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采用HNO3+HCl预消解、HNO3+H2O2高压消解,硫脲-抗坏血酸预还原等手段,建立了高压消解-双道氢化物发生-原子荧光光谱同时测定豆科中药材中砷和汞含量的分析方法。讨论并优化了分析测定条件,结果表明:砷和汞的线性范围分别为0—150、0—90.0ng.mL-1,相关系数分别为0.9992、0.9981,检出限分别是0.0879ng.mL-1和0.012ng.mL-1;相对标准偏差(n=6)砷不大于5.17%,汞不大于5.14%。应用于豆科6种中药材砷和汞含量的测定,该方法操作性强、用时短、灵敏度高。
The method of simultaneous determination of arsenic and mercury in leguminous Chinese medicinal materials by high pressure digestion-double hydride generation-atomic fluorescence spectrometry was established by means of HNO3 + HCl pre-digestion, HNO3 + H2O2 autoclaving and thiourea-ascorbic acid pre-reduction. . The analytical conditions were discussed and optimized. The results showed that the linear ranges of arsenic and mercury were 0-150,0-90.0ng.mL-1, the correlation coefficients were 0.9992 and 0.9981, the detection limits were 0.0879ng.mL- 1 and 0.012 ng.mL-1; relative standard deviation (n = 6) arsenic no greater than 5.17%, mercury no greater than 5.14%. The method is applied to the determination of arsenic and mercury in six traditional Chinese medicinal materials of legumes. The method has the advantages of strong operability, short time-use and high sensitivity.