气相色谱-质谱法测定软木塞中2种霉味物质

建立了一种简便、快速的可同时测定软木塞中两种霉味物质(2,4,6-三氯苯甲醚(TCA)和2,4,6-三溴苯甲醚(TBA))的气相色谱-质谱联用(GC-MS)方法。软木塞样品采用甲醇超声萃取,N-丙基乙二胺(PSA)固相萃取柱净化,浓缩后采用GC-MS进行分析,外标法定量。在10～10000 μg/L的质量浓度范围内,TCA和TBA均有较好的线性关系,相关系数(r2)大于0.99。通过对不同种类的软木塞空白样品进行加标回收率试验和精密度试验考察方法的可行性。结果表明TCA和TBA的回收率介于88.4%与97.6%之间,相对标准偏差介于1.02%与4.58%之间。TCA和TBA的检出限分别为12 μg/L和18 μg/L,定量限分别为40 μg/L和50 μg/L。本方法适用于市售瓶装葡萄酒软木塞中TCA和TBA的检测。

Determination of two mouldy compounds in cork by gas chromatography-mass spectrometry

A simple and fast method for the simultaneous determination of two mouldy compounds,2,4,6-trichloroanisole(TCA) and 2,4,6-tribromoanisole(TBA),in cork by gas chromatography-mass spectrometry(GC-MS) was established.The analytes were extracted by ultrasonic extraction with methanol,and purified then by solid phase extraction using primary secondary amine(PSA) as solid phase.After concentrating,the sample was analyzed by GC-MS and quantified by the external standard method.The linear ranges were from 10 μg/L to 10 000 μg/L for TCA and TBA,the correlation coefficients(r2) of the calibration curves were above 0.99.The recoveries and the relative standard deviations(RSDs) of TCA and TBA in different kinds of corks were investigated.The recoveries ranged from 88.4% to 97.6% with the RSDs between 1.02% and 4.58%(n=6).The limits of detection(LODs) were 12 μg/L for TCA and 18 μg/L for TBA,and the limits of quantification(LOQs) were 40 μg/L for TCA and 50 μg/L for TBA.The method is suitable to the determination of TCA and TBA in corks.