气相色谱法测定枳实及其炮制品中柠檬烯的含量

目的建立气相色谱法测定枳实及其炮制品种中柠檬烯的含量。方法分析色谱柱为DB-1,FID检测器温度为350℃。进样口温度为190℃。载气为氮气,柱流速为1.0 mL·min^-1,分流比为30:1。柱温箱程序升温初始温度70℃,以2℃·min^-1的速率升温至150℃,然后以20℃·min^-1升温至280℃,保持直至分析完成。结果枳实及其炮制品种中柠檬烯在0.001~4.806 mg·mL^-1范围内线性关系良好(R^2=0.9999,n=6);平均加样回收率为105.8%(RSD=3.4%,n=6),符合98%~110%限度范围,方法准确性良好。结论该方法操作简便快速、灵敏可靠,重现性好,适用于枳实及其炮制品种中柠檬烯的含量测定。

Determination of Limonene in Aurantii Fructus Immaturus and Its Processed Varieties by Gas Chromatography

OBJECTIVE To establish a method for determining the contents of limonene in Aurantii Fructus Immaturus and its processed varieties by gas chromatography.METHODS Gas chromatography was used.The chromatographic conditions were as follows:chromatographic column:DB-1;FID detector,detector temperature was 350℃,injection port temperature was 190℃,carrier gas:Nitrogen.The column flow rate was 1.0 mL·min^-1,the shunt ratio was 30∶1,the initial temperature of column incubator was set at 70℃,and raised to 150℃with a rate of 2℃·min^-1,and then heated to 280℃with a rate of 20℃·min^-1 until the analysis was completed.RESULTS The calibration curve of limonene in Aurantii Fructus Immaturus was linear in the range of 0.001-4.806 mg·mL^-1(R^2≤0.9999,n=6),The average recovery was 105.8%(RSD=3.4%,n=6),which was in accordance with the limit of 98%-110%.The accuracy of the method was good.CONCLUSION The established method is simple,rapid,sensitive and accurate.It can be used for the determination of limonene in Aurantii Fructus Immaturus and its processed varieties.