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投稿时间:2021-11-30 修订日期:2021-12-08
投稿时间:2021-11-30 修订日期:2021-12-08
中文摘要: 为准确定量拟黑多刺蚁体内的微量元素,本实验采用微波消解法,以HNO3-H2O2混合酸为消解体系对样品进行前处理,选择合适的同位素,以103Rh为内标测定52Cr、55Mn、60Ni、63Cu、66Zn、75As、78Se、88Sr和114Cd,以185Re为内标测定202Hg和208Pb,建立了电感耦合等离子体质谱法测定拟黑多刺蚁中11种微量元素的方法。实验发现,以HNO3-H2O2为消解体系,样品消解完全;采用KED模式消除质谱干扰,以内标法校正基体效应;通过绘制校准曲线及测定流程空白,各元素校准曲线的相关系数均大于0.999,方法检出限为0.0005 ~0.0109 mg/kg, 方法定量限为0.0016 ~0.0327 mg/kg。对拟黑多刺蚁实际样品进行测定,各元素的相对标准偏差(RSD,n=9)在1.19 %~5.47 %之间,加标回收率为91.2 % ~107.0 %;经过实验室间比对比对试验,相对偏差为-3.15 %~2.74 %;测定六个不同产地的拟黑多刺蚁样品,结果显示不同产地样品除Cd外,其他10种微量元素的含量均存在较大差异。此方法测定结果稳定可靠,能满足拟黑多刺蚁中11种微量金属元素含量的分析检测要求。
Abstract:In order to accurately quantify the trace elements in the ant, the samples were pretreated by microwave digestion with HNO3-H2O2 mixed acid as the digestion system.The appropriate isotopes were selected. 52Cr、55Mn、60Ni、63Cu、66Zn、75As、78Se、88Sr and 114Cd were determined with 103Rh as internal standard, and 202Hg and 208Pb were determined with 185Re as internal standard. A method for the determination of 11 trace elements in Polyrhachis vicina rogers by inductively coupled plasma mass spectrometry was established. It was found that the sample was completely digested with HNO3-H2O2 as the digestion system. Ked mode was used to eliminate the interference of mass spectrometry, and the matrix effect was corrected by internal standard method. By drawing the calibration curve and determining the blank of the process, the correlation coefficient of the calibration curve of each element was greater than 0.999, the detection limit of the method was 0.0005 -0.0109 mg /kg, and the quantitative limit of the method was 0.0016 -0.0327 mg/ kg.The actual samples of Polyrhachis vicina rogers were determined. The relative standard deviations (RSD, n = 9) were in the range of 1.19 %-5.47 %, and the recoveries were 91.2 %-107.0 %. Through the comparison test between laboratories, the relative deviations were between - 3.15 % and 2.74 %. The samples of Polyrhachis vicina roger from six different habitats were determined. The results showed that there were great differences in the contents of other 10 trace elements except cadmium in samples from different habitats.The results of this method were stable and reliable, and could meet the requirements for the analysis and detection of 11 trace metal elements in Polyrhachis vicina roger.
keywords: microwave digestion, ICP-MS, Polyrhachis vicina roger, multielement determination, Ked mode
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基金项目:广西科技基地和人才专项资助项目
引用文本:
古行乾,李光明,曾志平,施意华,唐碧玉,张征莲.微波消解-电感耦合等离子体质谱(ICP-MS)法测定拟黑多刺蚁中11种微量元素[J].中国无机分析化学,2022,12(5):92-97.
Gu Xingqian,Li Guangming,Zeng Zhiping,Shi Yihua,Tang Biyu,Zhang Zhenglian.Determination of 11 trace elements in PolyrhachisSvicinaSroger by inductively coupled plasma mass spectrometry after microwave digestion[J].Chinese Journal of Inorganic Analytical Chemistry,2022,12(5):92-97.
古行乾,李光明,曾志平,施意华,唐碧玉,张征莲.微波消解-电感耦合等离子体质谱(ICP-MS)法测定拟黑多刺蚁中11种微量元素[J].中国无机分析化学,2022,12(5):92-97.
Gu Xingqian,Li Guangming,Zeng Zhiping,Shi Yihua,Tang Biyu,Zhang Zhenglian.Determination of 11 trace elements in PolyrhachisSvicinaSroger by inductively coupled plasma mass spectrometry after microwave digestion[J].Chinese Journal of Inorganic Analytical Chemistry,2022,12(5):92-97.