为了寻求大豆油中铬(Cr)的快速检测方法,应用激光诱导击穿光谱(LIBS)技术对大豆油中Cr含量进行定量检测研究,采用松木对大豆油样品中的Cr进行富集,并利用双通道光谱仪采集其LIBS光谱信号;选择钙(Ca)422.64 nm为内标线,并以Cr的原子谱线C...为了寻求大豆油中铬(Cr)的快速检测方法,应用激光诱导击穿光谱(LIBS)技术对大豆油中Cr含量进行定量检测研究,采用松木对大豆油样品中的Cr进行富集,并利用双通道光谱仪采集其LIBS光谱信号;选择钙(Ca)422.64 nm为内标线,并以Cr的原子谱线Cr I 425.44 nm、Cr I 427.48 nm、Cr I428.94 nm及3条谱线之和为分析线,应用直接定标法和内定标法分别建立上述分析线的定标曲线。结果表明,Cr I 425.44 nm建立的定标曲线性能最佳,直接定标法和内定标法所建立的定标曲线的拟合度R2分别为0.9598和0.9894,检测限分别为14.82μg·g^(-1)和8.45μg·g^(-1);3个验证样品预测的相对误差分别为11.32%、12.78%、12.48%和7.91%、4.28%、7.64%。由此可知,LIBS技术用于大豆油中重金属Cr的检测具有一定的可行性,松木富集结合内定标法能减少定量分析误差,提高大豆油中Cr含量的预测精度。本研究结果可为食用油中重金属的快速检测提供理论依据。展开更多
采用共轴双脉冲激光诱导击穿光谱(DP-LIBS)技术对3种植物油中的重金属铬(Cr)含量进行定量分析.对实验配制的24个样品,来用桐木木片对其中的Cr进行富集,烘干后进行LIBS试验.选取Cr I 425.39 ran为定量分析谱线,CN分子谱线(421.49 nm)、C...采用共轴双脉冲激光诱导击穿光谱(DP-LIBS)技术对3种植物油中的重金属铬(Cr)含量进行定量分析.对实验配制的24个样品,来用桐木木片对其中的Cr进行富集,烘干后进行LIBS试验.选取Cr I 425.39 ran为定量分析谱线,CN分子谱线(421.49 nm)、Ca原子谱线(422.64 nm)以及它们谱线强度之和为内标线,分别建立了Cr的基本定标法、单谱线内标法和双谱线内标法的定标曲线,并用验证样品对它们进行检验.研究结果表明,3种植物油的基本定标曲线的拟合度R^2在0.97以上,低浓度验证样品预测的相对误差较大;采用单谱线内定标法时,定标曲线拟合度R^2在0.98以上,验证样品预测的相对误差较基本定标法有所降低;来用双谱线内标时,大豆油、花生油和玉米油的内定标曲线拟合度R^2分别为0.995,0.992和0.996,2个验证样品预测的相对误差分别为12.81%,1.73%,9.19%,6.05%和6.23%,6.69%.由此可见,采用双谱线内标法能有效减小定量分析误差,提高LIBS对植物油中Cr元素的预测能力.展开更多
The research on the application of X-ray diffraction in the quantitative analysis of Chinese medicines is rare. The main reason is that the technical problems related to the internal standard and the selection of quan...The research on the application of X-ray diffraction in the quantitative analysis of Chinese medicines is rare. The main reason is that the technical problems related to the internal standard and the selection of quantitative peaks are not well solved, and the accuracy and precision of the results are not satisfactory. This study employed the concept of mass absorption coefficient based on the internal standard method, and the full spectrum fitting and quantitative methods were used to solve the above technical problems. The sample was blended. the internal standard substance of zinc oxide was fully ground, and tablets were prepared by positive pressure method. Under certain instrumental conditions, the PXRD pattern was obtained by scanning. The percentage of gypsum fibrosum in Xiaokening tablet was obtained by quantitative analysis of full spectrum fitting internal standard by TOPAS software. The method was investigated by methodology. At the same time, the method was compared by ion chromatography, and SPSS software was used to make a significant t test on the results of the two methods. After the investigation, the average standard recovery rate of CaSO4-2H2O was 99.06%(RSD = 3.02%);and the recovery rate for simulated samples was 96.7%. The method had good specificity. After statistical analysis, there was no significant difference between the new PXRD method and the traditional method of ion chromatography.展开更多
文摘为了寻求大豆油中铬(Cr)的快速检测方法,应用激光诱导击穿光谱(LIBS)技术对大豆油中Cr含量进行定量检测研究,采用松木对大豆油样品中的Cr进行富集,并利用双通道光谱仪采集其LIBS光谱信号;选择钙(Ca)422.64 nm为内标线,并以Cr的原子谱线Cr I 425.44 nm、Cr I 427.48 nm、Cr I428.94 nm及3条谱线之和为分析线,应用直接定标法和内定标法分别建立上述分析线的定标曲线。结果表明,Cr I 425.44 nm建立的定标曲线性能最佳,直接定标法和内定标法所建立的定标曲线的拟合度R2分别为0.9598和0.9894,检测限分别为14.82μg·g^(-1)和8.45μg·g^(-1);3个验证样品预测的相对误差分别为11.32%、12.78%、12.48%和7.91%、4.28%、7.64%。由此可知,LIBS技术用于大豆油中重金属Cr的检测具有一定的可行性,松木富集结合内定标法能减少定量分析误差,提高大豆油中Cr含量的预测精度。本研究结果可为食用油中重金属的快速检测提供理论依据。
文摘The research on the application of X-ray diffraction in the quantitative analysis of Chinese medicines is rare. The main reason is that the technical problems related to the internal standard and the selection of quantitative peaks are not well solved, and the accuracy and precision of the results are not satisfactory. This study employed the concept of mass absorption coefficient based on the internal standard method, and the full spectrum fitting and quantitative methods were used to solve the above technical problems. The sample was blended. the internal standard substance of zinc oxide was fully ground, and tablets were prepared by positive pressure method. Under certain instrumental conditions, the PXRD pattern was obtained by scanning. The percentage of gypsum fibrosum in Xiaokening tablet was obtained by quantitative analysis of full spectrum fitting internal standard by TOPAS software. The method was investigated by methodology. At the same time, the method was compared by ion chromatography, and SPSS software was used to make a significant t test on the results of the two methods. After the investigation, the average standard recovery rate of CaSO4-2H2O was 99.06%(RSD = 3.02%);and the recovery rate for simulated samples was 96.7%. The method had good specificity. After statistical analysis, there was no significant difference between the new PXRD method and the traditional method of ion chromatography.
