摘要
目的确立水蒸汽蒸馏离子色谱法测定食品中亚硫酸盐含量的样品处理方法和测定条件。方法对样品采用水蒸气蒸馏的前处理方法,蒸出的二氧化硫收集在10%三乙醇胺溶液中,吸收液经过0.45μm的过滤膜后,用配有电导检测器的离子色谱仪测定,外标法定量。选用Metrosep A Supp10分离柱和5.0 mmol/L Na2CO3+5.0 mmol/L NaHCO3的淋洗液(添加2%的丙酮),流速0.8 ml/min,柱温40℃,进样体积100μl,亚硫酸根离子与硫酸根离子能很好地分离。结果在选定操作条件下,实验结果表明食品中SO32-的浓度在0.0μg/ml^6.0μg/ml范围内与其峰面积呈良好的线性关系,(r=0.9991);SO32-检出限为2.0 mg/kg;加标回收率为90.2%~105.4%,相对标准偏差在3.1%~6.8%之间。结论本方法具有快速、简便、准确度和精密度好的优点,适用于食品中亚硫酸盐浓度测定,用于实际样品的检测取得了较好的效果。
Objective To establish an ion chromatography method for the determination of sulfite content in food by steam dis- tillation. Methods The sample was extracted by means of steam distillation and absorbed by 10% triethanolamine solution through a 0.45 μm membrane and then analyzed by ion chromatography with electrical conductivity detector. The quantification was performed by external standard. The Metrosep A Supp 10 column was selected as the separation column, and 5.0 mmol/L Na2CO3 ＋5.0 mmol/L NaHCO3 with 2% acetone was used as mobile phase. The flow rate was set at 0.8 ml/min and the col- umn temperature was set at 40 ℃, sample volume was 100 μl, the sulfite ion was separated well. Results Under the regulated condition, the standard curves of sulfite content were linear in the concentration range of 0.0 μg/ml - 6.0 μg/ml with correla- tion coefficients of 0. 9991. The hmit of detection was 2.0 mg/kg, the recoveries ranged from 90.2% to 105.4% and relative standard deviations were from 3.1% to 6.8%. Conclusion The method is simple, rapid, accurate and reliable. It can be ap- plied to determine the sulfite content in food.
出处
《中国卫生检验杂志》
北大核心
2014年第4期483-485,共3页
Chinese Journal of Health Laboratory Technology
关键词
亚硫酸盐
水蒸气蒸馏
离子色谱
Suffite
Steam distillation
Ion chromatography
