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[1]张志刚.中药材汞含量的光谱法测定[J].武汉工程大学学报,2013,(10):28-31.[doi:103969/jissn16742869201310006]
　ZHANG Zhi\|gang.Analysis of mercury content in Chinese herbal medicines by using mercury vaporizer unit\|cold atom absorption spectrometry[J].Journal of Wuhan Institute of Technology,2013,(10):28-31.[doi:103969/jissn16742869201310006]
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中药材汞含量的光谱法测定(/HTML)
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《武汉工程大学学报》[ISSN:1674-2869/CN:42-1779/TQ]

卷:
期数:
2013年10期
页码:
28-31
栏目:
化学与化学工程
出版日期:
2013-11-10

文章信息/Info

Title:
Analysis of mercury content in Chinese herbal medicines by using mercury vaporizer unit\|cold atom absorption spectrometry
文章编号:
16742869(2013)10002804
作者:
张志刚
九州通医药集团湖北金贵中药饮片有限公司，湖北 武汉 430051
Author(s):
ZHANG Zhi\|gang
Hubei Jingui Chinese Herbal Pieces Company of Jointown Pharmaceutical Group, Wuhan 430051,China
关键词:
黄连; 苍术; 菊花; 汞; 消化; 水银发生器; 冷原子吸收
Keywords:
goldthread;  rhizoma atractylodis;  chrysanthemum;  mercury;  digestion;  mercury vaporizer unit;  cold atom absorption
分类号:
R917
DOI:
103969/jissn16742869201310006
文献标志码:
A
摘要:
取3 g药材粉末到250 毫升的具塞锥形瓶中，加65%硝酸\|70%高氯酸（9∶1）溶液100 毫升，再加0.05%重铬酸钾\|浓硝酸溶液1毫升，盖上塞子，浸泡过夜.拔掉塞子，将其放在电热板上加热，保持微沸，反复加入65%硝酸\|70%高氯酸（9∶1）适量，直至溶液变为无色透明.当蒸发后的消化液剩余40毫升左右时停止加热，冷却后用20%氢氧化钠中和酸.将样品过滤,结果显示：检出限为0.005 微克/升，线性范围为0~500 微克/升，相关系数为0.999 5，精密度为2.0%，回收率为98.0%.2%的硝酸浓度对实验稳定，能减少氯化亚锡的使用量，对实验无干扰；用20%氢氧化钠中和酸能减少氯化亚锡的使用量，减少实验干扰，避免加热消化过程中消化液局部温度过高汞的损失；保持微沸也是实验的操作要点.单一使用硝酸难以达到消化效果；加入总量10%的高氯酸后能显著提高消化效果；加入少量重铬酸钾能提高汞的还原能力.
Abstract:
Three gram traditional Chinese medicinal materials powders of Goldthread, Rhizoma atractylodis and Chrysanthemum were poured into a 250 mL conical flask with a plug, then 100 mL solution with 65% nitric acid -70% perchloric acid（9∶1）and 1mL 0.05% potassium bichromate\|nitric acid were poured into the conical flask. With the plug plugged, the powders were soaked for a night. With the solution boiling, the plug was pulled up and the conical flask was heated on an electric hot plate. An appropriate amount of 65%nitric acid\|70%perchloric acid（9∶1）was kept being added to the digested sample solution until the sample solution became colorless and transparent. The heating was finished when the digested solution was left about 40 mL.Acid was neutralized by 20% sodium hydroxide after the digested solution became cold, and then the neutralized solution was filtrated. Results show that detecting limit is 0.005 μg/L, linearity range of Hg is 0~500 μg/L, correlation coefficient is 0.999 5, precision is 2.0%, and recovery ratio is 98.0%; 2% nitric acid is stable for experiment, which can reduce usage amount of stannous chloride without interfering experiment; usage of 20% sodium hydroxide can reduce usage amount of stannous chloride and interference of experiment, and avoid loss of mercury as a result of local temperature of digested solution being too high during the heating process; micro\|boiling is also a key point of experiment operation. The single use of 65% nitric acid is difficult to achieve digestion effect; 70% perchloric acid with the content of 10% can significantly improve digestion effect; adding a little potassium bichromate can raise reducing capacity of mercury.

参考文献/References:

\[1\]蔡慧华，彭速标．痕量汞的测定方法进展\[J\]．理化检验\|化学分册， 2008（44）：385\|390.CAI Hui\|hua, PENG Su\|biao．Progress of methods for Determination of Trace amounts of mercury\[J\]．Physical Testing and Chemical Analysis\|chemical part， 2008（44）：385\|390.\[2\]阎海鱼，冯新斌．半封闭溶样冷原子荧光测定鱼体中总汞分析方法的建立\[J\]．地球与环境，2005，33(2)：89\|92.YAN Hai\|yu,FENG Xin\|bin．A methodological Development in measuring total mercury in fish using\|closed digestion and cvafs\[J\]．Earth and environment，2005，33(2)：89\|92.\[3\]杨莉丽，李娜．蒸气发生\|冷原子荧光光谱法测定中草药中不同形态的汞\[J\]．光谱学与光谱分析，2005，25(2)：286\|289.YANG Li\|li,LI Na．Speciation analysis of mercury intraditional Chinese medicine by vapor\|generation atomic fluorescence spectrometry\[J\]．Spectroscopy and spectral analysis，2005，25(2)：286\|289.

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备注/Memo

备注/Memo:
收稿日期：20130314作者简介：张志刚（1979\|），男，湖北蕲春人，高级工程师.研究方向：中药质量研究.
更新日期/Last Update: 2013-11-11