GC法测定鱼腥草挥发油中α-蒎烯、β-蒎烯等7种成分的含量

目的: 用GC同时测定鱼腥草挥发油中α-蒎烯、β-蒎烯、β-月桂烯、柠檬烯、4-萜品醇、乙酸龙脑酯和甲基正壬酮7种成分的含量。方法: 色谱柱:HP-5(30 m×0.32 mm×0.25 μm)石英毛细管柱;进样口温度:240 ℃;检测器:FID;检测器温度:260 ℃;柱温:70 ℃为起始温度,保持5 min,以4 ℃·min^-1升温至140 ℃,保持5 min,再以20 ℃·min^-1升温至250 ℃;载气:氮气;流速:1.0 mL·min^-1;进样方式:分流,分流比20:1;萘作为内标。结果: α-蒎烯、β-蒎烯、β-月桂烯、柠檬烯、4-萜品醇、乙酸龙脑酯和甲基正壬酮色谱峰分离良好;进样浓度分别在0.009 8~2.5、0.012~3.1、0.008 0~2.0、0.012~2.9、0.009 1~2.3、0.009 3~2.3、0.009 9~2.5 mg·mL^-1范围内线性关系良好;平均回收率(n=6)分别为99.2%、99.7%、98.2%、100.3%、98.6%、101.4%、99.4%,RSD分别为1.03%、0.95%、1.31%、1.48%、2.03%、1.87%、1.24%。对5批挥发油进行了含量测定,上述7个组分的含量分别为5.22%~11.9%、11.3%~29.4%、5.56%~13.8%、3.38%~4.13%、0.71%~6.27%、2.43%~4.02%、17.0%~27.5%。结论: 建立的鱼腥草挥发油GC含量测定方法简便、快速、准确,为鱼腥草挥发油质量综合评价提供了科学依据。

Objective: To establish a method for simultaneous determination of seven constituents(α-pinene, β-pinene, β-myrcene, limonene, 4-terpineol, bornyl acetate, and methyl n-nonylketone)in volatile oil from Houttuyniae Herba by GC.Methods: The sample was split in the 240 ℃ injection port with 20:1 split ratio, and separated on a DB-5(30 m×0.32 mm×0.25 μm film thickness)fused silica column with nitrogen as the carrier gas, the gas speed was 1.0 mL·min^-1.The temperature program was as follows:70 ℃ for 5min, then 4 ℃·min^-1 to 140 ℃, keep 5 min, 20 ℃·min^-1 to 250 ℃.The FID was used as detector and the FID temperature was set at 260 ℃.Naphthalene was used as internal standard.Results: The chromatographic peaks of α-pinene, β-pinene, β-myrcene, limonene, 4-terpineol, bornyl acetate, and methyl n-nonylketone had good separation.Good linearity of the seven components were obtained within the range of 0.009 8-2.5 mg·mL^-1(r=0.999 9), 0.012-3.1 mg·mL^-1(r=0.999 9), 0.008 0-2.0 mg·mL^-1(r=0.999 9), 0.012-2.9 mg·mL^-1(r=0.999 9), 0.009 1-2.3 mg·mL^-1(r=0.999 9), 0.009 3-2.3 mg·mL^-1(r=0.999 9)and 0.009 9-2.5 mg·mL^-1(r=0.999 9), respectively;the average recoveries of α-pinene, β-pinene, β-myrcene, limonene, 4-terpineol, bornyl acetate, and methyl n-nonylketone were 99.2%, 99.7%, 98.2%, 100.3%, 98.6%, 101.4%, and 99.4%;and the RSDs were 1.03%, 0.95%, 1.31%, 1.48%, 2.03%, 1.87%, and 1.24%, respectively.The contents of α-pinene, β-pinene, β-myrcene, limonene, 4-terpineol, bornyl acetate, and methyl n-nonylketone in five batches of samples were 5.22%-11.9%, 11.3%-29.4%, 5.56%-13.8%, 3.38%-4.13%, 0.71%-6.27%, 2.43%-4.02% and 17.0%-27.5% respectively.Conclusion: The method is simple, rapid, accurate, and provides a scientific basis for quality assessment of volatile oil from Houttuyniae Herba.