Question

翻译..........................................................................................

样品消解完毕,冷却,缓慢放气,取出消解罐,至160℃电热板上彻底赶酸。用适量超纯水将消解液定容至100mL,定容液直接用于Cu、Zn、Mn、Fe的测定;定容液加入氯化镧至浓度0.5%后,稀释10倍,用于Ca和Mg的测定;定容液加入氯化铯至浓度0.2%后,稀释100倍,用于K的测定。仪器工作条件见表2。
表2 仪器测定条件
2.2.2 校准曲线的绘制

分别准确吸取一定量Fe、Zn、Cu、Mn、Ca、K、Mg等7种金属元素的标准溶液,用超纯水按比例稀释成不同的工作液,依表2选定的工作条件测定吸光度并求得吸光度与浓度关系的一元线性回
3 结果与讨论
3.1 实验结果
3.1.1 2种重楼药材中7种金属元素含量的测定

分别取2种重楼药材消解液各5份,按照2.2.1项下的仪器工作条件对其中的7种金属元素
进行测定,计算5份平行样品液中金属元素含量的平均值,测定结果见表4。由表4可知,滇重楼和华重楼药材中的金属元素含量存在差异。其中滇重楼药材中宏量元素Ca、Mg、K的含量高于华重楼;而华重楼中除了Cu的含量略低于滇重楼外,其他微量元素Fe、Zn、Mn的含量均高于滇重楼。对于宏量元素而言,滇重楼药材中Ca>K>Mg,而华重楼中K>Ca>Mg;对于微量元素而言,2种药材中金属元素的含量组成均为Fe>Zn>Mn>Cu。
3.1.2 加样回收率的测定

为了考察方法的可靠性,在供试样品中分别加入一定量Ca、Mg、K、Fe、Zn、Cu、Mn标准物质进行回收实验,各元素的回收率测定结果见表5。滇重楼和华重楼各元素回收率在92.1%—107.5%之间,相对标准偏差(RSD)小于3%,说明本法稳定、可靠,可用于重楼药材金属元素的含量测定。
3.2 讨论

金属元素的分析测定,其精密度和准确度在较大程度上取决于样品的处理方法,样品处理是分析测定结果是否准确的关键[11]。本实验所测得的结果与已发表文献[6—8]的测定结果相比,滇重楼中各金属元素的含量均接近或超过已报道的测定结果[6,7](如实验测得Fe含量为1112.7μg/g,而王强等的测定结果为318.1μg/g),尤其是明显高于利用传统溶样法所测得的结果[6](如实验测得Ca含量为11351.1μg/g,而王强等的测定结果为5124μg/g),这可能是由于微波消解法处理样品能够进一步提高提取效率,降低样品损失率的原因。而与张金渝等[8]采用湿法硝酸-双氧水对样品进行消解处理的测定结果相比,Mg和Mn的含量略低于该文报道的测定结果,这种差异的存在是样品不同所致,还是样品处理方法差异所造成的结果,仍有待于进一步系统地研究。

Answer 1

Digestion is completed, cooling, slowly deflated, remove the digestion tank, electric panel to 160 ℃ completely catch acid. Ultra-pure water to digestion with the amount of liquid volume to 100mL, the constant volume liquid directly for Cu, Zn, Mn, Fe determination; constant volume liquid added to a concentration of 0.5% lanthanum chloride, the dilution of 10 times for Ca and Determination of Mg; constant volume to a concentration of cesium chloride solution by adding 0.2%, diluted 100 times for K determination. Instrument conditions in Table 2.
Table 2 Determination of condition of apparatus
2.2.2 Calibration Curve

Imbibe a certain amount of Fe, Zn, Cu, Mn, Ca, K, Mg metal elements of 7 standard solution, diluted with ultra pure water in proportion to the work of a different solution, according to Table 2 Determination of the working conditions of selected absorption absorbance and the concentration degree and obtained a linear relationship between back
3 Results and discussion
3.1 Experimental results
3.1.1 two kinds of re-building of 7 herbs Determination of Metal Elements

Were taken two kinds of re-building herbs digestion solution of 5 copies of the instrument in accordance with 2.2.1 working conditions under which the seven kinds of metal elements
Were measured to calculate 5 were parallel to the sample liquid metals, on average, measured results in Table 4. Table 4 shows, yunnanensis and Chinese herbs in the re-building are different metals. One yunnanensis macro elements in Radix Ca, Mg, K were higher than re-building of China; and China in addition to re-floor yunnanensis Cu content slightly lower than outside the building, and other trace elements Fe, Zn, Mn levels were than yunnanensis. For macro elements, the yunnanensis Radix Ca> K> Mg, the re-building in China K> Ca> Mg; for trace elements, the two kinds of medicinal herbs in the composition of the metal content of the elements were Fe> Zn> Mn> Cu.
3.1.2 Determination of recoveries

To examine the reliability of the method, the tested samples were added to a certain amount of Ca, Mg, K, Fe, Zn, Cu, Mn reference materials for recycling experiments, the recovery of the elements measured results in Table 5. Yunnanensis and China re-building the elements of the recovery between 92.1% -107.5%, relative standard deviation (RSD) less than 3%, indicating that this Act stable, reliable, and can be used to re-floor, the determination of metal elements in medicine.
3.2 Discussion

Determination of metal elements, the precision and accuracy to a large extent depends on the sample processing, sample processing is to analyze the key to determine the accuracy of the results of [11]. In this study, the measured results with the published literature [6-8] compared with the measured results, yunnanensis content of each metal elements are close to or exceed the measured results have been reported [6,7] (such as the experimentally measured Fe content was 1112.7μg / g, and the determination of such results Qiang 318.1μg / g), in particular, is significantly higher than those using conventional sample dissolution method measure the results of [6] (such as the experimentally measured Ca content 11351.1μg / g, and the determination of such results Qiang 5124μg / g), which may be due to sample treatment by microwave digestion method to further improve the extraction efficiency, reduce sample loss reasons. And Yu and Zhang [8] using wet nitric acid - hydrogen peroxide digested samples were compared with the measured results, Mg, Mn, slightly lower than the measured results reported in this paper, the existence of this difference is due to a difference samples, differences in sample handling or the result, the system still needs further study.

Answer 2