【摘要】 目的:建立测定藏药二十五味珊瑚丸中5种重金属含量的方法,并考察西藏不同地区5个厂家生产的该药品中重金属含量情况。方法:以浓硝酸-高氯酸(4∶1,V/V)消解二十五味珊瑚丸样品,采用火焰原子吸收分光光度法测定其中铜(Cu)、铅(Pb)、镉(Cd)3种重金属元素的含量,氢化物发生原子吸收分光光度法测定其中砷(As)、汞(Hg)2种重金属元素的含量。结果:5种重金属元素含量检测在相应质量浓度范围内线性关系均良好(r均≥0.999 1);Cu、Pb、Cd元素的检测限分别为0.001 6、0.041 2、0.036 3mg/L,定量限分别为0.005 3、0.137 3、0.121 0 mg/L;As、Hg元素的检测限分别为0.325 7、0.692 3μg/L,定量限分别为1.085 7、2.307 7μg/L;精密度试验的RSD均≤5.54%(n=6);稳定性试验的RSD均≤3.79%;重复性试验的RSD均≤3.72%;平均加样回收率为91.34%~110.11%,RSD为0.66%~6.80%(n=6)。含量测定结果显示,5个厂家的样品中Cu含量皆未超标,但Cd、Hg含量均超标;其中还有4个厂家样品中Pb含量超标,2个厂家样品中As含量超标。结论:建立的含量测定方法的准确度、灵敏度较高,且稳定性、重复性较好,适用于二十五味珊瑚丸中5种重金属含量的测定;5个厂家生产样品均在一定程度上存在重金属超标问题。更多还原

【Abstract】 OBJECTIVE:To establish a method for the contents determination of 5 heavy metals in Ershiwuwei shanhu pills,and to investigate the contents of heavy metals in Ershiwuwei shanhu pills produced by 5 manufacturers from different districts of Tibet. METHODS:Ershiwuwei shanhu pills were digested by HNO3-HCl O4(4 ∶ 1,V/V). The contents of 3 heavy metals as Cu,Pb,Cd in samples were measured by flame atomic absorption spectrometry(FAAS). The contents of 2 heavy metals as As,Hg in samples were measured by hydride generation atomic absorption spectrometry(HG-AAS). RESULTS:5 kinds of heavy metals have good linear relationship in the corresponding mass concentration range(all r≥0.999 1). The limits of detection of Cu,Pb,Cd were 0.001 6,0.041 2,0.036 3 mg/L,and the limits of quantitation were 0.005 3,0.137 3,0.121 0 mg/L;the limits of detection of As,Hg were 0.325 7,0.692 3 μ g/L,and the limits of quantitation were 1.085 7,2.307 7 μ g/L. RSDs of precision tests were ≤5.54%(n=6);RSDs of stability tests were all≤3.79%;RSDs of reproducibility tests were ≤3.72%. The average recovery rates were 91.34%-110.11%(RSDs were 0.66%-6.80%,n=6). Results of contents determination showed that the contents of Cu in samples from 5 manufacturers were not out of limits,but the contents of Cd and Hg were all out of limits; the contents of Pb in samples from 4 manufacturers were out of limits,and the contents of As in samples from 2 manufacturers were out of limits. CONCLUSIONS:The established method has good accuracy,sensitivity,stability and reproducibility,and it is suitable for contents determination of 5 heavy metals in Ershiwuwei shanhu pills. To some extent,there is a problem of excessive heavy metals in samples from 5 manufacturers.更多还原