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作 者:胡军华[1,2] 刘威[1,2] 仲海洁 李家春[1,2] 钱俊[1,2] 黄文哲[1,2] 王振中[1,2] 萧伟[1,2]
机构地区:[1]江苏康缘药业股份有限公司,江苏连云港222001 [2]中药制药过程新技术国家重点实验室,江苏连云港222001
出 处:《中国中药杂志》2015年第4期649-653,共5页China Journal of Chinese Materia Medica
基 金:国家"重大新药创制"科技重大专项(2013ZX09402203)
摘 要:采用电感耦合等离子体质谱法(ICP-MS),建立六味地黄多糖部位中锂(Li)、铍(Be)、硼(B)、钛(Ti)、镁(Mg)、铝(Al)、钒(V)、铬(Cr)、钴(Co)、锰(Mn)、铁(Fe)、镍(Ni)、铜(Cu)、锌(Zn)、镓(Ga)、砷(As)、锶(Sr)、镉(Cd)、锡(Sn)、锑(Sb)、钡(Ba)、汞(Hg)、铊(Tl)、铅(Pb)和铋(Bi)共25种重金属及微量元素的测定方法,并对其中Al,Fe,Mg,B,Ti,Mn,Zn,Sr,Ba共9种微量元素进行了水及不同醇浓度浸出率的研究.样品经微波消解后,以锗(Ge),铟(In)为内标,以灌木枝叶标准药材作为质控标准物质,用ICP-MS进行测定.各元素的检出限在0.007~2.225 μgL-1;精密度RSD≤4.0%;回收率在84.1%~116%.不同溶剂提取时微量元素的浸出率有较大差异. 该方法操作简便,分析速度快,灵敏度高,各项分析性能指标均达到要求,适用于六味地黄多糖部位微量元素的测定,溶出特性的研究结果为多糖部位微量元素形态的研究提供一定的指导 意义.A method was established for the simultaneous analysis of 25 trace elements and heavy metals in polysccharides from Liuwei Dihuang prescription, including Li, Be, B, Ti, Mg, Al, V, Cr, Mn, Co, Fe, Ni, Cu, Zn, Ga, As, Sr, Cd, Sn, Sb, Ba, Hg, Tl, Pb, Bi. The different rate of elemental extraction in Al, Fe, Mg, B, Ti, Mn, Zn, Sr, Ba was made in water and different concentration of alcohol. The samples, digested via microwave, calibrated by internal standard elements such as Ge and In, with bush branches and leaves as the controlled reference standard, were inlet into ICP-MS to analyze the contents of the 24 trace elements and heavy metals. The detection limits of the 24 elements were in the range of 0.007-2.225 μgL-1, while the RSD was below ≤4.0%,with their recovery ranging from 84.1% to 116%. Big different of the elemental extraction rates could be found by using different ethanol solutions. The method is simple, rapid and accurate,and can be used for the quality control of trace elements and heavy metals in Liuwei Dihuang polysccharides. With the aid of the obtained result, we may increase the extraction of necessary element while making an attempt at multi-element speciation in polysccharides from Liuwei Dihuang.keywords:polysccharides from Liuwei Dihuang
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