基于双频超声辅助酶解结合EDTA法快速高效提取水产品中的铅

A rapid and efficient extraction method for lead from aquatic products by dual-frequency ultrasonic-assisted enzymatic digestion combined with EDTA

建立了一种基于双频超声辅助酶解(DUED)结合乙二胺四乙酸二钠盐(EDTA)提取水产品中铅的前处理方法。该方法利用超声探头的空化效应促进蛋白酶的水解进程,并结合EDTA的强络合能力,可在12 min内快速提取鱼肉粉中的铅。通过单因素实验考察料液比、酶配方、酶解时间、EDTA提取时间和EDTA浓度对铅提取率的影响。在双频超声与EDTA提取相结合的模式下,最佳提取条件为:pH 7.0的磷酸盐溶液为缓冲溶液,料液比为1∶6(700 mg鱼肉粉样品+4.2 mL磷酸盐缓冲液),10 mg风味蛋白酶(5.5×10^(4)U/g)与70 mg中性蛋白酶(18.3×10^(5)U/g)为复配酶,超声辅助酶解时间为6 min,EDTA浓度为40 mmol/L,提取时间6 min。在最优条件下,鱼肉粉中铅的提取率可达(84.83±1.00)%。该前处理方法可实现鱼肉粉中铅的快速、高效提取,且与重金属的快速检测方法具有良好的兼容性,是一种有前景的食品安全检测前处理技术。

Herein,a pretreatment method based ondual-frequency ultrasonic-assisted enzymatic digestion(DUED)combined with disodium ethylenediaminetetraacetate(EDTA)for extracting lead from aquatic products was established.In this method,the cavitation effect of ultrasonic probe was employed to promote the hydrolysis process of protease,and combined with the strong complexing ability of EDTA,the lead in fish meal was quickly extracted within 12 min.The single factor experiment was carried out to investigate the effects of solid-liquid ratio,enzyme dosage,enzymolysis time,EDTA extraction time and concentrations on the extraction efficiency of lead.Under the mode of combining dual frequency ultrasound with EDTA extraction,the optimal extraction conditions were exhibited as follows:phosphate solution(pH 7.0)as buffer solution,solid-liquid ratio of 1∶6(700 mg of fish meal sample with 4.2 mL of phosphate buffer solution),10 mg of flavor protease(5.5×10^(4)U/g)and 70 mg of neutral protease(18.3×10^(5)U/g)as complex enzyme formula,40 mmol/L EDTA as extractant.The extraction rate of the lead from fish meal was around(84.83±1.00)%within 12 min,of which 6 min for DUED and 6 min for EDTA extraction.The results showed that the pretreatment method could achieve rapid and efficient extraction of lead from fish meal,and possesses favourable compatibility with the rapid determination of heavy metal.It can be recognized as a promising pretreatment technology for food safety detection.