不同检测方法测定食品中二氧化硫残留量的比较研究

Comparative study on determination of sulfur dioxide residues in food by different detection methods

中文关键词:  二氧化硫残留量  食品  碘量法  酸碱滴定法  离子色谱法  盐酸副玫瑰苯胺比色法  间断化学分析法  方法比较研究

英文关键词:residual amount of sulfur dioxide  iodimetry  acid-base titration  ion chromatography  pararosaniline hydrochloride colorimetry  intermittent chemical analysis  comparative study of methods

中文摘要:

      目的 比较不同检测方法测定食品中二氧化硫残留量的一致性和差异性。方法 本研究比较了碘量法、酸碱滴定法、离子色谱法、盐酸副玫瑰苯胺比色法和间断化学分析法5种检测方法测定食品中二氧化硫残留量的适用性、检出限、准确性, 并采用5种检测方法测定市售食品样品。结果 5种检测方法的检出限、定量限均不高于GB 2760—2014《食品安全国家标准 食品添加剂使用标准》中规定的限量要求, 且加标回收率和精密度均满足GB 5009.295—2023《食品安全国家标准 化学分析方法验证通则》要求。其中,对于固体和半流体样品而言, 盐酸副玫瑰苯胺比色法、离子色谱法和间断化学分析法的定量限低于人工蒸馏滴定方法。5种测定方法的准确度均能满足质控要求。但是离子色谱法和间断化学分析法的检测结果更接近质控样品的参考值。碘量法和酸碱滴定法不适用于八角等香辛料和香菇等食用菌中二氧化硫残留量的测定。配料中含有冰乙酸、乳酸、脱氢乙酸等有机酸添加剂的食品不适合采用酸碱滴定法测定其中的二氧化硫残留量。盐酸副玫瑰苯胺比色法自动程度低, 分析速度慢, 检测精度及准确度受人为因素影响大, 且所使用的浸提液四氯汞钠毒性较大, 对人体安全和环境影响较大, 建议尽量避免使用。间断化学分析法和离子色谱相比其他方法, 具有较高灵敏度, 且自动化水平高, 适用于大批量食品样品中二氧化硫残留量分析检测。结论 在实际检测中应根据样品类别及检测的实际情况选择合适的检测方法, 以减少方法差异引起判定错误。

英文摘要:

      Objective To compare the consistency and difference of different detection methods for the determination of sulfur dioxide residue in food. Methods In this study, the applicability, detection limits and accuracy of 5 kinds of detection methods including iodimetry, acid-base titration, ion chromatography, pararosaniline hydrochloride colorimetry and intermittent chemical analysis were compared for the determination of sulfur dioxide residues in food, and 5 kinds of detection methods were used to determine food samples. Results The limits of detection and limits of quantitative of 5 kinds of detection methods were not higher than the limit requirements specified in GB 2760—2014 National food safety standard-Food additive usage standard, and the recovery rates and precisions of the standard were all in line with the requirements of GB 5009.295—2023 National food safety standard-General rules for verification of chemical analysis methods. For solid and semi-fluid samples, the limits of quantitation of pararosaniline hydrochloride colorimetry, ion chromatography and intermittent chemical analysis were lower than those of manual distillation titration. The accuracy of 5 kinds of methods could meet the quality control requirements. However, the detection results of ion chromatography and intermittent chemical analysis were closer to the reference value of the quality control sample. Iodimetry and acid-base titration were not suitable for the determination of sulfur dioxide residues in spices such as star anise and edible mushrooms such as mushrooms. Foods contained organic acid additives such as glacial acetic acid, lactic acid and dehydroacetic acid were not suitable for the determination of sulfur dioxide residue by acid-base titration. The colorimetric method of para-rosaniline hydrochloride was low in automaticity, slow in analysis speed, and the detection accuracy and accuracy were greatly affected by human factors. Moreover, the extraction solution used was highly toxic and has great impact on human safety and environment, so it was recommended to avoid using it as far as possible. Compared with other methods, intermittent chemical analysis and ion chromatography had higher sensitivity and high automation level, which was suitable for the analysis and detection of sulfur dioxide residues in large quantities of food samples. Conclusion The appropriate detection method should be selected according to the sample type and the actual situation of detection in order to reduce the error of judgment caused by the difference of methods.