1. .暨南大学理工学院
2. 广东出入境检验检疫局检验检疫技术中心
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余书奇, 奚星林, 陈文锐, 等. 手性柱分离气相色谱法测定辐照酒中2,3-丁二醇异构体[J]. 分析测试学报, 2012,31(7):877-880.
Determination of 2,3-Butanediol Isomers in Irradiated Liquor Using Chiral Capillary Column with Gas Chromatography[J]. 2012,31(7):877-880.
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 determination 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-BT 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 performed by the external standard method.The calibration curves of d-BT,l-BT and meso-BT were linear 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 RSDs(n=6)of 1.7%-3.8%,respectively.The detection limit was 1.0 mg/L.The method was applied in the determinations of d-BT,l-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.
23-丁二醇光学异构体酒气相色谱辐照
23-butanediolisomerswinegas chromatographyirradiation
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