海蜇中铝测定前处理方法及检测方法比较

摘要

目的：采用4种不同的前处理方法结合2种不同检测方法对海蜇产品中铝含量进行测定，探索简易、精密度高、准确度高、适用性强的检测方法。方法取鲜海蜇、盐渍海蜇、即食海蜇样品，采用水煮消解、酸煮消解、微波消解、电热板消解4种不同前处理方法结合滴定和 ICP-MS2种方法测定海蜇产品中铝，同时做精密度及回收率试验。结果酸煮消解、微波消解及电热板消解3种前处理方法检测结果经统计学检验无显著性差异(P>0.01)，三种前处理方法的 RSD%<2%，回收率在101.2%~105.4%；水煮消解法测定铝含量低，与其他方法有显著性差异(P<0.01)；酸煮消解-ICP-MS 法回收率低，只有78.7%。结论水煮消解法提取率低，不适用于海蜇产品中铝提取；酸煮滴定法检测成本低、有较高精密度及准确度，可被企业及检测机构用于海蜇中铝的测定；电热板消解-滴定法亦取得满意效果，样品量较大时可考虑代替酸煮滴定法用于企业检测；微波消解-ICP-MS测定法操作方便、灵敏度高、回收率高，适用于检测条件较好的研究机构。%Objective Four different pre-treatment methods combined with two different detection methods was established to determinate the aluminum content in jellyfish products to explore simple, precise, accuracy, strongly applicable detection method. Methods Fresh jellyfish, salted jellyfish and instant jellyfish samples were prepared by boiled digestion, acid digestion, microwave digestion and electric-heating-plate digestion respectively, and then aluminum content of each sample was determined using titration and ICP-MS methods, respectively. The precision and recoveries were measured simultaneously. Results There were no significant difference among 3 preparation approaches including acid digestion, microwave digestion and electric-heating-plate digestion with paired t-test (P>0.01). The recoveries were in the range of 101.2%∼105.4% with RSD<2%. Significant difference was found between boiled digestion and the other methods (P<0.01), and the recovery ratio was only 78.7% for acid digestion-ICP-MS method. Conclusion Boiled digestion was not suitable for pretreatment of aluminum in jellyfish products with low extraction rate. Acid titration method could be used for the determination of jellyfish aluminum by enterprises and inspection agencies, with low costs, high precision and accuracy. Electric-heating-plate digestion plus titration method could be applied with satisfactory precision and accuracy to replace acid titration detection by the enterprises in case of a large quantity of samples. Microwave digestion plus ICP-MS method was suitable for research institutes of high standard facilities, because of its convenient operation, high sensitivity, and high recovery ratio.