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手性柱分离气相色谱法测定辐照酒中2,3-丁二醇异构体

     

摘要

A chiral capillary column with gas chromatographic method was developed for the determi-nation of three isomers of 2, 3-butanediol, e. g. (25, 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 per-formed by the external standard method. The calibration curves of d-BT, Z-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% -1.2% , 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, /-BT and meso-BT in wine samples and si pint 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.%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、0.9996和0.9999.3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.

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