稀酸提取-ICP-MS法快速测定大米中锰、铜、锌、铅、镉、铷、锶的含量
|
摘要
建立了常温条件下,利用稀酸提取-电感耦合等离子体质谱法快速测定大米中元素(锰、铜、锌、铅、镉、铷、锶)的方法。实验通过优化影响提取的各个因素,确定了最终提取条件。该方法各元素的回收率均在90%～111%,且标准物质相关元素的浸提结果均在相应赋值范围内。多家实验室联合验证的统计结果显示7家实验室的各元素HorRat值均小于1,表明该方法拥有很好的重现性和再现性。稀酸温和提取-电感耦合等离子体质谱法具有高效、快速、准确的特点,可将样品处理时间缩短至30 min内,与经典微波消解-ICP-MS法比较,锰、铜、锌、铅、镉、铷、锶元素的测定值无显著性差异(P>0. 05)。
The method for rapid determination of the elements(Cd, Mn, Pb, Zn, Cu, Rb and Sr) in rice was established using diluted acid extraction method by ICP-MS. The influence factors of the experiment were optimized to make the best extraction condition. The spiked recoveries of all elements at different concentrations in rice ranged from 90% to 111 %, and the extraction results of related elements in the standards reference materials was verified to be in the range of standard uncertainties. A collaborative study was organized to evaluate the methods. Many laboratories' joint verification and statistics result showed that each element of HorRat value of the 7 laboratories were all less than 1,which confirmed that the method had perfect repeatability and reproducibility. The diluted acid mild extraction method reduced the pretreatment time to 30 min and the detected result had no significance difference with the traditional microwave digest method( P > 0. 05).
The method for rapid determination of the elements(Cd, Mn, Pb, Zn, Cu, Rb and Sr) in rice was established using diluted acid extraction method by ICP-MS. The influence factors of the experiment were optimized to make the best extraction condition. The spiked recoveries of all elements at different concentrations in rice ranged from 90% to 111 %, and the extraction results of related elements in the standards reference materials was verified to be in the range of standard uncertainties. A collaborative study was organized to evaluate the methods. Many laboratories' joint verification and statistics result showed that each element of HorRat value of the 7 laboratories were all less than 1,which confirmed that the method had perfect repeatability and reproducibility. The diluted acid mild extraction method reduced the pretreatment time to 30 min and the detected result had no significance difference with the traditional microwave digest method( P > 0. 05).
引文
[1]任艳丽,王建林.锶的生物学效应研究进展[J].北京联合大学学报,2018,31(1):44-48REN Yanlin,WANG Jianlin. Reserch progress on the biological effect of strontium[J]. Journal of Beijing Union University,2018,31(1):44-48
[2]秦俊法.铷的生物必需性及人体健康效应[J].广东微量元素科学,2000,7(8):1-18QIN Junfa. Biological essentiality of Rubidium and its health effects on humans[J]. Guangdong Trace Elements Science,2000,7(8):1-18
[3]章连香.食品中重金属元素检测方法研究进展[J].中国无机分析化学,2017,7(01):13-18ZHANG Lianxiang. Research progress on determination of heavy metal elements in food[J]. Chinese Journal of Inorganic Analytical Chemistry,2017,7(01):13-18
[4] GB 5009. 268-2016,食品安全国家标准食品中多元素的测定[S]GB 5009. 268—2016,Determination of multielement in foods[S]
[5]JULSHAMN K,MAAGE A,NORLI H S,et al. Determinationof arsenic, cadmium, mercury, and lead in foods by pressure digestion and inductively coupled plasma/mass spectrometry[J]. Journal of Journal of Association of Official Analytical Chemists International,2013,96(5):1101-1102
[6]张建辉,张继红,张丽,等.ICP-MS法和石墨炉原子吸收法测定大米中镉含量不确定度评估的比较[J].食品科学,2016,37(18):185-189ZHANG Jianhui,ZHANG Jihong,ZHANG Li,et al. Comparative study of uncertainty evaluation of cadmium content in rice by inductively coupled plasma-mass spectrometry(ICPMS)and graphite furnace atomic absorption spectrometry[J]. Journal of Food Science,2016,37(18):185-189
[7]张更宇,吴超,邓宇杰.电感耦合等离子体质谱(ICPMS)联用技术的应用及展望[J].中国无机分析化学,2016,6(3):19-26ZHANG Gengyu, WU Chao, DENG Yujie. Application and outlook of the hyphenated ICP-MS technique[J]. Chinese Journal of Inorganic Analytical Chemistry, 2016, 6(3):19-26
[8]杨雪娇,黄伟,林涛,等.不同前处理方法检测食品中的重金属含量[J].现代食品科技,2008,10(24):1051-1054,1011YANG Xuejiao, HUANG Wei, LIN Tao,et al. Determination of heavy metal contents in foodstuffs by three pretreatment methods[J]. Modern Food Science and Technology,2008,10(24):1051-1054,1011
[9]周明慧,王松雪,伍燕湘.稀酸温和提取直接进样石墨炉原子吸收法快速测定谷物中铅的含量[J].分析化学,2014,42(3):459-460ZHOU Minghui,WANG Songxue,WU Yanxiang. Rapid direct sampling detection of Pb in grain using diluted acid extraction coupled with graphite furnace atomic absorption spectropho-tometry[J]. Chinese Journal of Analytical Chemistry,2014,3(42):459-460
[10]周明慧,王松雪,伍燕湘.稀酸温和提取直接进样快速测定大米中镉含量的研究[J].中国粮油学报,2015,30(2):97-102ZHOU Minghui,WANG Songxue,WU Yanxiang. Rapid direct sampling detection of Cd in grain using diluted acid extraction[J]. Journal of the Chinese Cereals and Oils Association,2015,30(2):97-102
[11]JJF 1159-2006,四极杆电杆耦合等离子体质谱仪校准规范[S]JJF 1159—2006, Calibration specification for quadrupole inductively coupled plasma mass spectrometers[S]
[12]JJF 1343-2012,标准物质定值的通用原则及统计学原理[S]JJF 1343—2012,General and statistical principles for characterization of reference materials[S]
[13]BS ISO 5725-5-1998 Accuracy(trueness and precision)of measurement methods and results-Alternative methods for the determination of the precision of a standard measurement method[S]
[14] HORWITZ W, ALBERT R. Performance characteristics of methods of analysis used for regulatory purposes. Part II. Pesticide formulations[J]. Journal of Association of Official Analytical Chemists,1991,74(5):718-744
[15] HORWITZ W, ALBERT R. The Horwitz ratio(HorRat):A useful index of method performance with respect to precision[J]. Journal of Association of Official Analytical Chemists international,2006,89(4):1095-1109
[16] WHO&FOA. Codex alimentarius commission procedural manual[M]. Version 24. Food and Agriculture Organization of the United Nations,2015:66-67.
[2]秦俊法.铷的生物必需性及人体健康效应[J].广东微量元素科学,2000,7(8):1-18QIN Junfa. Biological essentiality of Rubidium and its health effects on humans[J]. Guangdong Trace Elements Science,2000,7(8):1-18
[3]章连香.食品中重金属元素检测方法研究进展[J].中国无机分析化学,2017,7(01):13-18ZHANG Lianxiang. Research progress on determination of heavy metal elements in food[J]. Chinese Journal of Inorganic Analytical Chemistry,2017,7(01):13-18
[4] GB 5009. 268-2016,食品安全国家标准食品中多元素的测定[S]GB 5009. 268—2016,Determination of multielement in foods[S]
[5]JULSHAMN K,MAAGE A,NORLI H S,et al. Determinationof arsenic, cadmium, mercury, and lead in foods by pressure digestion and inductively coupled plasma/mass spectrometry[J]. Journal of Journal of Association of Official Analytical Chemists International,2013,96(5):1101-1102
[6]张建辉,张继红,张丽,等.ICP-MS法和石墨炉原子吸收法测定大米中镉含量不确定度评估的比较[J].食品科学,2016,37(18):185-189ZHANG Jianhui,ZHANG Jihong,ZHANG Li,et al. Comparative study of uncertainty evaluation of cadmium content in rice by inductively coupled plasma-mass spectrometry(ICPMS)and graphite furnace atomic absorption spectrometry[J]. Journal of Food Science,2016,37(18):185-189
[7]张更宇,吴超,邓宇杰.电感耦合等离子体质谱(ICPMS)联用技术的应用及展望[J].中国无机分析化学,2016,6(3):19-26ZHANG Gengyu, WU Chao, DENG Yujie. Application and outlook of the hyphenated ICP-MS technique[J]. Chinese Journal of Inorganic Analytical Chemistry, 2016, 6(3):19-26
[8]杨雪娇,黄伟,林涛,等.不同前处理方法检测食品中的重金属含量[J].现代食品科技,2008,10(24):1051-1054,1011YANG Xuejiao, HUANG Wei, LIN Tao,et al. Determination of heavy metal contents in foodstuffs by three pretreatment methods[J]. Modern Food Science and Technology,2008,10(24):1051-1054,1011
[9]周明慧,王松雪,伍燕湘.稀酸温和提取直接进样石墨炉原子吸收法快速测定谷物中铅的含量[J].分析化学,2014,42(3):459-460ZHOU Minghui,WANG Songxue,WU Yanxiang. Rapid direct sampling detection of Pb in grain using diluted acid extraction coupled with graphite furnace atomic absorption spectropho-tometry[J]. Chinese Journal of Analytical Chemistry,2014,3(42):459-460
[10]周明慧,王松雪,伍燕湘.稀酸温和提取直接进样快速测定大米中镉含量的研究[J].中国粮油学报,2015,30(2):97-102ZHOU Minghui,WANG Songxue,WU Yanxiang. Rapid direct sampling detection of Cd in grain using diluted acid extraction[J]. Journal of the Chinese Cereals and Oils Association,2015,30(2):97-102
[11]JJF 1159-2006,四极杆电杆耦合等离子体质谱仪校准规范[S]JJF 1159—2006, Calibration specification for quadrupole inductively coupled plasma mass spectrometers[S]
[12]JJF 1343-2012,标准物质定值的通用原则及统计学原理[S]JJF 1343—2012,General and statistical principles for characterization of reference materials[S]
[13]BS ISO 5725-5-1998 Accuracy(trueness and precision)of measurement methods and results-Alternative methods for the determination of the precision of a standard measurement method[S]
[14] HORWITZ W, ALBERT R. Performance characteristics of methods of analysis used for regulatory purposes. Part II. Pesticide formulations[J]. Journal of Association of Official Analytical Chemists,1991,74(5):718-744
[15] HORWITZ W, ALBERT R. The Horwitz ratio(HorRat):A useful index of method performance with respect to precision[J]. Journal of Association of Official Analytical Chemists international,2006,89(4):1095-1109
[16] WHO&FOA. Codex alimentarius commission procedural manual[M]. Version 24. Food and Agriculture Organization of the United Nations,2015:66-67.
© 2004-2018 中国地质图书馆版权所有 京ICP备05064691号 京公网安备11010802017129号 地址：北京市海淀区学院路29号 邮编：100083 电话：办公室：(+86 10)66554848；文献借阅、咨询服务、科技查新：66554700 |