半消解-电感耦合等离子体质谱法测定分心木中锰、铜、锶和钡
Determination of Mn, Cu, Sr and Ba in Diaphragma Juglandis Fructus by Semi-Digestion-ICP-MS
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摘要: 本研究建立了半消解-电感耦合等离子体质谱法测定分心木中锰、铜、锶和钡元素，分析了消解液种类、硝酸体积和消解时间对样品中微量元素回收率的影响。在优化的条件下，各待测元素的标准曲线呈良好的线性关系，相关系数大于0999 8，检出限为0037~011 μg/L，相对标准偏差为045%~299%，平均加标回收率为957%~1093%。使用该方法检测国家标准物质GBW10020柑橘叶，结果均在标准参考值范围内。t检验表明，该方法与微波消解法的测定结果无显著性差异。该方法操作简单、快速、结果准确，可为分心木中微量元素的检测提供方法参考。
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关键词:
- 半消解法 /
- 分心木 /
- 电感耦合等离子体质谱法（ICP-MS） /
- 微量元素
Abstract: Diaphragma Juglandis Fructus, the dry wood diaphragm tissue that grows inside the Juglans regia L., has been used for treating many diseases such as kidney asthenia, chronic glomerulonephritis and chronic renal insufficiency. Analytical methods for determination of trace elements in Diaphragma Juglandis Fructus have been reported. The main pretreatment method is wet digestion, which has some shortcomings such as tedious preparation steps, long digestion time and high chemical reagent consumption. Therefore, it is essential to develop an appropriate analytical methodologies for determination of trace elements in Diaphragma Juglandis Fructus. In this work, a method of semidigestioninductively coupled plasma mass spectrometry (ICPMS) was developed for the determination of manganese, copper, strontium and barium trace elements in Diaphragma Juglandis Fructus. In order to get good digestion efficiencies of the target elements, the important factors affecting the semidigestion procedure were discussed, such as nature of acid solution, volume of concentrated nitric acid and digestion time. Finally, 0.2 g Diaphragma Juglandis Fructus sample treated with 2 mL of concentrated nitric acid and then transferred to graphite digestion instrument(120 ℃) for 10 min. Then the digestion solution was filtered by 045 μm polyethersulfone filtration membrane and detected by ICPMS. Results of semidigestion method were compared with those obtained with microwaveassisted digestion as reference method. The results showed that the standard curve of each element has a good linear correlation with a coefficient higher than 0999 8. The detection limits are 0037011 μg/L. The relative standard deviations (RSDs) and average recoveries are in the range of 045%299% and 957%1093%, respectively. The results of national standard substance (GBW 10020 citrus leaf) are all within the standard reference value range. The results of ttest indicated that difference in the results from semidigestion and microwaveassisted digestion is not significant. The method is simple, rapid and accurate, which is suitable for determination of the 4 trace elements in Diaphragma Juglandis Fructus. -
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[1] 国家中医药管理局《中华本草》编委会. 中华本草（第五卷）[M]. 上海：上海科学技术出版社，1999. [2] 赵焕新，景援朝，白虹，王英爱，周洪雷. 分心木中的化学成分及抗氧化活性研究[J]. 中国实验方剂学杂志,2016,22(7):5457.
ZHAO Huanxin, JING Yuanchao, BAI Hong, WANG Ying′ai, ZHOU Honglei. Chemical constituents from Diaphragma Juglandis Fructus and their antioxidant activity[J]. Chinese Journal of Experimental Traditional Medical Formulae, 2016, 22(7): 5457(in Chinese).[3] 高莉，王艳梅，帕提古丽·马合木提. 核桃分心木粗提物抑菌活性的研究[J]. 食品科学,2008,29(11):6971.
GAO Li, WANG Yanmei, PATIGUL Mahmut. Study on antibacterial activities of walnut diaphragm extracts[J]. Food Science, 2008, 29(11): 6971(in Chinese).[4] 王丹，董红敬，杨鹏，王晓，耿岩玲. 分心木中化学成分的分离与鉴定[J]. 食品工业科技,2018,39(14):231234.
WANG Dan, DONG Hongjing, YANG Peng, WANG Xiao, GENG Yanling. Separation and identification of chemical constituents from Diaphragma Juglandis Fructus[J]. Science and Technology of Food Industry, 2018, 39(14): 231234(in Chinese).[5] KRAVCHENKO J, DARRAH T H, MILLER R K, LYERLY H K, VENGOSH A. A review of the health impacts of barium from natural and anthropogenic exposure[J]. Environmental Geochemistry and Health, 2014, 36(4): 797814. [6] MENG Q R, WANG Y Q, CHEN F, XIAO T C, ZHANG L F. Polysaccharides from Diaphragma Juglandis Fructus: extraction optimization, antitumor, and immuneenhancement effects[J]. International Journal of Biological Macromolecules, 2018, 115: 835845. [7] 邵双双，贺亮，韦朝阳，李卫旗. 分心木酸性多糖SJP2的理化性质及其抗氧化活性研究[J]. 食品工业科技,2016,37(5):5963.
SHAO Shuangshuang, HE Liang, WEI Chaoyang, LI Weiqi. Physicochemical properties and antioxidant activity of acid polysaccharide sjp2 from Semen Juglandis[J]. Science and Technology of Food Industry, 2016, 37(5): 5963(in Chinese).[8] 王艳梅，白洁，马木提·库尔班，艾合买提江，帕提古丽·马合木提. 核桃隔膜总黄酮和微量元素的测定[J]. 食品科学,2007(10):477479.
WANG Yanmei, BAI Jie, MAMUT Kurban, AHMATJAN, PATIGUL Mahmut. Determination of total Flavone and microelements from dissepiment of Walnut[J]. Food Science, 2007(10): 477479(in Chinese).[9] 王利，陈晓枫，许雪姣，王静梅. 电感耦合等离子体原子发射光谱测定鱼肉中常见营养元素的样品消解方法[J]. 分析科学学报,2016,32(1):116118.
WANG Li, CHEN Xiaofeng, XU Xuejiao, WANG Jingmei. Comparison of various digestion methods for determination of essential elements in fish by ICPMS[J]. Journal of Analytical Science, 2016, 32(1): 116118(in Chinese).[10] 林洁，黄棉汝，彭乐恺. 半消解混合基体改进剂石墨炉原子吸收法测定生食腌制海产品中铅镉[J]. 中国卫生检验杂志,2014,24(2):185187.
LIN Jie, HUANG Mianru, PENG Lekai. Determination of lead and cadmium in salted aquatic products by GFAAS with mixed matrix modifier after incomplete digestion[J]. Chinese Journal of Health Laboratory Technology, 2014, 24(2): 185187(in Chinese).[11] 金晶，许浩. 半消解电感耦合等离子体发射光谱法测定食品中的镉、铬[J]. 中国卫生检验杂志,2017,27(21):3 0683 070.
JIN Jing, XU Hao. Determination of cadmium and chromium in food by inductively coupled plasma atomic emission spectrometry after incomplete digestion[J]. Chinese Journal of Health Laboratory Technology, 2017, 27(21): 3 0683 070(in Chinese).[12] 王欣美，吴思霖，杨仁康，王珂. 快速湿法消解电感耦合等离子体质谱法同时测定紫菜中铅、砷、汞、镉含量[J]. 中国卫生检验杂志，2018，28(23):2 8352 837.
WANG Xinmei, WU Silin, YANG Renkang, WANG Ke. Simultaneous determination of lead, arsenic, mercury and cadmium in laver by fast wet digestionICPMS[J]. Chinese Journal of Health Laboratory Technology, 2018, 28(23): 2 8352 837(in Chinese).[13] 杨加桂，李先和，张晓天，王颖. 石墨消解电感耦合等离子体质谱法测定海绵钯中18种杂质元素[J]. 冶金分析,2016,36(7):4650.
YANG Jiagui, LI Xianhe, ZHANG Xiaotian, WANG Ying. Determination of eighteen impurity elements in sponge palladium by inductively coupled plasma mass spectrometry with graphite digestion[J]. Metallurgical Analysis, 2016, 36(7): 4650(in Chinese).[14] 黄鑫彦，乐丽欢. 石墨消解法在电感耦合等离子体质谱测定重金属中的运用[J]. 粮食与油脂,2018,31(4):8990.
HUANG Xinyan, LE Lihuan. Application of graphite digestion in determination of heavy metals by inductively coupled plasma mass spectrometry[J]. Cereals and Oils, 2018, 31(4): 8990(in Chinese).[15] 张灵莉，丁玉龙，张美，桂瑞，宁曦，李俊，吴玉萍. 微波消解ICPMS法测定中华白海豚额隆中微量元素及其含量特征分析[J]. 光谱学与光谱分析,2016,36(10):3 3263 331.
ZHANG Lingli, DING Yulong, ZHANG Mei, GUI Rui, NING Xi, LI Jun, WU Yuping. Determination of trace element in the melon of IndoFacific Humpback Dolphins (Sousa Chinensis) with ICPMS[J]. Spectroscopy and Spectral Analysis, 2016, 36(10): 3 3263 331(in Chinese).[16] 赵良成，姜云军，郭秀平，李星，王亦丹，郭小彪，路峰，刘华杰. 电感耦合等离子体发射光谱法/质谱法检测地衣样品中主次微量元素的方法优化[J]. 光谱学与光谱分析,2016,36(10):3 3203 325.
ZHAO Liangcheng, JIANG Yunjun, GUO Xiuping, LI Xing, WANG Yidan, GUO Xiaobiao, LU Feng, LIU Huajie. Optimization of ICPAES and ICPMS techniques for the determination of major, minor and micro elements in lichens[J]. Spectroscopy and Spectral Analysis, 2016, 36(10): 3 3203 325(in Chinese).[17] 曹璨. 微波消解ICPMS法测定中链甘油三酸酯中铜、铅、铬、镍、锡[J]. 质谱学报,2014,35(4):341346.
CAO Can. Determination of Cu, Pb, Cr, Ni and Sn in medium chain triglycerides by microwave digestionICPMS[J]. Journal of Chinese Mass Spectrometry Society, 2014, 35(4): 341346(in Chinese).[18] 刘宏伟，秦宗会，谢华林，曹恕. ICPOES/ICPMS测定葵花子中28种无机元素[J]. 光谱学与光谱分析,2013,33(1):224227.
LIU Hongwei, QIN Zonghui, XIE Hualin, CAO Shu. Study on the determination of 28 inorganic elements in sunflower seeds by ICPOES/ICPMS[J]. Spectroscopy and Spectral Analysis, 2013, 33(1): 224227(in Chinese).[19] 万家亮，曾胜年，李俊义. 分析化学[M]. 北京：高等教育出版社，2001. -
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