同位素稀释-气相色谱-质谱法测定蜂蜜中甘露糖含量  

Determination of mannose in honey by isotope dilution gas chromatography mass spectrometry

作　　者：黄学者 纪欣欣 姜晓林 贾光群 曹彦忠 陈磊 徐锦忠 崔宗岩 HUANG Xuezhe;JI Xinxin;JIANG Xiaolin;JIA Guangqun;CAO Yanzhong;CHEN Lei;XU Jinzhong;CUI Zongyan(Technology Center of Qinhuangdao Customs,Qinhuangdao 066004,China;Chengde Customs,Chengde 067000,China;Animal,Plant and Food Inspection Center,Nanjing Customs,Nanjing 210019,China;Nanjing Zhongpu Biotechnology Co.Ltd.,Nanjing 210032,China)

机构地区：[1]秦皇岛海关技术中心,秦皇岛066004 [2]承德海关,承德067000 [3]南京海关动植物与食品检测中心,南京210019 [4]南京众谱生物科技有限公司,南京210032

出　　处：《分析试验室》2022年第9期1034-1040,共7页Chinese Journal of Analysis Laboratory

基　　金：海关总署科研项目(2019HK090)资助。

摘　　要：建立了一种同位素稀释-气相色谱/质谱(GC-MS)测定蜂蜜中甘露糖含量的方法。选择了一种新型化合物[13C;D]-D-甘露糖作为蜂蜜中甘露糖检测的同位素内标,优化了甘露糖及其内标的气相色谱分离条件和质谱参数。蜂蜜样品经70%乙醇水溶液溶解后加入同位素内标,采用两步衍生法对蜂蜜中糖组分进行衍生化,即先加入2.5%盐酸羟胺-吡啶溶液进行肟化衍生,再加入N,O-双(三甲基硅基)三氟乙酰胺(BSTFA)进行硅烷化衍生,采用GC-MS对甘露糖进行定性分析和定量检测。结果表明,以洋槐蜜、油菜蜜、荆条蜜和椴树蜜为代表性样品基质,甘露糖的检出限均为6 mg/kg,定量限为20 mg/kg,在20,40,200 mg/kg 3个添加水平下方法的平均回收率在66.1%~91.7%之间,相对标准偏差不超过20%。该方法适用于不同类型蜂蜜中甘露糖含量的测定。A method for the determination of mannose in honey by isotope dilution gas chromatography-mass spectrometry(GC-MS)was established,using[13C;D]-D-mannose as the isotope internal standard.The gas chromatographic separation conditions and mass spectrometric parameters of mannose and its internal standard were optimized.After the honey sample was dissolved in 70%ethanol aqueous solution,the isotope internal standard was spiked.The sugar components in honey were derivatized by two-step derivatization method.Firstly,2.5%hydroxylamine hydrochloride pyridine solution was added for oximation derivatization,and then N,O-bis(trimethylsilyl)trifluoroacetamide(BSTFA)was added for silylation derivatization.Finally,in the representative acacia honey,rape honey,vitex honey,and linden honey,mannose was qualitatively and quantitatively detected by GC-MS.The results showed that the detection limit of mannose was 6 mg/kg,and the limit of quantification was 20 mg/kg.The average recoveries of mannose were 66.1%-91.7%at the spiked levels of 20,40 and 200 mg/kg,and the relative standard deviation was less than 20%.The method is applicable for the determination of mannose in different types of honey.

关 键 词：蜂蜜 甘露糖 同位素稀释 气相色谱-质谱 

分 类 号：S896.1[农业科学—特种经济动物饲养]