优化建立了固相微萃取-气相色谱-质谱联用技术(HS-SPME-GC/MS)检测酱油中氨基甲酸乙酯含量的方法。取5 mL样品,调节pH值为7.5,70℃水浴,搅拌速率800 r/min,平衡时间10 min,采用75μm CAR/PDMS萃取纤维头,萃取时间30 min,气相进样解吸10 min。在此条件下,方法检出限(S/N=3)为1.0μg/L,酱油中氨基甲酸乙酯的回收率在70.56%~129.21%,检测结果的日内RSD为3.69%,日间RSD为8.50%。所建立方法可快速、准确地检测酱油中氨基甲酸乙酯含量。

A method of headspace solid-phase micro-extraction combined gas chromatography–tandem mass spectrometry was developed and applied to the determination of ethyl carbamate in soy sauce.75 μm CAR/PDMS fiber was chosen for extracting the ethyl carbamate from the soy sauce.After 5mL of soy sauce(adjusted to pH 7.5) equilibrated 10 min at 70 ℃ under 800 r/min,the CAR/PDMS fiber was inserted into the vial for 30 min then injected into GC-MS for 10 min.Under the extraction conditions,the limit of detection was 1.0 μg/mL.The recoveries of ethyl carbamate in soy sauce were 70.56 %~129.21 %.The precisions(RSD) were 3.69 %(intraday) and 8.50 %(inter day).The HS-SPME/GC/MS technique is suitable for the fast,reliable and inexpensive determination of ethyl carbamate in soy sauce.