在线蒸馏-流动注射法测定食糖中的二氧化硫
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摘要
目的建立在线蒸馏-流动注射法测定食糖中二氧化硫含量的分析方法。方法采用全自动流动注射分析仪测定食糖中的二氧化硫,对硫酸溶液浓度和反应温度进行优化,并与国家标准测定方法进行比较。结果在最佳条件下,方法在0.5~10 mg/L的质量浓度范围内具有良好线性(r=0.9994),方法的检出限为5.0 mg/kg,精密度实验的相对标准偏差(relative standard deviation,RSD)为1.43%~2.01%,平均回收率为93.2%~102.6%。结果证明该方法比国标蒸馏法灵敏度更高。结论该方法具有灵敏度高、重复性好等优点,以自动的在线蒸馏代替了较为繁琐的传统蒸馏方式,检测过程易操作,实现自动化,提高了检测效率,适用于食糖中二氧化硫的测定。
Objective To establish a method for the determination of sulfur dioxide in sugar by online distillation-flow injection analysis. Method The content of sulfur dioxide in sugar was determined by automatic flow injection analyzer. The sulfuric acid concentration and reaction temperature were optimized and compared with the national standard method. Results Under the optimum conditions, the method had a good linearity(r=0.9994) in the concentration range of 0.5-10 mg/L and the limit of detection was 5.0 mg/kg. The precision test relative standard deviation(RSD) was 1.43%-2.01% and the average recovery rate was 93.2%-102.6%. The result showed that the sensitivity of this method was better than the national standard distillation. Conclusion This method has good sensitivity and repeatability. In addition, the online distillation-flow injection analysis takes place of tedious traditional distillation method and the detection process is easy to operate with automation, which can improve the detection efficiency and is suitable for the detection of sulfur dioxide in sugar.
Objective To establish a method for the determination of sulfur dioxide in sugar by online distillation-flow injection analysis. Method The content of sulfur dioxide in sugar was determined by automatic flow injection analyzer. The sulfuric acid concentration and reaction temperature were optimized and compared with the national standard method. Results Under the optimum conditions, the method had a good linearity(r=0.9994) in the concentration range of 0.5-10 mg/L and the limit of detection was 5.0 mg/kg. The precision test relative standard deviation(RSD) was 1.43%-2.01% and the average recovery rate was 93.2%-102.6%. The result showed that the sensitivity of this method was better than the national standard distillation. Conclusion This method has good sensitivity and repeatability. In addition, the online distillation-flow injection analysis takes place of tedious traditional distillation method and the detection process is easy to operate with automation, which can improve the detection efficiency and is suitable for the detection of sulfur dioxide in sugar.
引文
[1]马凯,朱亚伟,徐雪.2017-2026年中国食糖市场形势展望[J].世界农业,2017,(8):147-151.Ma K,Zhu YW,Xu X.The prospect of the sugar market in China from2017 to 2026[J].World Agric,2017,(8):147-151.
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[3]霍汉镇.白糖残留二氧化硫问题[J].广西蔗糖,2004,(4):31-33.Huo HZ.The problem of sulfur dioxide residue in white sugar[J].Guangxi Sugar Canes,2004,(4):31-33.
[4]GB 2760-2014食品安全国家标准食品添加剂使用标准[S].GB 2760-2014 National food safety standard-Standard for the use of food additives[S].
[5]GB/T 317-2006白砂糖[S].GB/T 317-2006 White granulated sugar[S].
[6]GB/T 1445-2000绵白糖[S].GB/T 1445-2000 White soft sugar[S].
[7]QB/T 1174-2002(2017)多晶体冰糖[S].QB/T 1174-2002(2017)Multicrystal rock sugar[S].
[8]QB/T 1173-2002(2017)单晶体冰糖[S].QB/T 1173-2002(2017)Monocrystal rock sugar[S].
[9]QB/T 2343.1-1997赤砂糖[S].QB/T 2343.1-1997 Brown granulated sugar[S].
[10]李芳.食品中二氧化硫的危害及检测方法[J].职业与健康,2009,25(3):315-316.Li F.Hazard and detection method of sulfur dioxide in food[J].Occup Health,2009,25(3):315-316.
[11]尹洁,朱军莉,励建荣.食品中二氧化硫的来源与检测方法[J].食品科技,2009,34(11):292-296.Yin J,Zhu JL,Li JR.Origin and determination method of sulfur dioxide in foods[J].Food Sci Technol,2009,34(11):292-296.
[12]杨丽.食品中二氧化硫的来源、危害及国标中检测方法综述[J].中外食品工业月刊,2014,(3):42-43.Yang L.Summary of the sources,hazards and the detection methods in national standard of sulfur dioxide in food[J].Glob Food Ind,2014,(3):42-43.
[13]李翠萍.食糖产品中二氧化硫残留量测定方法影响因素的探讨[J].广东化工,2015,42(14):220-221.Li CP.Discussion on factors affecting the determination of sulfur dioxide in sugar[J].Guangdong Chem Ind,2015,42(14):220-221.
[14]GB 5009.34-2016食品安全国家标准食品中二氧化硫的测定[S].GB 5009.34-2016 National food safety standard–Determination of sulfur dioxide in food[S].
[15]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.He JZ,Pan BZ,Chen XM,et al.Determination of total sulfur dioxide in wine by continuous flow analysis[J].Adv Meas Lab Manage,2015,(5):10-12.
[16]Silva KR,Jr RI,Gimenez IF,et al.Optical sensor for sulfur dioxide determination in wines[J].J Agric Food Chem,2006,54(23):8697-8701.
[17]Mataix E,Luque DCMD.Determination of total and free sulfur dioxide in wine by pervaporation-flow injection[J].Analyst,1998,123(7):1547-1549.
[18]邢朝宏,曹扬,薛峰,等.流动注射仪测定化妆品中无机亚硫酸盐类和亚硫酸氢盐类的方法研究[J].香料香精化妆品,2017,(2):40-43.Xing CH,Cao Y,Xue F,et al.Research on determination of inorganic sulfites and bisulfites in cosmetics by flow injection analysis[J].Flavour Frag Cosmet,2017,(2):40-43.
[2]谢彩锋,马英群,丁慧敏,等.一种甘蔗混合汁无硫二步澄清工艺优化研究[J].食品工业,2016,37(7):63-67.Xie CF,Ma YQ,Ding HM,et al.Optimization of a two-step sulfur-free clarification process of sugarcane mixed juice[J].Food Ind,2016,37(7):63-67.
[3]霍汉镇.白糖残留二氧化硫问题[J].广西蔗糖,2004,(4):31-33.Huo HZ.The problem of sulfur dioxide residue in white sugar[J].Guangxi Sugar Canes,2004,(4):31-33.
[4]GB 2760-2014食品安全国家标准食品添加剂使用标准[S].GB 2760-2014 National food safety standard-Standard for the use of food additives[S].
[5]GB/T 317-2006白砂糖[S].GB/T 317-2006 White granulated sugar[S].
[6]GB/T 1445-2000绵白糖[S].GB/T 1445-2000 White soft sugar[S].
[7]QB/T 1174-2002(2017)多晶体冰糖[S].QB/T 1174-2002(2017)Multicrystal rock sugar[S].
[8]QB/T 1173-2002(2017)单晶体冰糖[S].QB/T 1173-2002(2017)Monocrystal rock sugar[S].
[9]QB/T 2343.1-1997赤砂糖[S].QB/T 2343.1-1997 Brown granulated sugar[S].
[10]李芳.食品中二氧化硫的危害及检测方法[J].职业与健康,2009,25(3):315-316.Li F.Hazard and detection method of sulfur dioxide in food[J].Occup Health,2009,25(3):315-316.
[11]尹洁,朱军莉,励建荣.食品中二氧化硫的来源与检测方法[J].食品科技,2009,34(11):292-296.Yin J,Zhu JL,Li JR.Origin and determination method of sulfur dioxide in foods[J].Food Sci Technol,2009,34(11):292-296.
[12]杨丽.食品中二氧化硫的来源、危害及国标中检测方法综述[J].中外食品工业月刊,2014,(3):42-43.Yang L.Summary of the sources,hazards and the detection methods in national standard of sulfur dioxide in food[J].Glob Food Ind,2014,(3):42-43.
[13]李翠萍.食糖产品中二氧化硫残留量测定方法影响因素的探讨[J].广东化工,2015,42(14):220-221.Li CP.Discussion on factors affecting the determination of sulfur dioxide in sugar[J].Guangdong Chem Ind,2015,42(14):220-221.
[14]GB 5009.34-2016食品安全国家标准食品中二氧化硫的测定[S].GB 5009.34-2016 National food safety standard–Determination of sulfur dioxide in food[S].
[15]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.He JZ,Pan BZ,Chen XM,et al.Determination of total sulfur dioxide in wine by continuous flow analysis[J].Adv Meas Lab Manage,2015,(5):10-12.
[16]Silva KR,Jr RI,Gimenez IF,et al.Optical sensor for sulfur dioxide determination in wines[J].J Agric Food Chem,2006,54(23):8697-8701.
[17]Mataix E,Luque DCMD.Determination of total and free sulfur dioxide in wine by pervaporation-flow injection[J].Analyst,1998,123(7):1547-1549.
[18]邢朝宏,曹扬,薛峰,等.流动注射仪测定化妆品中无机亚硫酸盐类和亚硫酸氢盐类的方法研究[J].香料香精化妆品,2017,(2):40-43.Xing CH,Cao Y,Xue F,et al.Research on determination of inorganic sulfites and bisulfites in cosmetics by flow injection analysis[J].Flavour Frag Cosmet,2017,(2):40-43.