基于微波消解的ICP-OES/ICP-MS法测定茶叶中30种矿物质元素

本文建立微波消解电感耦合等离子体光谱法/电感耦合等离子体质谱法（ICP-OES/ICP-MS）测定茶叶中矿物质元素的含量,分析和探究某地区茶叶中矿物质元素的组成。ICP-OES测定营养元素,在质量浓度0²00 mg/L范围内线性相关系数处于0.9995¹.0000之间,检出限全部不高于0.05 mg/L;ICP-MS测定重金属元素和稀土元素氧化物总量,在质量浓度0¹00μg/L范围内线性相关系数处于0.9996¹.0000之间,检出限均不高于0.082μg/L。监测了福建地区32个茶叶样品的矿物质元素分布,该方法快速简便、灵敏度高,适合通量测定茶叶样品的元素组成,为科学地评价茶叶中矿物质含量提供数据参考。      

中温大曲制曲过程中金属元素的变化规律研究

利用微波消解结合电感耦合等离子体质谱（ICP-MS）检测的方法测定了中温大曲制作过程中Na、K、As、Pb、Cd、Sn、Ti、Mg、Fe、Cu、Mn、Zn、Ca、Al、Ni、Cr和Ba 17种金属元素的含量,并借助SPSS统计学软件采用t检验分析了曲皮和曲心中对应元素的差异性。结果显示,绝大部分金属元素浓度在大曲发酵过程中含量变化较小,与发酵时间无显著相关性。曲心中的Cu和Fe元素随发酵时间出现显著下降,曲皮中则出现相应上升。曲心中的Zn随着发酵时间出现了上升,曲皮出现相反变化。三种金属元素含量在曲心和曲皮中随发酵时间的不同变化规律可能主要源于发酵过程中厌氧型和好氧型微生物的选择性迁移。      

ICP-OES/ICP-MS法测定罗汉果中46种元素

建立了电感耦合等离子体发射光谱（ICP-OES）/电感耦合等离子体质谱（ICP-MS）测定罗汉果中46种元素的方法。ICP-OES检出限在0.68¹8.10μg/L之间,ICP-MS检出限在0.001⁰.093μg/L之间。此方法的精密度（RSD）处于0.73%⁶.83%之间,回收率介于88.7%¹12.1%。国家标准物质灌木枝叶的检测结果与参考值基本相符。测定结果表明,罗汉果中含有丰富的微量元素,其中含量在2 mg/kg以上的达到13种。本方法快速灵敏,适用于罗汉果中多元素的同时分析。      

电感耦合等离子体质谱法测定复配水分保持剂中的18种杂质元素

建立了电感耦合等离子体质谱法测定复配水分保持剂中Cu、Se和Mn等18种杂质元素的检测方法。复配水分保持剂的主要成分为磷酸盐,质谱分析时基体干扰较严重,但经微波消解后,采用以CH4作为反应气的动态反应池模式能较好地消除质谱基体干扰。方法检出限在0.002~0.084μg/g之间,回收率可达82.3%~104.8%。该法在复配水分保持剂多元素同时测定中可获得良好的灵敏度和准确度。      

云南野生与栽培茯苓中矿质元素含量研究

建立微波消解-电感耦合等离子体质谱法（ICP-MS）测定云南15个产地野生与栽培茯苓菌核中Fe、Mn、Cu、Zn、Co、Li、V、Ba、Cr、As、Cd、Pb等12种矿质元素,探讨茯苓中矿质元素的含量分布特征。采用SPSS 21.0进行主成分分析和相关性分析。结果显示,线性回归方程相关系数r均大于0.9990,检出限范围在0.009¹.035μg/L之间,参考物菠菜（GBW10015）和灌木枝叶（GBW07603）测定值在国家参考标准值范围内,表明该方法准确、可靠。所测样品中含有丰富的矿质元素,栽培种Fe、Mn、Co、V、Cr等元素含量高于野生;野生和栽培菌核中Fe元素含量范围分别为31.8¹08.3、49.7⁸05.6 mg/kg,Mn元素含量分别为5.59³5.6、12.9⁶7.7 mg/kg;Cu、Zn和Ba元素平均含量在1¹0 mg/kg之间;Co、Li、V、As、Cd、Pb、Cr等均小于1 mg/kg,其中As（<0.16 mg/kg）、Cd（<0.03 mg/kg）、Pb（<0.35 mg/kg）等有毒重金属均低于食品安全国家标准、世界卫生组织（WHO）和《中国药典》（2015版）最高限量。第一主成分解释原始数据变量的49.060%,Mn、Fe、V、Li、As、Cr等元素载荷值较大,茯苓中特征元素为Mn、Fe、V、Li、As、Cr。相关性分析显示14对矿质元素呈现显著相关（p<0.05）或极显著相关（p<0.01）。元素在茯苓生长过程中存在内在的相关关系,不同产地样品中元素含量差异显著,可能与降水、温度、生长的土壤环境和生长方式有关。      

南宁市售茶叶重金属含量及健康风险评价

采用电感耦合等离子体质谱(ICP–MS)法测定了南宁市售茶叶中Cu、Zn、Pb、Cd、As、Cr和Ni七种重金属的含量,运用内梅罗综合污染指数对重金属污染水平进行评价,运用靶标危害系数法对重金属人体健康风险进行评估.结果表明:试验方法精密度和准确度都较高,市售茶叶中重金属Cu、Zn、Pb、Cd、As、Cr和Ni的含量差...     

电感耦合等离子体质谱法测定核级海绵锆中痕量硼

硼的存在会严重影响核级海绵锆的中子平衡和反应堆的正常运转,因此,需要准确测定核级海绵锆中痕量硼.在采用电感耦合等离子体质谱法(ICP-MS)测定核级海绵锆中痕量硼时,锆基体干扰比较严重,必须对其进行校正或消除.实验用硝酸和氢氟酸溶解样品,以11B为测定同位素,采用标准加入法克服基体干扰,建立了ICP-MS测定核级海绵锆...     

Speciation of selenium in selenium-enriched seeds,buckwheat (<Emphasis Type="Italic">Fagopyrum esculentum</Emphasis> Moench) and quinoa (<Emphasis Type="Italic">Chenopodium quinoa</Emphasis> Willdenow)

Buckwheat (Fagopyrum esculentum Moench) and quinoa (Chenopodium quinoa Willdenow) are widely used as food ingredients. The nutritional characteristics of these plants, i.e., high contents of proteins and amino acids suggest that selenium (Se) is preserved as selenoamino acid derivatives, in particular, selenomethionine (SeMet) in proteins, similar to selenized yeast. Therefore, buckwheat and quinoa are expected to be a good nutritional source of Se. Selenized buckwheat and quinoa were cultivated on Se-fortified soil using sparingly soluble Se salts, such as barium selenate and barium selenite. Se concentration in the edible parts of these plants was determined, and Se extraction efficiency with enzyme or alkali was evaluated. In addition, the chemical species of Se in the low molecular weight fraction of these plants were determined by HPLC-ICP-MS. Total Se concentrations in the edible parts of selenized buckwheat and quinoa were 170.4 ± 2.9 μg/g and 102.7 ± 2.4 μg/g wet weight, respectively. Thus, these selenized seeds were found to be Se accumulators. The results indicate that Se in selenized buckwheat exists mainly as SeMet, while Se in selenized quinoa exists not only as SeMet but also as selenate (Se(VI)) and non-protein forms.     

炭黑氨基柱净化HPLC-ICP-MS测定黄酒中砷形态及含量

建立了一种同时测定黄酒中亚砷酸根、砷酸根、砷甜菜碱、一甲基砷酸和二甲基砷酸等5种砷形态的高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)分析方法。黄酒经炭黑氨基柱净化,体积分数为10%甲醇水溶液洗脱,采用Hamilton PRP-XIO0阴离子交换色谱柱(4.1 mm×250 mm,10 μm),60 mmol/L硝酸铵梯度洗脱,高效液相色谱分离,电感耦合等离子体质谱进行定性和定量分析。在0.5～20.0 μg/L范围内各砷形态线性良好,相关系数R均＞0.999;加标回收率85%～92%,相对标准偏差(RSD)1.4%～5.2%;5种砷形态的定量限均为0.10 μg/L,检出限均为0.03 μg/L。利用该方法对不同年份、不同企业及不同类型的黄酒进行了检测,该方法适用于黄酒中砷残留的分析检测。     

Quantification of trace elements in raw cow’s milk by inductively coupled plasma mass spectrometry (ICP-MS)

The levels of trace elements are an important component of safety and quality of milk. While certain elements such as chromium are essential at low levels, an excess can result in deleterious effects on human health. International quality control standards for milk are published by the Codex Alimentarious Commission and levels of heavy metals in milk intended for human consumption are routinely monitored. This paper describes a new method for demonstrating the levels of V, Cr, Mn, Sr, Cd and Pb in raw cow’s milk, using an ICP-MS. Samples (n = 24) of raw cow’s milk were collected from dairy farms close to mines in Gauteng and North West Provinces of South Africa. In order to destroy organic matrix, each freeze dried milk sample was mineralised by using a microwave assisted digestion procedure. Concentrations of trace elements in digested milk samples were measured by ICP-MS. A whole milk powder reference material (NIST SRM 8435) was used to evaluate the accuracy of the proposed method. It was found that the levels of V, Cr, Mn, Sr, Cd and Pb obtained using the new method showed concordance with certified values.