芝麻香白酒中3-甲硫基丙醇的GC-FPD分析
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(1.北京工商大学 北京市食品风味化学重点实验室, 北京 100048;2.北京工商大学 食品质量与安全北京实验室, 北京 100048;3.山东扳倒井集团 技术中心, 山东 高青 256300)

作者简介:

孙啸涛,男,实验师,主要从事白酒分析方面的研究; *孙宝国,男,教授,主要从事食品风味方面的研究. 通讯作者.

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基金项目:

国家自然科学基金青年科学基金项目(31301466);北京市教委科技计划重点项目(KZ201410011015). 


GC-FPD Analysis of 3-Methylthiopropanol in Sesame-Flavor Liquor
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(1.Beijing Key Laboratory of Flavor Chemistry, Beijing Technology and Business University, Beijing 100048,China;2.Beijing Laboratory for Food Quality and Safety, Beijing Technology and Business University, Beijing 100048,China;3.Technical Center of Bandaojing Co. Ltd., Gaoqing 256300,China)

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    摘要:

    建立了利用气相色谱-火焰光度检测器检测芝麻香白酒风味成分3-甲硫基丙醇的方法. 样品前处理方法为CH2Cl2萃取,酒样浓缩50倍分析;色谱方法为DB-FFAP(60m×0.25mm×0.25μm)毛细管柱,程序升温,进样口温度为260℃,检测器温度为200℃;采用外标法定量. 结果表明:在3-甲硫基丙醇质量浓度为5~100mg/L时,线性相关系数为0.9913,检测限为2.5mg/L,定量限为5mg/L. 在3-甲硫基丙醇质量浓度为8,30,80mg/L 3个水平下,回收率为84.3%~89.7%,相对标准偏差为3.7%~4.6%. 对国内5家芝麻香型白酒骨干生产企业共18个酒样的3-甲硫基丙醇经换算后的检测结果是:企业Ⅰ原酒及商品酒中均未检出3-甲硫基丙醇;企业Ⅱ原酒中未检出3-甲硫基丙醇,商品酒Ⅱ-a、Ⅱ-b、Ⅱ-c和Ⅱ-d中3-甲硫基丙醇质量浓度分别为1.03,0.35,0.80,0.67mg/L;企业Ⅲ原酒及商品酒中均未检出3-甲硫基丙醇;企业Ⅳ原酒及商品酒中3-甲硫基丙醇质量浓度低于0.1mg/L;企业V原酒中未检出3-甲硫基丙醇,商品酒Ⅴ-a中3-甲硫基丙醇质量浓度为0.18mg/L.

    Abstract:

    methylthiopropanol in Sesame-Flavor Liquor was analyzed by gas chromatography-flame photometric detector (GC-FPD) in this study. The wine was concentrated 50 times and extracted by dichloromethane for sample pretreatment. The chromatographic condition carried out that:polar chromatogra-phic column DB-FFAP (60m×0.25mm×0.25μm), programmed temperature, inlet temperature 260℃, detector temperature 200℃. External standardmethod was adopted. The results showed that with the concentration of 5-100mg/L of 3-methylthiopropanol the linear correlation coefficient( R2 ) was 0.9913, LOD was 2.5mg/L, LOQ was 5mg/L, while with the level of 8,30,80mg/L recovery rates were between 84.3% to 89.7%, R.S.D. ranged from 3.7% to 4.6%. Five major Sesame Flavor Liquor corporations and 18 samples were inspected. The 3-methylthiopropanol couldn't be detected in commercial wines including the corporation of Ⅰ and Ⅲ, original wines such as Ⅰ, Ⅱ, Ⅲ and Ⅴ. While the concentration of 3-methylthiopropanol in the commercial wines of Ⅱ-a, Ⅱ-b, Ⅱ-c, Ⅱ-d and Ⅴ-a were 1.03,0.35,0.80,0.67,0.18mg/L, respectively. In the corporation of Ⅳ original wine and commercial wine, its concentration were all below 0.1mg/L.

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孙啸涛,张锋国,董蔚,孙金沅,孙宝国.芝麻香白酒中3-甲硫基丙醇的GC-FPD分析[J].食品科学技术学报,2014,32(5):27-34.

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  • 收稿日期:2014-08-25
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  • 在线发布日期: 2014-11-06
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