将全自动智能蒸馏仪与自动电位滴定仪相结合,建立了全自动蒸馏-电位滴定快速测定食品中二氧化硫残留量的方法。考察了蒸馏过程中馏出液体积、蒸馏功率、滴定过程中搅拌速率对二氧化硫含量测定结果的影响。采用该方法对橘子罐头、开心果、枸杞、葡萄酒、蜜饯凉果和果干等6种样品中的二氧化硫残留量进行检测分析,并采用F-test和t-test分析法对测定结果与国标法进行比对。结果表明,2种方法对橘子罐头、开心果和枸杞(二氧化硫含量＜20 mg/kg)的测定结果差异在可接受范围内(t0.05,10<t<t0.01,10),对葡萄酒、蜜饯凉果和果干(二氧化硫含量≥20 mg/kg)的测定结果无显著差异(t<t0.05,10)。另外考察了该方法对橘子罐头、开心果、葡萄酒和蜜饯凉果等4种样品加标回收试验,回收率为83.2%~99.1%,RSD(n=3)为5.7%~9.3%。该方法测定结果准确可靠,与国标相比具有批量操作、抗基质干扰能力强等优点。
An automatic distillation-potential titration method was established for the determination of sulfur dioxide residue in food by using an automatic intelligent distillation apparatus and a potentiometric titrator. Three critical factors, including distillate volume, distillation power and stirring rate, were studied and optimized for the determination of the sulfur dioxide residue of six different kinds of food samples. The results obtained from national standard method were compared using F-test and t-test. An acceptable difference (t0.05,10<t<t0.01,10) was observed in the determination of samples like canned orange, pistachios and medlar (SO2＜20 mg/kg), while no significant difference (t<t0.05,10) was observed in wine, candied fruit and dried fruit (SO2≥20 mg/kg). The recoveries levels obtained from canned orange, pistachios, wine and candied fruit ranged from 83.2% to 99.1%, with the precision (n=3) of 5.7%-9.3%. The established method is not only accurate and reliable but also has a good advantage of batch operation and strong ability of resistance to matrix interference comparing with the national standard method.
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