离子色谱法测定肉类中总硫的含量

Determination of total sulfur in meats by ion chromatography

中文关键词:  离子色谱法  总硫  褐煤  燃烧  肉

英文关键词:ion chromatography  total sulfur  lignite  burning  meats

中文摘要:

      目的 建立肉类中总硫含量的离子色谱(ion chromatography, IC)检测方法。方法 肉类经过粉碎、混合均匀后,于70 ℃真空烘干3 h。取50 mg烘干的样品与100 mg褐煤混合燃烧, 产生的二氧化硫、三氧化硫用艾士卡试剂(Eschka)吸收转化成硫酸盐。用10.0 mL去离子水溶解艾氏卡试剂, 取稀释后的上清液过水相膜进样。经阴离子交换柱分离, 用离子色谱法对硫酸根离子进行检测, 采取外标法定量。结果 硫酸根离子在0.0781～10.0 mg/L范围内线性关系良好, 相关系数大于0.999。方法检出限、定量限分别为4.00和10.0 mg/kg; 相对标准偏差为9.15%～14.7%。结论 该方法简便、基质干扰小; 其准确度、检出限等参数均能满足相关的技术规范的要求, 适合用于市售肉类中总硫的检测。

英文摘要:

      Objective To establish a method for determination of total sulfur in meats by ion chromatography(IC). Methods The meat sample was crushed and mixed evenly, then dried in vacuum at 70 ℃ for 3 h. Then 50 mg dried sample were mixed with 100 mg lignite for burning, and the sulfur dioxide and sulfur trioxide originated from burning were absorbed by Eschka agent and converted into sulfates. The Eschka agent was dissolved with 10.0 mL deionized water and then the diluted supernatant was taken and injected through aqueous phase membrane. Sulfate radical was analyzed by IC after anion exchange column isolation, and then quantified by external standard method. Results The calibration curve of sulfate ion appeared good linearity in the range of 0.0781– 10.0 mg/L, with a correlation coefficient greater than 0.999 (r2>0.999). The the limit of detection (LOD) and limit of quantification (LOQ) was 4.00 and 10.0 mg/kg, respectively. Relative standard deviations (RSDs) were 9.15% –14.7%. Conclusion The method is simple, the matrix interference is small, its accuracy, detection limit and other parameters can meet the requirements of relevant technical specifications, which is suitable for the detection of total sulfur in commercial meat.