The volatile oils in fresh red pine needles from Xiao Hinggan Mountains,were extracted by steam distillation,and then analyzed by comprehensive two-dimensional gas chromatographytime-of-flight mass spectrometry (GC × GC-TOF MS).The chromatographic separation conditions were optimized,and the best conditions were confirmed to be a modulation period of 6 s,a second dimensional column length of 3 m,and a temperature of 20 ℃ for the second dimensional column higher than that for the first dimensional column all the time.Under the optimal conditions,217 kinds of compounds were identified based the NIST library,and the quantitative calculation was carrled out by area normalization method.Total of the compounds identified was four times more than that identified by one-dimensional gas chromatography (1DGC).124 terpenoids,including 48 monoterpenoids,64 sesquipenoids and 12 diterpenoids were identified from the volatile oils of fresh red pine needles,accounting for about 69％ of all.And 33 ester compounds accounting for about 12％ of all,6 organic acids,15 alcoholic compounds,15 aldehyde compounds,11 ketone compounds and 13 other compounds were also identified.Compaired with the one-dimensional gas chromatography,two-dimensional gas chromatography-time-of-flight mass spectrometry possesses higher resolution and sensitivity,and it shows a unique superiority in the analysis of complex natural products.%选取产于小兴安岭的新鲜赤松松针,采用水蒸气蒸馏法提取其中的挥发油,并通过全二维气相色谱/飞行时间质谱(GC × GC/TOF MS)对松针挥发油进行分析和鉴定.对色谱条件进行了优化,确定调制周期为6 s,二维色谱柱长为3 m,二维柱箱相对一维柱箱温度高20 ℃为最佳色谱条件.通过分析,鉴定出217种物质,其中萜类124种,包含单萜48种、倍半萜64种、二萜12种,共占总含量约69％,酯类33种,占总含量约12％,有机酸类6种,醇类15种,醛类15种,酮类11种和其他类化合物13种.相比于传统一维色谱(1DGC),全二维气相色谱(GC×GC)能提供数倍的峰容量,并对一些天然产物的异构体有着很好的分离,因此其在复杂天然产物分析方面具有独特优势.
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