微波消解-电感耦合等离子体质谱法测定畜禽粪便中8种金属元素
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摘要
目的建立微波消解-电感耦合等离子体质谱法(microwave digestion-inductively coupled plasma mass spectrometry, ICP-MS)测定畜禽粪便中8种金属元素的含量。方法干燥后的畜禽粪便样品经高速球磨仪球磨匀,采用微波消解仪对样品进行消解,消解后的样品用ICP-MS混合模式测定畜禽粪便中的砷、汞、铅、镉、铬、锌、铜和镍等8种金属元素,内标法定量。结果 8种元素检出限分别在0.017～0.64μg/L之间,线性关系良好,相关线性系数r>0.999;不同元素的添加回收率为92.0%～101.9%,相对标准偏差为0.9%～5.0%。结论该方法样品前处理简单高效、分析用时短、准确度和精密度高,适用于批量畜禽粪便中多元素的测定。
Objective To establish a method for determination the content of 8 metallic elements in livestock manure by microwave digestion-inductively coupled plasma mass spectrometry(ICP-MS). Methods The samples of livestock manure were dried and then mill with a high-speed ball mill. The samples were digested by microwave digestion instrument. After digested the 8 metallic elements of arsenic, mercury, lead, cadmium, chromium, zinc, copper and nickel in the sample were analyzed by mixed mode, and 8 kinds of metal elements were quantified by internal standard method. Results The results showed that the limits of detection of the 8 elements were 0.017-0.64 μg/L, and the linear correlation coefficients were more than 0.999. The recoveries of different elements were 92.0%-101.9%, with the relative standard deviations of 0.9%-5.0%. Conclusion The method is simple, rapid, high in accuracy and precision, and is suitable for simultaneous determination of multi-elements in livestock manure.
Objective To establish a method for determination the content of 8 metallic elements in livestock manure by microwave digestion-inductively coupled plasma mass spectrometry(ICP-MS). Methods The samples of livestock manure were dried and then mill with a high-speed ball mill. The samples were digested by microwave digestion instrument. After digested the 8 metallic elements of arsenic, mercury, lead, cadmium, chromium, zinc, copper and nickel in the sample were analyzed by mixed mode, and 8 kinds of metal elements were quantified by internal standard method. Results The results showed that the limits of detection of the 8 elements were 0.017-0.64 μg/L, and the linear correlation coefficients were more than 0.999. The recoveries of different elements were 92.0%-101.9%, with the relative standard deviations of 0.9%-5.0%. Conclusion The method is simple, rapid, high in accuracy and precision, and is suitable for simultaneous determination of multi-elements in livestock manure.
引文
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[12]刘芸,曹国松,程佩,等.微波消解-ICP-MS法测定土壤中的硒含量[J].化学与生物工程,2017,34(11):67-70.Liu Y,Cao GS,Cheng P,et al.Determination of selenium content in soil by microwave digestion-ICP-MS[J].Chem Bioeng,2017,34(11):67-70.
[13]王小如.电感耦合等离子体质谱应用实例[M].北京:北京化学工业出版社,2005.Wang XR.Inductively coupled plasma mass spectrometry application examples[M].Beijing:Beijing Chemical Industry Press,2005.
[14]候建荣,周洪伟,黄聪,等.电感耦合等离子体质谱法同时测定玉米面中铅、镉、砷和总汞的含量[J].中国卫生检验杂志,2014,24(22):3235-3237.Hou JR,Zhou HW,Huang C,et al.Simultaneous determination of lead,cadmium,arsenic and total mercury content in corn flour by ICP-MS[J].Chin J Health Lab Technol,2014,24(22):3235-3237.
[15]张建,卢垣宇,田志强,等.ICP-MS检测食品中铅、砷、汞、镉、钡、铬、银、镍8种有害元素[J].食品工业,2015,3:278-281.Zhang J,Lu YY,Tian ZQ,et al.Determination of lead,arsenic,mercury,cadmium,barium,chromium,silver and nickel in food by ICP-MS[J].Food Ind,2015,3:278-281.
[16]黄子敬,陈孟君,邓华阳,等.微波消解-ICP-MS混合模式测定动植物源性食品中11种金属元素[J].分析试验室,2017,36(1):24-28.Huang ZJ,Chen MJ,Deng HY,et al.Determination of 11 trace elements in animal and plant origin food by microwave digestion with ICP-MS in mixed mode[J].Chin J Anal Lab,2017,36(1):24-28.
[2]孙西宁,李艳霞,张增强,等.城市污泥好氧堆肥过程中重金属的形态变化[J].环境科学学报,2009,29(9):1836-1841.Sun XN,Li YX,Zhang ZQ,et al.Extractable forms of heavy metals produced during municipal sludge composting[J].Acta Sci Circumst,2009,(9):1836-1841.
[3]熊雄,李艳霞,韩杰,等.堆肥腐殖质的形成和变化及其对重金属有效性的影响[J].农业环境科学学报,2008,27(6):2137-2142.Xiong X,Li YX,Han J,et al.Formation and transformation of humus in composting and its impacts on bioavailability of toxic metals[J].JAgro-Environ Sci,2008,27(6):2137-2142.
[4]贾双珠,李长安,解田,等.ICP-MS分析应用进展[J].分析试验室,2016,35(6):731-735.Jia SZ,Li CA,Xie T,et al.Application of inductively coupled plasma mass spectrometry in material analysis[J].Chin J Anal Lab,2016,35(6):731-735.
[5]冯先进,屈太原.电感耦合等离子体质谱法(ICP-MS)最新研究进展[J].中国无机分析化学,2011,1(1):46-52.Feng XJ,Qu TY.The latest application progress of inductively coupled plasma mass spectrometry[J].Chin J Inorg Anal Chem,2011,1(1):46-52.
[6]胡曙光,苏祖俭,黄伟雄,等.食品中重金属元素痕量分析消解技术的进展与应用[J].食品安全质量检测学报,2014,5(5):1270-1278.Hu SG,Su ZJ,Huang WX,et al.Progress and application in the digestion technology of trace heavy metal elements determination in food[J].JFood Staf Qual,2014,5(5):1270-1278.
[7]蒋次清,王岚,廖臻,等.微波马弗炉测定烟草中灰分的研究[J].安徽农业科学,2012,40(7):3980-3996.Jiang CQ,Wang L,Liao Z,et al.Study on the determination of ash in tobacco by microwave muffle furnace[J].J Anhui Agric Sci,2012,40(7):3980-3996.
[8]樊祥,张润何,刘博,等.高效液相色谱-原子荧光光谱法测定水产品中不同形态汞含量[J].食品安全质量检测学报,2017,8(1):76-81.Fan X,Zhang RH,Liu B,et al.Determination the content of mercury in different speciations in aquatic products by high performance liquid chromatography-atomic fluorescence spectrometry[J].J Food Saf Qual,2017,8(1):76-81.
[9]宋洪强,郝云彬,吴益春,等.原子荧光亮度法中湿法消解、微波消解、干灰化前处理法测定水产品中总砷含量的比较[J].浙江海洋学院学报,2010,29(4):367-372.Song HQ,Hao YB,Wu YC,et al.Comparison of wet,microwave digestion and dry ash pretreatment methods for the determination of total arse nic in seafood by atomic fluorescence spectrometer[J].J Zhejiang Ocean Univ,2010,29(4):367-372.
[10]杨延,周小力.高压密封消化罐在光谱分析样品前处理中的应用[J].光谱学与光谱分析,2001,21(6):886-888.Yang Y,Zhou XL.Applicaton of digestion pot of hp hermetic seal in sample pretreatment in spectral analysis[J].Spectrosc Spect Anal,2001,21(6):886-888.
[11]刘华.微波消解技术在分析食品中微量元素方面的应用[J].中国卫生检验杂志,2001,11(4):406-408.Liu H.The technical application of the method breaking down the food sample in tne special microwave oven for analyzing microelement[J].Chin J Health Lab Technol,2001,11(4):406-408.
[12]刘芸,曹国松,程佩,等.微波消解-ICP-MS法测定土壤中的硒含量[J].化学与生物工程,2017,34(11):67-70.Liu Y,Cao GS,Cheng P,et al.Determination of selenium content in soil by microwave digestion-ICP-MS[J].Chem Bioeng,2017,34(11):67-70.
[13]王小如.电感耦合等离子体质谱应用实例[M].北京:北京化学工业出版社,2005.Wang XR.Inductively coupled plasma mass spectrometry application examples[M].Beijing:Beijing Chemical Industry Press,2005.
[14]候建荣,周洪伟,黄聪,等.电感耦合等离子体质谱法同时测定玉米面中铅、镉、砷和总汞的含量[J].中国卫生检验杂志,2014,24(22):3235-3237.Hou JR,Zhou HW,Huang C,et al.Simultaneous determination of lead,cadmium,arsenic and total mercury content in corn flour by ICP-MS[J].Chin J Health Lab Technol,2014,24(22):3235-3237.
[15]张建,卢垣宇,田志强,等.ICP-MS检测食品中铅、砷、汞、镉、钡、铬、银、镍8种有害元素[J].食品工业,2015,3:278-281.Zhang J,Lu YY,Tian ZQ,et al.Determination of lead,arsenic,mercury,cadmium,barium,chromium,silver and nickel in food by ICP-MS[J].Food Ind,2015,3:278-281.
[16]黄子敬,陈孟君,邓华阳,等.微波消解-ICP-MS混合模式测定动植物源性食品中11种金属元素[J].分析试验室,2017,36(1):24-28.Huang ZJ,Chen MJ,Deng HY,et al.Determination of 11 trace elements in animal and plant origin food by microwave digestion with ICP-MS in mixed mode[J].Chin J Anal Lab,2017,36(1):24-28.