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目的建立微波消解-ICP-MS法同时测定烤鱼片中铅、镉、砷、汞、镍、铬6种元素的方法,了解烤鱼中重金属污染状况。方法针对烤鱼片样品基质复杂和汞元素在仪器管路中易残留等问题,本研究系统优化了消解方式、赶酸温度、稀释倍数、内标物和金溶液浓度等主要影响因素,采用硝酸作为消解体系,微波消解后170℃赶酸,加入Au溶液后25倍稀释样品测试铅、镉、镍、铬、汞,100倍稀释测试砷,采用ICP-MS法检测烤鱼中6种元素含量。结果经优化的前处理方案有效降低了基质效应和汞残留,各元素的方法检出限为0.000 5 mg/kg~0.008 0 mg/kg,加标回收率为81.2%~115.0%,精密度(RSD)为0.7%~6.2%。结论该方法安全快速,汞残留少,精密度高,准确度好,适用于烤鱼片等烤制食品中铅、镉、砷、汞、镍、铬等多元素同时检测。
Objective To establish a method for the simultaneous determination of 6 elements of lead, cadmium, arsenic, mercury, nickel and chromium in roasted fish by microwave digestion-ICP-MS and understand the status of heavy metal pollution in roasted fish. Methods In order to solve the problems of the complex matrix of sample and the residue of mercury in the instrument pipeline, the main influencing factors such as digestion mode, temperature, dilution ratio, internal standard and concentration of gold solution were optimized. Nitric acid As digestion system, microwave digestion 170 ℃ catch acid, adding Au solution 25 times diluted samples tested lead, cadmium, nickel, chromium, mercury, 100 times diluted test arsenic, ICP- . Results The optimized pretreatment scheme effectively reduced the matrix effect and mercury residue. The detection limits of each element were 0.000 5 mg / kg ~ 0.008 0 mg / kg, and the recoveries were 81.2% ~ 115.0%. The precision RSD) of 0.7% to 6.2%. Conclusion The method is safe, rapid, less mercury residue, high precision and good accuracy. It is suitable for the simultaneous detection of multiple elements such as lead, cadmium, arsenic, mercury, nickel and chromium in grilled food such as grilled fish fillets.