建立了香水中5种合成麝香的顶空固相微萃取-气相色谱-质谱联用分析方法.实验选用65μm的聚二甲基硅氧烷-二乙烯基苯(PDMS-DVB)萃取纤维,在磁力搅拌600 r/min条件下,考察了萃取温度、平衡时间、萃取时间、解吸时间、进样口温度和盐效应6个方面对实验结果的影响.优化后的条件为:10 mL顶空瓶中加入适量用水稀释过的样品,于60℃平衡3 min后,顶空萃取20 min,随即插入气相色谱进样口,于250℃解吸3 min进行定性、定量分析.5种合成麝香在0.05 ~ 1.00 μg/g范围内线性关系良好,检出限(LOD)为0.6~2.1 ng/g.空白样品在3个浓度加标水平下(0.05,0.50,1.00 μg/g)的回收率为82.0% ~ 103.3%,相对标准偏差(RSD)为1.8% ~9.4%.本方法简便、准确、快速、灵敏,适用于香水中合成麝香的分析检验工作.
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