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Rapid Determination of Mercury in Native Chinese Herbal Medicine by Hydride Generation-Atomic Fluorescence Spectrometry with Aqua Regia-Hydrogen Peroxide Heat Extraction
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摘要: 采用王水-过氧化氢预氧化水浴热浸提处理样品, 应用原子荧光光谱法快速检测原生中草药中痕量汞.其方法回收率在98.6%~105.4%之间, 相对标准偏差在3.0%~7.4%之间, 标准系列质量浓度在0.000~6.000μg/L范围内线性关系良好, 相关系数为0.9999, 一元线性回归方程为:IF=301.512C+1.235, 方法检出限达到0.0216μg/L.试验证实, 方法具有简便、快速、灵敏度高、取样量少等优点, 为原生中草药中痕量汞的检测提供了有效的分析方法.Abstract: A method for the rapid determination of trace mercury in Chinese herbal medicine by hydride generation-atomic fluorescence spectrometry is established. The samples were dissolved by aqua regia-hydrogen peroxide oxidation in a hot water bath, the recoveries were 98.6%~105.4%, the relative standard deviations were 3.0%~7.4%, when the concentration of standard series in the range of 0.000~6.000 μg/L, the standard curve liner relationship was good, the correlation coefficient was 0.999 9, the linear regression equation was: IF=301.512C+1.235, the detection limit of the method was 0.021 6 μg/L. The method is simple, rapid, highly sensitive with less sample quantity, the method is effective for the analysis of trace amount of mercury in native Chinese herbal medicine.
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Key words:
- heat extraction /
- atomic fluorescence spectrometry /
- Chinese herbal medicine /
- mercury
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表 1 间歇泵进样程序
Table 1. Program of pump intermittent sampling
进样步骤 时间/s 泵转速/rpm 读数 1 4 0 No 2 5 100 No 3 4 0 No 4 11 120 Yes 5 0 0 No 
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表 2 精密度试验结果
Table 2. Results of precision test
样品编号 测定质量分数/(μg/kg) 测定次数 平均质量分数/ (μg/kg) 标准偏差 相对标准偏差/% 2010T003-28 27.4、26.0、26.2、25.3、26.7 5 26.3 0.79 3.0 2010T003-44 12.9、13.5、12.3、13.1、14.9 5 13.3 0.98 7.4
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表 3 方法回收率
Table 3. Recovery of the method
样品编号 样品质量分数/(μg/kg) 加标质量分数/(μg/kg) 测得质量分数/(μg/kg) 回收率/% 2010T003-11 6.71 15.5 22.0 98.6 2010T003-49 10.2 5.00 15.3 102.0 2010T003-78 1.05 1.50 2.61 104.0 GBW07604 26±3 / 27.4 105.4
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表 4 样品与标准物质分析结果
Table 4. Contents of samples and control of standard material
(μg/kg) 样品编码 样品名称 实测质量分数 标准值 2010T003-11 中草药 6.71 / 2010T003-28 中草药 26.3 / 2010T003-44 中草药 13.3 / 2010T003-78 中草药 1.24 / GBW07604 杨树叶 27.4 26±3 GBW07605 茶叶 14.2 (13)
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