半微量碘量法测定葡萄酒中总二氧化硫含量
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摘要
对葡萄酒中SO_2残留量的直接碘量法测定进行了半微量化改进研究。通过减小取样体积,减弱了有色葡萄酒中色素对滴定终点判断的影响;通过超声振荡加速结合态SO_2的解离,缩短了分析时间;通过加碎冰控制反应温度改进为冰水浴控制,避免了稀释作用对反应的不良影响。经过方法学验证,该方法的精密度良好,相对标准偏差小于1%,准确度较高,回收率在95.0%～100.7%;方法的适用性强,可以测定不同类型葡萄酒中SO_2的含量。使用改进后的方法对四大类别12个品牌的葡萄酒中SO_2残留量进行了检测,结果均低于国家最高限量标准。
This study aimed to use semi-micro iodometric analysis to determine total sulfur dioxide in red grape wine. By reducing the sampling volume, influences of pigments in colored wine at titration end points were weakened. Dissociation of bound sulfur dioxide was accelerated by ultrasonic oscillation, leading to shorter analysis time. Ice water bath was used to control the reaction temperature to avoid adverse effects of dilution on the reaction. Methodological verification showed that the improved method had good precision and high accuracy, and its relative standard deviation was less than 1%. Besides, its recovery rate reached 95.0%-100.7%. The method was highly adaptable for determining sulfur dioxide in different types of wine. The residual sulfur dioxide in 12 brands of wine from four categories were determined, and the results showed that they were all qualified referring to the national standard.
This study aimed to use semi-micro iodometric analysis to determine total sulfur dioxide in red grape wine. By reducing the sampling volume, influences of pigments in colored wine at titration end points were weakened. Dissociation of bound sulfur dioxide was accelerated by ultrasonic oscillation, leading to shorter analysis time. Ice water bath was used to control the reaction temperature to avoid adverse effects of dilution on the reaction. Methodological verification showed that the improved method had good precision and high accuracy, and its relative standard deviation was less than 1%. Besides, its recovery rate reached 95.0%-100.7%. The method was highly adaptable for determining sulfur dioxide in different types of wine. The residual sulfur dioxide in 12 brands of wine from four categories were determined, and the results showed that they were all qualified referring to the national standard.
引文
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[2] 胡名志.论述葡萄酒中的二氧化硫[J].酿酒,2016,43(3):29-31.
[3] 胡桂仙,赖爱萍,袁玉伟,等.消费者膳食中二氧化硫残留量的累积性风险评估[J].中国农业科学,2017,50(7):1 317-1 325.
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[6] THANH N T K,DECNOP W L G,KOK W T.Determination of sulphite in wine by flow in jection analysis with indirect electrochemical detection[J].Fresenius J Anal Chem,1994,349:469-472.
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[8] 卫峰,陈明生,于玲,等.高效液相色谱_荧光检测法测定葡萄酒中总亚硫酸盐[J].色谱,1999,17(6):583-585.
[9] 陈梅兰,范云场,叶明立,等.离子色谱柱后衍生光度法检测食品中含硫的阴离子化合物[J].中国科学:B辑:化学,2009,39(8):819-824.
[10] KOCH M,KO O,PPEN R,et al.Determination of total sulfite in wine by ion chromatography after in-sample oxidation[J].J Agric Food Chem,2010,58(17):9 463-9 467.
[11] 中华人民共和国卫生部中国国家标准化管理委员会.GB/T 5009.49—2008,发酵酒及其配制酒卫生标准的分析方法[S].北京:中国标准出版社,2010.
[12] 中华人民共和国国家卫生和计划生育委员会.GB 5009.34— 2016,食品安全国家标准食品中二氧化硫的测定[S].北京:中国标准出版社,2017.
[13] 中国轻工业联合会.葡萄酒、果酒通用分析方法:GB/T15038—2006[S].北京:中国标准出版社,2008.
[14] 逄晓薇,孙辉,武锋,等.两种葡萄酒中二氧化硫检测方法研究[J].酿酒科技,2018,6:91-94,99.
[15] 梁宏,林燕奎,王丙涛,等.葡萄酒中二氧化硫的几种检测方法对比[J].食品科学,2012,33(4):178-181.
[16] 韩璐.半微量滴定分析实验的可行性研究[J].化工时刊,2017,31(3):25-27
[17] 陈晓红.碘量法测定葡萄糖含量微型化实验研究[J].光谱实验室,2006,23(6):1 265-1 266.
[18] 王华.葡萄酒分析检验[M].北京:中国农业出版社,2011:160-161.
[2] 胡名志.论述葡萄酒中的二氧化硫[J].酿酒,2016,43(3):29-31.
[3] 胡桂仙,赖爱萍,袁玉伟,等.消费者膳食中二氧化硫残留量的累积性风险评估[J].中国农业科学,2017,50(7):1 317-1 325.
[4] 中华人民共和国国家卫生和计划生育委员会.GB2760—2014,食品安全国家标准食品添加剂使用标准[S].北京:中国标准出版社,2016.
[5] 林军,胡群,叶敏芳,等.葡萄酒中SO2残留量电位滴定检测方法的探讨[J].食品科学,2008,29(3):380-382.
[6] THANH N T K,DECNOP W L G,KOK W T.Determination of sulphite in wine by flow in jection analysis with indirect electrochemical detection[J].Fresenius J Anal Chem,1994,349:469-472.
[7] 何吉子,潘丙珍,陈秀明,等.连续流动分析法测定葡萄酒中的总二氧化硫[J].现代测量与实验室管理,2015,5:10-12.
[8] 卫峰,陈明生,于玲,等.高效液相色谱_荧光检测法测定葡萄酒中总亚硫酸盐[J].色谱,1999,17(6):583-585.
[9] 陈梅兰,范云场,叶明立,等.离子色谱柱后衍生光度法检测食品中含硫的阴离子化合物[J].中国科学:B辑:化学,2009,39(8):819-824.
[10] KOCH M,KO O,PPEN R,et al.Determination of total sulfite in wine by ion chromatography after in-sample oxidation[J].J Agric Food Chem,2010,58(17):9 463-9 467.
[11] 中华人民共和国卫生部中国国家标准化管理委员会.GB/T 5009.49—2008,发酵酒及其配制酒卫生标准的分析方法[S].北京:中国标准出版社,2010.
[12] 中华人民共和国国家卫生和计划生育委员会.GB 5009.34— 2016,食品安全国家标准食品中二氧化硫的测定[S].北京:中国标准出版社,2017.
[13] 中国轻工业联合会.葡萄酒、果酒通用分析方法:GB/T15038—2006[S].北京:中国标准出版社,2008.
[14] 逄晓薇,孙辉,武锋,等.两种葡萄酒中二氧化硫检测方法研究[J].酿酒科技,2018,6:91-94,99.
[15] 梁宏,林燕奎,王丙涛,等.葡萄酒中二氧化硫的几种检测方法对比[J].食品科学,2012,33(4):178-181.
[16] 韩璐.半微量滴定分析实验的可行性研究[J].化工时刊,2017,31(3):25-27
[17] 陈晓红.碘量法测定葡萄糖含量微型化实验研究[J].光谱实验室,2006,23(6):1 265-1 266.
[18] 王华.葡萄酒分析检验[M].北京:中国农业出版社,2011:160-161.