采用顶空固相微萃取与气相色谱-质谱法结合进行柑橘蜜中挥发性组分的定性和半定量分析。取柑橘蜜4.00 g与水1.00 g置于顶空瓶中,用DVB/CAR/PDMS纤维头作萃取头,将顶空瓶密封,在50 ℃水浴中搅拌10 min,萃取50 min。取出萃取头,插入气相色谱仪中于255 ℃解吸3.5 min,经TG-5MS毛细管柱分离,质谱测定采用电子轰击离子化方式。用此方法分析了4种柑橘蜜样品,鉴定了72种挥发性组分,主要有醇、烃、酮、醛及酯类化合物,并确定柠檬烯、反式和顺式氧化芳樟醇、β-芳樟醇以及柠檬醛为其特征性成分。按方法对8种样品进行分析,测得各特征性成分的绝对峰面积的相对标准偏差(n=5)在2.9%~20%之间。

GC-MS with head-space SPME was applied to qualitative and semi-quantitative analysis of Chinese citrus honey samples for their volatile components. The fibre head of DVB/CAR/PDMS was used as microextractor in SPME. The honey sample (4.00 g) and water (1.00 g) were mixed in the head-space flask and after capping tightly, it was equilibrated at 50 ℃ for 10 min, and extracted for 50 min. The microextractor was removed out and desorbed (at 255 ℃ for 3.5 min) at the sampling inlet of GC. TG-5MS capillary column was used for chromatographic separation. Mode of EI was adopted in MS. Four Chinese citrus honey samples of different floral origins were analyzed by the proposed method, 72 volatile components were identified, including mainly alcohols, hydrocarbons, ketones, aldehydes and esters, among which limonene, trans- and cis- linalool oxide, β-linalool and citral were acknowledged as characteristic components (or markers). In analyzing 8 honey samples by the present method, values of RSD′s (n=5) of absolute peak area of the markers were found in the range of 2.9%-20%.