提出了顶空固相微萃取-气相色谱-串联质谱法测定香精香料中黄樟素含量的方法。为使固相微萃取达到更高的效率,选用65 μm聚二甲基硅氧烷/二乙烯苯作为微萃取的涂层,萃取温度及时间为(25±5) ℃和30 min。用DB-5MS毛细管色谱柱分离,电子轰击离子源串联质谱模式检测。选定黄樟素的母离子和子离子分别为m/z 162和m/z 131,内标丙酸苯乙酯的定量离子为m/z 104。黄樟素的线性范围为20~1 000 ng·g-1,方法的检出限(3S/N)为2.2 ng·g-1。在3个浓度水平上做回收试验,加标回收率在71.1%~114.0%之间,相对标准偏差(n=5)在3.4%~16%之间。

GC-MS/MS with headspace-solid phase micro-extraction (HS-SPME) was applied to the determination of safrole in essence and perfume. To attain a higher efficiency in SPME, 65 μm PDMS/DVB fiber was selected as coating for the micro-extraction, and the extraction was carried out at (25±5) ℃ for 30 min. The analyte were separated on DB-5MS capillary column and detected by EI ion source with MS/MS. The ions with m/z of 162 and 131 were selected as parent ion and daughter ion respectively for safrole, and the ion with m/z 104 was selected as quantitative ion for the internal standard of phenylethyl propionate. Linearity range for safrole was between 20-1 000 ng·g-1, with detection limit (3S/N) of 2.2 ng·g-1. Tests for recovery were performed by addition of standard of safrole at 3 concentration levels for 5 parallel determinations each, results of average recovery found were in the range of 71.1%-114.3% with RSD′s (n=5) in the range of 3.4%-16%.