.), and the recovery rate is 99.08%~100.7%. The average recovery (n = 9) 99.70%. Hexane is the best solvent Cordyceps cicadae squalene content determination, the content of squalene as (74.36 + 0.24) g, respectively.Conclusion: the method validation of this method can be used to determine the content of cicada squalene.
         滕州市翔鹰分析技术有限公司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*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:毛细管色谱柱(柱长30 m,内径0.32 mm,涂布厚度0.25 μm,XiangyingGC7990plus);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,*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*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.