GC和GC-MS法测定饮料中香兰素和乙基香兰素含量

本文建立了一种气相色谱（GC）和气相色谱-质谱（GC-MS）法测定饮料中香兰素和乙基香兰素含量的方法。无色样品经乙醚萃取、离心、取上清液浓缩定容经0.22μm有机相滤膜净化进样,有颜色样品经乙醚萃取、离心、取乙醚上清液浓缩至近干,丙酮溶解混匀,过石墨化碳黑柱净化,浓缩定容,分别进GC-FID和GC-MS测定及确证,外标法定量。GC法测定香兰素和乙基香兰素的添加回收率范围为80%¹05%,相对标准偏差（RSD）小于6.0%。GC-MS法测定香兰素和乙基香兰素的添加回收率范围为81%¹10%,相对标准偏差（RSD）小于6.0%。该方法中GC仪器操作简单、成本较低,可广泛应用于饮料中香兰素和乙基香兰素日常检测,GC-MS法采用选择离子扫描（SIM）排除GC法测定的假阳性结果,使测定结果更准确可靠,两种方法互补使用,适合饮料中香兰素和乙基香兰素的日常分析检测和质量控制。 

Determination of vanillin and ethyl vanillin contents in beverages by GC and GC- MS

A method for determination of vanillin and ethyl vanillin in beverages by gas chromatography( GC) and gas chromatography- mass spectrometry( GC- MS) was established.If samples were colorless,firstly extracted by ether,centrifuged and then the supernatant fluid were purified by 0.22 μm organic phase membrane and quantified by GC and GC- MS. If samples were color,firstly extracted by ether,centrifuged and then the supernatant fluid were collected and enrichment to nearly dry,then dissolved by acetone,purified and concentrated by Carbon-GCB.Finally,they were quantified and certified by GC and GC- MS,using external standard. The recoveries of vanillin and ethyl vanillin by the GC method and GC- MS method ranged from 80% to 105% and from 81% to 110%respectively,as well as RSD was less than 6.0%.GC instrument was operated simply and that the cost of operation was relatively low,so it can be widely used in vanillin and ethyl vanillin daily testing in beverages.GC- MS method using selected ion scan( SIM) to rule out false positives sample which was tested by GC method and made the results more accurate and reliable.The two methods were complement each other,which were suitable for the daily determination and quality control of vanillin and ethyl vanillin contents in beverages.