手性柱分离气相色谱法测定辐照酒中2,3-丁二醇异构体  

Determination of 2,3-Butanediol Isomers in Irradiated Liquor Using Chiral Capillary Column with Gas Chromatography

作　　者：余书奇[1] 奚星林[2] 陈文锐[2] 晏日安[1] 邵仕萍[2] 潘丙珍[2] 庞世琦[2] 

机构地区：[1]暨南大学理工学院,广东广州510632 [2]广东出入境检验检疫局检验检疫技术中心,广东广州510623

出　　处：《分析测试学报》2012年第7期877-880,共4页Journal of Instrumental Analysis

基　　金：广东省科技计划项目(2010B020316006)

摘　　要：建立了直接测定辐照酒中2,3-丁二醇3种异构体:(2S,3S)-(+)-丁二醇(d-BT)、(2R,3R)-(-)-丁二醇(l-BT)以及meso-(R,S)-丁二醇(meso-BT)的手性柱分离气相色谱法。葡萄酒中的2,3-丁二醇采用乙酸乙酯和甲醇的混合溶液(4∶1)振荡提取,石墨化碳黑柱固相萃取净化提取液,经Varian CP-Chirasil-DEX CB手性毛细管柱分离后,以氢火焰检测器检测,外标法定量。d-BT、l-BT和meso-BT分别在10～75、60～300、20～100 mg/L范围内呈线性关系,相关系数分别为0.999 1、0.999 6和0.999 9。3种异构体在葡萄酒中的加标回收率为90%～113%,相对标准偏差(n=6)为1.1%～7.2%;在白酒中的加标回收率为96%～99%,相对标准偏差(n=6)为1.7%～3.8%;方法检出限为1.0 mg/L。将该方法用于白酒样品和葡萄酒样品辐照前后(剂量为10 kGy)d-BT、l-BT、meso-BT含量的测定。结果表明,白酒样品辐照后产生了d-BT,而葡萄酒则无此变化。这为鉴定白酒是否经过辐照提供了依据。A chiral capillary column with gas chromatographic method was developed for the determi- nation of three isomers of 2, 3-butanediol, e.g. （2S, 3S）-（ ＋ ）-butanediol （d-BT for short）, （2R, 3R）-（ - ）-butanediol（l-BT for short）and meso-（R, S）-butanediol（meso-ST for short）, in liquor sample. The samples were extracted via vibration with ethyl acetate and methanol （4 ： 1 ） mixed solution. The extract was purified with graphitization carbon black column using solid phase extraction device. The 2, 3-butanediol isomers were separated on a CP-Chirasil-DEX CB capillary column, and detected with flame ionization detector. The quantification of three isomers was per- formed by the external standard method. The calibration curves of d-BT, /-BT and meso-BT were lin- ear in the ranges of 10 -75, 60 -300, 20 -100 mg/L, respectively, with correlation coefficients of 0. 999 1, 0. 999 6 and 0. 999 9, respectively. The spiked recoveries of three butanediol isomers were 90% - 113% in wine with RSDs（n =6）of 1.1% -7.2% , and 96% -99% in spirit with RS- Ds（n =6）of 1.7% -3.8% , respectively. The detection limit was 1.0 mg/L. The method was ap- plied in the determinations of d-BT, I-BT and meso-BT in wine samples and sipirit samples before and after irradiated by Cobalt 60-gamma rays with irradiation dose of 10 kGy. The results showed that d- BT was detected in spirit samples after irradiation, but no obvious change of d-BT content occured in red wine, which could provide an evidence on whether the sipirit samples were irradiated or not.

关 键 词：2 3-丁二醇 光学异构体 酒 气相色谱 辐照 

分 类 号：O657.71[理学—分析化学] O622.3[理学—化学]