GC法同时测定枫香精油中4个主要成分的含量

Simultaneous Determination of Four Components in Essential Oil of Liquidambaris Resin by GC

目的:建立同时测定枫香精油中α-蒎烯、莰烯、β-蒎烯、β-石竹烯4个主要成分含量的GC法。方法:采用DB-5毛细管柱(30 m×0.32 mm,0.25μm),程序升温,进样口温度250℃,FID检测器温度280℃,载气为高纯氮气,流速:1.0 ml·min^(-1),进样量:1μl,分流比:10∶1。结果:α-蒎烯、莰烯、β-蒎烯、β-石竹烯质量浓度分别在0.0353~0.3533 mg·ml^(-1)(r=0.9989)、0.0084~0.0836 mg·ml^(-1)(r=0.9989)、0.0250~0.2501 mg·ml^(-1)(r=0.9990)、0.0511~0.5107 mg·ml^(-1)(r=0.9991)范围内具有良好线性关系;平均回收率分别为98.7%,98.5%,97.6%,98.7%,RSD分别为1.06%,1.28%,1.43%,0.95%(n=6)。各批次枫香精油中4个主要成分的含量范围分别为129.70~177.50 mg·g^(-1)、37.70~56.30 mg·g^(-1)、100.90~141.70 mg·g^(-1)、261.20~333.90 mg·g^(-1)。结论:该方法符合方法学验证要求,可用于枫香精油的多成分含量测定及质量控制。

Objective:To establish a GC method for the simultaneous determination ofα-pinene,camphene,β-pinene andβ-caryophyllene in essential oil of Liquidambaris resin.Methods:GC was performed on a DB-5 capillary column(30 m×0.32 mm,0.25μm)with an FID detector using temperature program.The inlet temperature was set at 250℃.The detector temperature was controlled at 280℃.The carrying gas was high-purity nitrogen(1.0 ml·min^(-1)),the injection volume was 1μl,and the split ratio was 10∶1.Results:The methodology validation for the assay ofα-pinene,camphene,β-pinene andβ-caryophyllene presented that they were in good linear relationships within the ranges of(0.0353-0.3533)mg·ml^(-1)(r=0.9989),(0.0084-0.0836)mg·ml^(-1)(r=0.9989),(0.0250-0.2501)mg·ml^(-1)(r=0.9990)and(0.0511-0.5107)mg·ml^(-1)(r=0.9991)with the average recoveries of 98.7%(RSD=1.06%),98.5%(RSD=1.28%),97.6%(RSD=1.43%)and 98.7%(RSD=0.95%),respectively(n=6).In all batches of essential oil of Liquidambaris resin,the content ranges of four components were(129.70-177.50)mg·g^(-1) forα-pinene,(37.70-56.30)mg·g^(-1) for camphene,(100.90-141.70)mg·g^(-1) forβ-pinene,and(261.20-333.90)mg·g^(-1) forβ-caryophyllene.Conclusion:The established method is in accordance with the requirements of methodology validation,and can be used for the simultaneous determination of multiple components and the quality control of essential oil of Liquidambaris resin.