原子吸收分光光度法测定藏药二十五味珊瑚丸中5种重金属含量
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篇名: | 原子吸收分光光度法测定藏药二十五味珊瑚丸中5种重金属含量 |
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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 3 mg/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 3 μg/L,定量限分别为1.085 7、2.307 7 μg/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。 |
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-HClO4 (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 μg/L, and the limits of quantitation were 1.085 7, 2.307 7 μg/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. |
期刊: | 2018年第29卷第7期 |
作者: | 刘兰,张勇仓,钟铧,次仁久米,王聚乐 |
AUTHORS: | LIU Lan,ZHANG Yongcang,ZHONG Hua,Cirenjiumi,WANG Jule |
关键字: | 火焰原子吸收分光光度法;氢化物发生原子吸收分光光度法;二十五味珊瑚丸;重金属;含量测定 |
KEYWORDS: | Flame atomic absorption spectrometry; Hydride generation atomic absorption spectrometry; Ershiwuwei shanhu pills; Heavy metals; Content determination |
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