自动石墨消解-ICP-MS法检测水产罐头中的铅、铬等7种金属

试验建立了全自动石墨消解仪消解水产罐头样品,电感耦合等离子体质谱法同时检测铅、铬、铝、砷、锡、镍、铜金属残留的分析方法。水产罐头样品经全自动石墨消解仪消解,消解酸选择HNO3-H2O2(3︰2,V/V),消解完毕后上机分析,内标法定量检测。结果显示,铅、铬、铝、砷、锡、镍、铜7种金属在质量浓度0.1~20μg/L范围内具有良好的线性关系,相关系数(R2)均高于0.995;检测限为:铅0.004 mg·kg^-1,铬0.006 mg·kg^-1,铝0.012mg·kg^-1,砷0.009 mg·kg^-1,锡0.0014 mg·kg^-1,镍0.008 mg·kg^-1和铜0.005 mg·kg^-1;加标范围在0.1~10μg/L质量浓度内,回收率在87.4%~106.2%之间;重复性和精密度RSD(n=6)均在5.0%以内。该方法具有简便、污染小、准确、前处理简单等优点。

Automatic Graphite Digestion-ICP-MS Method for Detection of Seven Metals Including Lead and Chromium in Canned Aquatic Products

Automatic graphite digestion ICP-MS method for determination of plumbum,chromium,aluminum,arsenic,tin,nickel and copper residues in canned aquatic products was established.Canned aquatic products were digested by automatic graphite digestion.The volume ratio of HNO3 and H2O2 selected for digestion acid was 3︰2.After digestion,samples were analyzed on ICP-MS,and internal standard method was selected as quantitative detection.The result showed that plumbum,chromium,aluminum,arsenic,tin,nickel and copper had good linear relationships in the range 0.1-20μg/L,and correlation coefficients were all above 0.995.Detection limits were as follows:plumbum 0.004 mg·kg^-1,chromium 0.006 mg·kg^-1,aluminum 0.012 mg·kg^-1,arsenic 0.009 mg·kg^-1,tin 0.0014 mg·kg^-1,nickel 0.008 mg·kg^-1,and copper 0.005 mg·kg^-1,respectively.The markup range is within 0.1-10μg/L,and the recovery rate is between 87.4%and 106.2%;The average recoveries in 3 different levels were ranged from 87.4%-106.2%.Relative standard deviation of precision and reproducibility were less than 5.0%(n=6).This method has the advantages of simplicity,less pollution,accuracy and simple pretreatment.