顶空-气相色谱-离子迁移谱联用技术快速鉴别沉香  

Rapid identification of agarwood by headspace-gas chromatography-ion mobility spectrometry

作　　者：曹雅静 刘亚雄[1] 黄国凯[1] 罗卓雅[1] Cao Yajing;Liu Yaxiong;Huang Guokai;Luo Zhuoya(Guangdong Institute for Drug Control,Guangzhou 510663,China)

机构地区：[1]广东省药品检验所,广州510663

出　　处：《化学分析计量》2021年第9期38-41,47,共5页Chemical Analysis And Meterage

基　　金：广东省科技厅科技计划项目(2021B1111610005,2018B020207008)。

摘　　要：建立顶空-气相色谱-离子迁移谱联用技术对沉香进行快速鉴别方法。以17批合格沉香和12批不合格沉香为样品,采用顶空进样方式,顶空温度为120℃,顶空时间为30 min,称样量为0.2 g,进样体积为0.5 mL。利用MXT-WAX强极性色谱柱进行一维分离,柱温为80℃,分离时间为25 min;利用离子迁移谱技术进行二维分离,迁移管温度为80℃,迁移气体流量为150 mL/min,获得沉香挥发性指纹图谱,并采用主成分分析法对合格沉香与不合格沉香进行区分。最终从沉香挥发物指纹图谱中提取获得3个特征峰,通过主成分分析显示合格沉香与不合格沉香区分总占比为90%,方法可行。该方法样品使用量少,无需样品前处理,可以快速有效对合格与不合格沉香进行准确鉴别。A method by headspace-gas chromatography-ion mobility spectrometry was established for rapid identification of agarwood.17 batches of qualified agarwood and 12 batches of unqualified agarwood were used as the materials.The headspace injection method was adopted.The headspace temperature was 120℃,the headspace time was 30 min,the sample weight was 0.2 g,and the injection volume was 0.5 mL.One-dimensional separation was carried out by a MXT-WAX strong polarity chromatographic column.The column temperature was 80℃and the separation time was 25 min;The two-dimensional separation was carried out by ion mobility spectrometry.The temperature of the migration tube was 80℃,and the flow rate of migration gas was 150 mL/min.The volatile fingerprint of agarwood was obtained,and the qualified and unqualified agarwood were distinguished by principal component analysis.Finally,three characteristic peaks were extracted from the volatile fingerprint of aloes.Principal component analysis showed that the total proportion of qualified and unqualified aloes was 90%,and the method was feasible.The method has the advantages of less sample consumption,and no sample pretreatment,and it can quickly and effectively identify qualified and unqualified agarwood.

关 键 词：顶空-气相色谱-离子迁移谱 沉香 挥发性特征峰 快速鉴别 

分 类 号：O657[理学—分析化学]