不同前处理方法对ICP-MS法测定热带水果中主要重金属元素的影响
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摘要
分别采用微波消解法、湿式消解法以及干法灰化法对水果样品进行前处理,并建立最佳消解方法,然后采用电感耦合等离子体质谱法(ICP-MS)对不同前处理样品中的Pb、Cd、Cr、Ni等4种元素进行检测分析。结果表明:Pb、Cd、Cr、Ni等4种元素经过微波消解后的方法检出限分别为0.029 0、0.002 6、0.021 0、0.250 0μg·L~(-1),相对标准偏差均小于2.5%,加标回收率为88.1%～108.3%;4种元素经过湿法消解后的方法检出限为0.028 0、0.002 4、0.018 0、0.210 0μg·L~(-1),相对标准偏差均小于3.5%,加标回收率为86.7%～106.9%;4种元素经过干法灰化法后的方法检出限为0.031 0、0.002 8、0.023 0、0.250 0μg·L~(-1),相对标准偏差均小于3.5%,加标回收率为86.6%～111.5%。这3种前处理方法与ICP-MS法结合均能对热带水果中重金属元素进行较为准确的检测,微波消解法具有检测结果准确、耗时少、操作简便等优点;湿式消解法具有方法检出限低、结果准确且重现性好等优点;干法灰化法具备结果准确等优点,但耗时较长。
Microwave digestion,wet digestion and dry digestion were used for the pretreatment of the fruit samples,and the best digestion method was established.Then,four elements including Pb,Cd,Cr and Ni in the samples with different pretreatment methods were detected and analyzed by using ICP-MS method.The results showed that the method detection limits of Pb,Cd,Cr and Ni after microwave digestion were respectively 0.029 0,0.002 6,0.021 0 and 0.250 0μg·L~(-1),and the relative standard deviations were all less than 2.5%,while the adding standard recovery was 88.1%-108.3%.The method detection limits of four elements after wet digestion were 0.028 0,0.002 4,0.018 0,0.21μg·L~(-1),and the relative standard deviations were all less than 3.5%,while the adding standard recovery was 86.7%-106.9%.The method detection limits of four elements after dry digestion were 0.031 0、0.002 8、0.023 0、0.250 0μg·L~(-1),and the r relative standard deviations were all less than 3.5%,while the adding standard recovery was 86.6%-111.5%.By combining with ICP-MS method,the three pretreatment methods could all be used for the accurate detection of heavy metal elements in tropical fruits.Microwave digestion method had the advantages of accurate detection results,less time consumption and simple & convenient operation.Wet digestion method had the advantages of low method detection limits,accurate results and good reproducibility.Dry digestion method had the advantages of accurate results and more time consumption.
Microwave digestion,wet digestion and dry digestion were used for the pretreatment of the fruit samples,and the best digestion method was established.Then,four elements including Pb,Cd,Cr and Ni in the samples with different pretreatment methods were detected and analyzed by using ICP-MS method.The results showed that the method detection limits of Pb,Cd,Cr and Ni after microwave digestion were respectively 0.029 0,0.002 6,0.021 0 and 0.250 0μg·L~(-1),and the relative standard deviations were all less than 2.5%,while the adding standard recovery was 88.1%-108.3%.The method detection limits of four elements after wet digestion were 0.028 0,0.002 4,0.018 0,0.21μg·L~(-1),and the relative standard deviations were all less than 3.5%,while the adding standard recovery was 86.7%-106.9%.The method detection limits of four elements after dry digestion were 0.031 0、0.002 8、0.023 0、0.250 0μg·L~(-1),and the r relative standard deviations were all less than 3.5%,while the adding standard recovery was 86.6%-111.5%.By combining with ICP-MS method,the three pretreatment methods could all be used for the accurate detection of heavy metal elements in tropical fruits.Microwave digestion method had the advantages of accurate detection results,less time consumption and simple & convenient operation.Wet digestion method had the advantages of low method detection limits,accurate results and good reproducibility.Dry digestion method had the advantages of accurate results and more time consumption.
引文
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[3]李刚丽.基于GSM的智能温湿度监测系统设计[J].中小企业管理与科技,2013(8):282-283.
[4]李志强,屈国普,陈列尊,等.基于GSM的温湿度远程监控系统设计[J].核电学与探技术,2010(4):533-536.
[5]谢金成,苏燕婷.基于GSM测控的蝴蝶兰花养殖系统[J].福建师大福清分校学报,2014(S1):110-114.
[6]罗悠,邓飞跃,孟时贤.湿法消解-电感耦合等离子体原子发射光谱(ICP-AES)法测定饲料中19种微量元素[J].中国无机分析化学,2017(2):72-77.
[7]贾春晓.现代仪器分析技术及其在食品中的应用[M].北京:中国轻工业出版社,2017:282.
[8]孙秀敏,雷敏,李璐,等.微波消解-ICP-MS法同时测定土壤中8种重(类)金属元素[J].分析试验室,2014(10):1177-1180.
[9]王小如.电感耦合等离子体质谱应用实例[M].北京:化学工业出版社,2005:35.
[10]刘虎生,邵宏翔.电感耦合等离子体质谱技术与应用[M].北京:化学工业出版社,2005:131.
[11]刘丽萍,毛红,张妮娜,等.电感耦合等离子体质谱法(ICP-MS)测定运动员食品中砷、镉、铜[J].质谱学报,2006,27(2):90-93.
[12]林立,陈玉红,田艳玲,等.电感耦合等离子体质谱法直接测定酱油中的铅[J].环境化学,2007,26(3):410-412.
[13]陈国友.微波消解ICP-MS法同时测定蔬菜中14种元素[J].分析测试学报,2007,26(5):742-745.
[14]国家药典委员会.中华人民共和国药典[M].北京:化学工业出版社,2005:附录45.
[15]中华人民共和国国家卫生和计划生育委员会,国家食品药品监督管理总局.食品安全国家标准食品中污染物限量:GB2762-2017[S].北京:中国标准出版社,2017.