葡萄酒中游离二氧化硫的比色法测定研究
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摘要
目的引入样品前处理方法,建立一个用甲醛吸收液-盐酸副玫瑰苯胺比色法测定葡萄酒中游离二氧化硫的方法。方法在一定温度和酸性条件下,通入空气,葡萄酒样品中的游离二氧化硫随空气进入吸收管被甲醛吸收液吸收后,生成稳定的羧甲基磺酸,在加入氢氧化钠后释放出二氧化硫,与盐酸副玫瑰苯胺反应生成红色化合物,比色定量。结果用本文的样品前处理方法对葡萄酒样品进行处理后,溶液中存在的颜色、还原性物质等均被除去,对测定结果无干扰。同时由于样品被浓缩,用本比色法测定游离二氧化硫含量还可以降低检出限。本法回收率为92. 5%～96. 8%,相对标准偏差为0. 5%～1. 81%。结论本文建立的样品前处理方法和比色法测定葡萄酒中游离二氧化硫含量,其测定结果准确度高、灵敏度高、精密度好、可靠且实用性强。
Objective To establish a colorimetry method for free sulfur dioxide determination in wine with reagents of formaldehyde absorption solution-pararosaniline hydrochloride and a new sample pretreatment procedure. Methods Free sulfur dioxide was generated along with atmosphere through air introduction. Then it entered an absorption tube,where it reacted with formaldehyde and a stable product of hydroxyl methanesulfonic acid was produced at the specified temperature and acidity.Sulfur dioxide was released with the addition of sodium hydroxide. A new compound with red color was obtained with the reaction between the released sulfur dioxide and pararosaniline hydrochloride,and then it was determined by colorimetry.Results Both the color and the reducing substances were eliminated with the pretreatment procedure proposed in this paper and the analytical results were no more interfered. Moreover,the detection limit for free sulfur dioxide was further decreased as the sample was concentrated in the pretreatment procedure. The recoveries ranged from 92. 5% to 96. 8% with the relative standard deviations( RSDs) of 0. 5%-1. 81%. Conclusion The established sample pretreatment and colorimetry procedure in determination of free sulfur dioxide in wine was of high accuracy,high sensitivity and good precision as well as excellent practicability.
Objective To establish a colorimetry method for free sulfur dioxide determination in wine with reagents of formaldehyde absorption solution-pararosaniline hydrochloride and a new sample pretreatment procedure. Methods Free sulfur dioxide was generated along with atmosphere through air introduction. Then it entered an absorption tube,where it reacted with formaldehyde and a stable product of hydroxyl methanesulfonic acid was produced at the specified temperature and acidity.Sulfur dioxide was released with the addition of sodium hydroxide. A new compound with red color was obtained with the reaction between the released sulfur dioxide and pararosaniline hydrochloride,and then it was determined by colorimetry.Results Both the color and the reducing substances were eliminated with the pretreatment procedure proposed in this paper and the analytical results were no more interfered. Moreover,the detection limit for free sulfur dioxide was further decreased as the sample was concentrated in the pretreatment procedure. The recoveries ranged from 92. 5% to 96. 8% with the relative standard deviations( RSDs) of 0. 5%-1. 81%. Conclusion The established sample pretreatment and colorimetry procedure in determination of free sulfur dioxide in wine was of high accuracy,high sensitivity and good precision as well as excellent practicability.
引文
[1]中华人民共和国国家卫生和计划生育委员会. GB 5009. 34—2016食品中二氧化硫测定[S].北京:中国标准出版社,2016.
[2]中华人民共和国国家质量监督检验检疫局总局. GB/T 15038—2006葡萄酒、果酒通用分析方法[S].北京.中国标准出版社. 2006.
[3]柳滢春,王锐银,巫敏玲,等.红葡萄酒中二氧化硫残留量测定方法的改进研究[J].安徽农业科学,2012,40(12):7407-7409.
[4]何龙凉,何宇玫.不同方法测定进口葡萄酒中二氧化硫残留量的比较[J].大众科技,2011,147(11):98-99.
[5]环境保护部. HJ 482—2009环境空气二氧化硫的测定甲醛吸收-副玫瑰苯胺分光光度法[S].北京:中国环境科学出版社,2009.
[6]中华人民共和国卫生部. GBZ/T 160. 33—2004工作场所空气中有毒物质测定硫化物[S].北京:中国标准出版社,2004.
[7]刘杰,叶运莉,汤艳,等.空气中二氧化硫测定方法的对比分析[J].泸州医学院学报2012,35(2):198-200.
[8]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.
[9]胡名志.论述葡萄酒中的二氧化硫[J].酿酒,2016,43(3):29-31.
[10]李堃,李建红,赵丹莹,等.离子色谱法测定葡萄酒中的二氧化硫[J].中国卫生检验杂志,2015,25(6):908-909,912.
[11]冯俊贤,李家栋,孙晓丽,等.电位间隔电位滴定法测定葡萄酒中游离二氧化硫[J].中国卫生检验杂志,2013,23(3):603-604.
[12]安文佳,李伟明,赵涛,等.盐酸副玫瑰苯胺法测定进口葡萄酒中二氧化硫的方法补充[J].食品研究与开发,2010,31(9):144-146.
[13]李小那.盐酸副玫瑰苯胺法测定葡萄酒中二氧化硫的方法探讨[J].酿酒,2012,39(2):76-78.
[14]中华人民共和国卫生部. 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,2008.
[15]陈露璐.二氧化硫在葡萄酒中的作用及常用检测方法的比较[J].食品安全导刊,2016(12):51.
[16]尚云青,唐若莹,俞捷,等.干红葡萄酒中二氧化硫测定方法的比较研究[J].食品工程,2013(1):41-43.
[2]中华人民共和国国家质量监督检验检疫局总局. GB/T 15038—2006葡萄酒、果酒通用分析方法[S].北京.中国标准出版社. 2006.
[3]柳滢春,王锐银,巫敏玲,等.红葡萄酒中二氧化硫残留量测定方法的改进研究[J].安徽农业科学,2012,40(12):7407-7409.
[4]何龙凉,何宇玫.不同方法测定进口葡萄酒中二氧化硫残留量的比较[J].大众科技,2011,147(11):98-99.
[5]环境保护部. HJ 482—2009环境空气二氧化硫的测定甲醛吸收-副玫瑰苯胺分光光度法[S].北京:中国环境科学出版社,2009.
[6]中华人民共和国卫生部. GBZ/T 160. 33—2004工作场所空气中有毒物质测定硫化物[S].北京:中国标准出版社,2004.
[7]刘杰,叶运莉,汤艳,等.空气中二氧化硫测定方法的对比分析[J].泸州医学院学报2012,35(2):198-200.
[8]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.
[9]胡名志.论述葡萄酒中的二氧化硫[J].酿酒,2016,43(3):29-31.
[10]李堃,李建红,赵丹莹,等.离子色谱法测定葡萄酒中的二氧化硫[J].中国卫生检验杂志,2015,25(6):908-909,912.
[11]冯俊贤,李家栋,孙晓丽,等.电位间隔电位滴定法测定葡萄酒中游离二氧化硫[J].中国卫生检验杂志,2013,23(3):603-604.
[12]安文佳,李伟明,赵涛,等.盐酸副玫瑰苯胺法测定进口葡萄酒中二氧化硫的方法补充[J].食品研究与开发,2010,31(9):144-146.
[13]李小那.盐酸副玫瑰苯胺法测定葡萄酒中二氧化硫的方法探讨[J].酿酒,2012,39(2):76-78.
[14]中华人民共和国卫生部. 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,2008.
[15]陈露璐.二氧化硫在葡萄酒中的作用及常用检测方法的比较[J].食品安全导刊,2016(12):51.
[16]尚云青,唐若莹,俞捷,等.干红葡萄酒中二氧化硫测定方法的比较研究[J].食品工程,2013(1):41-43.