为了有效地检测和监测葡萄酒中的木塞污染物,更好把控葡萄酒的品质,建立了自动顶空-固相微萃取-气相色谱三重四级杆质谱(Automatic headspace-solid phase microextraction combined with gas chromatography-triple quadrupole mass spectrometry,Auto-HS-SPME-GC-MS/MS)检测葡萄酒中9种卤代苯甲醚和卤代苯酚类木塞污染物的方法.实验中,卤代苯酚类化合物与乙酸酐发生在线衍生化反应得到乙酰化产物,卤代苯甲醚和卤代苯酚乙酰化产物再通过HS-SPME浓缩富集后经GC-MS/MS检测,同位素内标法定量.通过优化自动固相微萃取的实验条件,对葡萄酒和起泡酒的样品进行了测定.结果表明,方法线性范围为3～300 ng/L,相关系数R2为0.9988～0.9999,线性关系良好.方法检出限为1 ng/L,9种目标物加标回收率在63.7％～118.4％之间,具有较好的准确度;相对标准偏差为2.0％～16.4％,说明实验方法及仪器具有良好的精密度.该方法自动化程度高且可靠稳定,适用于葡萄酒中卤代苯甲醚、卤代苯酚类化合物的痕量检测.
Determination of Nine Kinds of Cork Pollutants in Wine Based on Automatic Headspace-Solid Phase Microextraction Combined With Gas Chromatography-Mass Spectrometry
In order to effectively detect and monitor cork pollutants in wine,and better control of wine quality,a method was established using automatic headspace-solid phase microextraction coupled with gas chromatography-triple quadrupole mass spectrometry(HS-SPME-GC-MS/MS)to detect nine halogenated anisole and halogenated phenol cork taint compounds in wine.Halogenated phenol compounds were derivated with acetic anhydride to obtain acetylated products.The acetylated products of halogenated anisole and halogenated phenol were concentrated and enriched by HS-SPME,and then detected by GC-MS/MS,and quantified by isotope internal standard method.During the experiment,wine and sparkling wine samples were tested by optimizing the experimental conditions of automatic solid-phase microextraction.The results showed that the method had a linear range of 3 ng/L to 300 ng/L,with correlation coefficients(R2)ranging from 0.9988 to 0.9999,indicating a good linear relationship.The detection limit of the method was 1 ng/L,with recoveries of the nine target compounds ranging from 63.7％to 118.4％,demonstrating good accuracy.The relative standard deviation(RSD)values were between 2.0％and 16.14％,indicating that the method and instrumentation provide good precision.The method has high automation,reliability and stability,and is suitable for trace determination of halogenated anisole and halogenated phenol compounds in wine.
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