A Comparative Study of Selected Trace Element Content in Malay and Chinese Traditional Herbal Medicine (THM) Using an Inductively Coupled Plasma-Mass Spectrometer (ICP-MS)

A total of 60 products of traditional herbal medicine (THM) in various dosage forms of herbal preparation were analyzed to determine selected trace elements (i.e., Zn, Mn, Cu, Cd, and Se) using ICP-MS. Thirty types of both Chinese and Malay THMs were chosen to represent each population. The closed vessel acid microwave digestion method, using CEM MARS 5, was employed for the extraction of the selected trace elements. The digestion method applied was validated by using certified reference material from the Trace Element in Spinach Leaves (SRM1570a). The recoveries of all elements were found to be in the range of 85.3%–98.9%. The results indicated that Zn, Mn, Cu, Cd and Se have their own trends of concentrations in all samples studied. The daily intake concentrations of the elements were in the following order: Mn > Zn > Cu > Se > Cd. Concentrations of all five elements were found to be dominant in Chinese THMs. The essentiality of the selected trace elements was also assessed, based on the recommended daily allowance (RDA), adequate intake (AI) and the United States Pharmacopeia (USP) for trace elements as reference. The concentrations of all elements studied were below the RDA, AI and USP values, which fall within the essential concentration range, except for cadmium.     

电感耦合等离子体质谱法高纯镍粉中18种杂质元素含量的测定

建立了一种高纯镍中18种杂质元素电感耦合等离子体质谱测定方法,通过加入内标元素Sc、Rh、Tm,有效的消除了测定中的基体效应,仪器的检出限为0.03-0.22ng/ml,加标回收率为85％-107％,相对标准偏差均小于5％.该方法能够满足高纯镍粉中杂质的测定.     

Distribution Coefficients of 60 Elements on Cation and Anion-Exchange Resin in Ammonium Chloride Solutions

ABSTRACT

Ammonium chloride is a widely available non-corrosive and non-toxic chemical. When in contact with protein NH₄Cl is non-destructive and allows softer conditions for labeling of organic substances. These properties make NH₄Cl appropriate for use in multiple areas such as pharmaceutical production, low-background research, etc. For such purposes, a multitude of pure elements could be applied. In order to obtain pure elements their separation (purification) is necessary. One of the most successful methods of elements separation is ion exchange. In this work, we study the distribution coefficient of 60 elements on anion exchange (Dowex 1-x8) and cation exchange (Dowex 50w-x8) resins with NH₄Cl solutions with varying concentrations via ICP-MS.     

Isotope dilution inductively coupled plasma mass spectrometry for determination of 126Sn content in spent nuclear fuel sample

The ¹²⁶Sn content in a spent nuclear fuel solution was determined by isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS) for its inventory estimation in high-level radioactive waste. A well-characterized irradiated UO₂ fuel sample dissolved in a hot cell was used as a sample to evaluate the reliability of the methodology. Prior to the ICP-MS measurement, Sn was separated from Te (¹²⁶Te), which causes major isobaric interference in the determination of ¹²⁶Sn content, along with highly radioactive coexisting elements, such as Sr (⁹⁰Sr), Y (⁹⁰Y), Cs (¹³⁷Cs) and Ba (^137m Ba), using an anion-exchange column. The absence of counts attributed to Te at m/z = 125, 128, and 130 in the Sn-containing effluent (Sn fraction) indicates that Te was completely removed from the anion-exchange column. After washing, Sn retained on the column was readily eluted with 1 M HNO₃ accompanied with approximately 80% of the Cd and 0.03% of the U in the initial sample. Owing to the presences of Cd and U in Sn fraction, the measurements of ¹¹⁶Sn and ¹¹⁹Sn were affected by the isobaric ¹¹⁶Cd and the doubly charged ²³⁸U²⁺ion, resulting in the positive bias of the determined values. With the exception of the isotopic ratios including ¹¹⁶Sn and ¹¹⁹Sn, ¹¹⁷Sn/¹²⁶Sn, ¹¹⁸Sn/¹²⁶Sn, ¹²⁰Sn/¹²⁶Sn, ¹²²Sn/¹²⁶Sn and ¹²⁴Sn/¹²⁶Sn were successfully determined and showed good agreement with those obtained through ORIGEN2 calculations. The measured concentration of ¹²⁶Sn in the spent nuclear fuel sample solution was 0.74 ± 0.14 ng/g, which corresponds to 23.0 ± 4.5 ng per gram of the irradiated UO₂ fuel (excluding the presence of ¹²⁶Sn in the insoluble residue). The results reported in this paper are the first experimental values of ¹²⁶Sn content and isotope ratios in the spent nuclear fuel solution originating in spent nuclear fuel irradiated at a nuclear power plant in Japan.     

小试金-碲保护留铅灰吹富集测定矿石中痕量贵金属

采用小铅试金富集,以5 mg碲为灰吹保护剂,通过留铅灰吹法将矿石样品中痕量贵金属(金、铂、钯、铑、铱和钌)定量富集在50 mg左右的铅合粒中。铅合粒先以(1+1)硝酸溶解,再加入盐酸进一步增强溶解能力,基体通过以氯化铅形式沉淀得以分离,采用电感耦合等离子体质谱法(ICP-MS)测定。相对标准偏差(RSD,n=6)为:Au 4.6%、Pt 8.7%、Pd 4.5%、Rh 9.2%、Ir 6.1%、Ru 5.8%。方法用于国家一级标准物质和黑色页岩样品中痕量贵金属的测定,测定值与认定值基本吻合。     

ICP-MS测定钢中痕量元素Mn、Ti、Mo

建立了ICP-MS测定钢中锰、钛、钼的分析方法。实验优化了仪器的工作参数,选择了适合锰、钛、钼测定的功率、雾化气、辅助气、冷却气等仪器条件,讨论了基体效应等对测定元素信号的影响和消除。锰、钛、钼的质量浓度在0～100 ng/mL范围内有良好的线性关系,相关系数在0.999%以上,测定范围为0.000 01%～0.01%,本方法准确、快速、简便。     

ICP-MS法测定香精中重金属的不确定度研究

建立利用微波消解-ICP-MS检测香精中重金属的方法,并根据JJF1059-1999《测量不确定度评价与表示》对该方法进行不确定度分析。以重金属锑为例建立数学模型,包括对称重、标准溶液配制、实验人员、环境等因素引入的不确定度进行分析。其中在方法的不确定度评定过程中,应主要考虑不确定度贡献较大的分量,从而简化实验操作步骤,提高工作效率。在置信区间为95%时,k=2,得出不确定度结果为UC=56.10μg/kg,测量结果报告表示为：c=（492.13±56.10）μg/kg。     

ICP-MS测定水稻不同部位6种元素含量

把水稻植株的稻米、谷壳、根、茎叶四个部位进行预处理,湿法消解后,ICP-MS测定Cr、Cd、Pb、Co、Mo、V等6种元素含量。实验结果表明：Cr主要集中在谷壳中;Cd、Pb、Co、V主要集中在水稻植株根部;Mo在糙米中的含量最高。该测定方法对各元素的检出限为0.001~0.025 mg/kg,加标回收率为93.3%~102.5%。对国家标准物质大米（GBW 10010）的分析结果与所给的标准值吻合,方法准确可靠,结果满意。     

ICP-OES法测定高纯石英粉中金属杂质

研究建立用等离子发射光谱法直接测定石英粉中7种金属杂质元素的方法,试验了相关实验条件,所测元素回收率96％～103％,精密度为0.16％～1.34％.     

ICP-MS法测定化妆品中汞的干扰现象分析及消除

分析并消除以电感耦合等离子体质谱（ICP-MS）法测定化妆品中汞含量时干扰因素对结果的影响。考察了不同质量数对测定结果的影响,采用204作为汞测定质量数,测定化妆品中的汞含量,有效消除了质谱型干扰,加样回收率为100.4%-104.2%。测定结果用冷原子吸收法加以验证,结果满意。