电感耦合等离子体发射光谱法测定食品中聚二甲基硅氧烷的含量

食品样品中的聚二甲基硅氧烷(PDMS)用航空煤油提取,经高速离心净化后,用电感耦合等离子体发射光谱法进行测定,外标法定量。当PDMS在鸡肉、牛肉、猪肉、黄瓜、菠萝样品中添加水平为5.0、10.0mg/kg和100.0mg/kg、在大豆油、花生油、棕榈油样品中添加水平为1.0、2.0mg/kg和10.0mg/kg、在裹粉炸粉样品中添加水平为2.5、5.0mg/kg和10.0mg/kg时,平均回收率为71.2%～122.9%,相对标准偏差小于15.0%,标准曲线在0.1～50.0mg/L之间,r≥0.995,针对动物肌肉和果蔬产品、食用油脂、裹粉的方法检出限分别为5.0、1.0、2.5mg/kg。本方法前处理操作简单,适用基质范围广,能够满足对食品中PDMS的检测要求,适合大量样品的快速、准确定性和定量分析。     

电感耦合等离子发射光谱法同时测定连云港产草莓中的铅铬镉铜

采用干法、湿法及微波消解分别处理5个品种草莓样品,全谱直读电感耦合等离子体原子发射光谱法(ICP-AES)同时测定试样中铅、铬、镉、铜微量元素含量并与国标限量进行比较,同时对方法学进行考察。结果表明,5种草莓品种的重金属含量在国标限量范围内,干法、湿法、微波-ICP-AES的加标回收率分别为85.3%～104.5%、94.3%～104.6%、99.8%～106.3%,除个别值外,RSD均小于20%。可以得出结论,干法、湿法、微波-ICP-AES均适合草莓铅、铬、镉、铜含量的测定,方法简便、准确,精密度好,可用于草莓中铅、铬、镉、铜的快速检测;5种品种草莓中的重金属含量未超标。     

微波消解-电感耦合等离子体发射光谱法测定茶叶中的镉

采用微波消解前处理技术,结合电感耦合等离子体发射光谱法对茶叶中镉元素含量进行测定,并以该方法对随机抽取的绿茶、乌龙茶、茉莉花茶和普洱茶各10个茶样中的镉元素含量进行分析。结果表明：镉标准物质质量浓度在0～100μg/L范围内,线性良好,相关系数R为0.9998,仪器检出限为1.88μg/L;茶样添加标准物质的回收率在95.7%～102.3%之间,茶样中镉元素含量6次重复测定的相对标准偏差为1.1%,方法回收率与精密度都较好,适合茶样中镉的快速测定;随机抽取的40个茶样的镉含量在0.017～0.138mg/kg之间,平均值为0.082mg/kg±0.028mg/kg,其中被检测的绿茶镉含量为0.060mg/kg±0.014mg/kg,乌龙茶为0.098mg/kg±0.027mg/kg,茉莉花茶为0.082mg/kg±0.032mg/kg,普洱茶为0.090mg/kg±0.023mg/kg。绿茶与其余3类茶镉含量的平均值差异显著(P＜0.05)。     

ICP—AES测定卷烟烟气中钾、钠金属离子

建立了全谱直读电感耦合等离子发射光谱法(ICP–AES),同时测定了其中卷烟烟气中钾钠离子的含量。研究了元素分析标准曲线、精准度、回收率以及不同种类烟草样品中两种离子的含量差别。结果表明,在选定的波长下测定,元素间也没有干扰.该方法快速,准确可靠,加标回收率为95~98%,相对标准偏差RSD均小于4%,适用于对卷烟主流烟气的检测。     

电感耦合等离子体原子发射光谱法同时测定江西脐橙中多种微量元素

采用硝酸-高氯酸对江西赣南8个县所产的脐橙样品进行消解,电感耦合等离子体原子发射光谱法(ICP-AES)同时测定试样中Al、As、Ba、B、Ca、Co、Cr、Cu、Fe、K、Li、Mg、Mn、Ni、P、Pb、Zn、Be、Cd、Se、Sr、La、Ce、Y、Sm、Lu等元素的含量。该法的相对标准偏差为0.42%～4.51%,加标回收率为87.7%～114.1%。实验结果表明:脐橙中含有丰富的K、Ca、P和Mg,不同县所产的脐橙各种微量元素含量存在一定差异。     

啤酒中硅的ICP—AES测定

硅钼蓝化学法测定Ｓｉ繁杂费时，湿法消解时，硅又易形成沉淀。我们用ＩＣＰ－ＡＥＳ地啤酒中的Ｓｉ进行直接稀释测定，回收率１０２－１０８％。     

Determination of Metals and Metalloids in Wine Using Inductively Coupled Plasma Optical Emission Spectrometry and Mini-torch

In the present study, an inductively coupled plasma optical emission spectrometer ICPE-9820 with the mini-torch technology that significantly reduces the consumption of plasma gas to 7.0 L min^?1 was applied for the multielemental analysis of wine samples. Three sample preparation procedures (microwave digestion in closed vessels, acid digestion in open vessels in a water bath, both with HNO₃, and 1:10 dilution with deionized water) were compared for the determination of 15 elements in wines. In all wines analyzed, the lowest concentration was obtained for Li (0.06–0.09 mg L^?1) and the highest for K (475–995 mg L^?1). The concentration >1 mg L^?1 of B, Fe, and Na was determined in all wines analyzed by the three sample preparation procedures. The average concentrations found for the acid extracts for Al (1.31 mg L^?1) and Fe (3.40 mg L^?1) were higher in comparison to results of sample dilution (0.73 and 1.56 mg L^?1 respectively). The recoveries were between 88.2 and 110 %, 65.9 and 106 %, and 62.8 and 109 %, whereas the relative standard deviations (RSDs) varied between 0.04 and 4.62 %, 0.74 and 5.57 %, and 0.70 and 5.80 %, respectively, for the procedure of sample dilution, microwave digestion, and water bath digestion.     

ICP测定不锈钢餐厨具中锰含量的不确定度评定

在不锈钢产品的元素成分检测方法中,电感耦合等离子体发射光谱法(ICP)是较常用的一种方法.文章以测定锰含量为例,对该检测方法的不确定度进行了评定,确定了测定过程的不确定度来源,主要有测定全过程的重复性、样品称量、标准曲线、标准溶液、玻璃量具及仪器等.应用了现代数理统计方法对该检测方法中的不确定度分量进行了逐一分析,并得出了总合成不确定度.在不确定度分量中,标准系列和标准溶液对总合成不确定度的影响最大,因此在检测工作中应特别注意标准系列和标准溶液配制的相关操作.     

A Comparison of Mineral Extraction Techniques of Citrus Juices as Analyzed by Inductively Coupled Plasma Atomic Emission Spectrometry

Two methods of mineral extraction for citrus juices were investigated: dry ashing in a muffle furnace and wet ashing in a microwave oven. Elemental concentrations were determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). For reference, a synthetic multielement mixture was prepared and analyzed. Results for the multielement solution using wet ashing in a microwave oven or dry ashing in a muffle furnace differed by less than 10% from those for an undigested, but diluted solution. An exception was boron, of which 96% was lost in the muffle furnace. Grapefruit juice analysis showed differences in concentration of less than 10% for all elements. Orange juice samples, however, showed greater losses for Na (16%), Si (13%), and Sn (11%) with the dry ashing method.     

电感耦合等离子体质谱仪半定量方法在盲样液元素分析中的应用

采用电感耦合等离子体质谱法（ICP-MS）,建立了一种盲样元素分析的半定量检测方法。对合成样品的半定量分析以及对实际样品的加标回收试验结果显示,该方法能够有效消除干扰,快速测定样品中存在的元素及浓度范围,测定结果的偏差为-29.0%～17.0%,加标回收率为-29.0%～17.0%。该方法可应用于盲样元素含量扫描分析,为快速了解盲样元素信息提供科学根据。     

Determination of Inorganic Elements in Teas Using Inductively Coupled Plasma Optical Emission Spectrometry and Classification with Exploratory Analysis

Multivariate optimization was employed to obtain the best conditions of the inductively coupled optical emission spectrometer (ICP OES) (nebulization gas flow rate of 0.47 L min^?1 and applied power of 1.36 kW) for the determination of Al, Ba, Ca, Cu, Fe, K, Mg, Na, and Mn in 27 green tea samples. In the hierarchical cluster analysis, it was possible to observe the formation of five different groups (imported Japanese samples, samples without specifications, organically cultivated samples, samples in capsules, and ready-to-drink iced tea samples) besides the separation according to brand. In the principal component analysis we verified that the first four main components explained 99.98 % of the total variance. The ICP OES technique and the exploratory analysis were shown effective tools that can be used jointly in the quality control and classification of green tea samples.     

电感耦合等离子体原子发射光谱法同时测定鼠曲草中九种微量元素

选择硝酸-过氧化氢作消解液,采用湿法消解法对鼠曲草（全草）进行消化处理,探究了消解液用量、消解时间、酸度影响和离子干扰等条件。用ICP-AES法测定其中铜、锌、铅、铁、镉、镍、铬、砷、锰9种元素。该法加标回收率为95.0%～110.0%,检出限为0.427～2.28μg/L,RSD<6%。利用该方法分析了茶树叶标准物质（GBW08513）的9种金属元素,测定结果与标准值一致。实验结果表明该法耗样少,准确度高,快速,测定结果令人满意。      

电感耦合等离子体原子发射光谱法同时测定鼠曲草中九种微量元素

选择硝酸-过氧化氢作消解液,采用湿法消解法对鼠曲草(全草)进行消化处理,探究了消解液用量、消解时间、酸度影响和离子干扰等条件.用ICP-AES法测定其中铜、锌、铅、铁、镉、镍、铬、砷、锰9种元素.该法加标回收率为95.0％ ～ 110.0％,检出限为0.427～2.28μg/L,RSD＜ 6％.利用该方法分析了茶树叶标准物质(GBW08513)的9种金属元素,测定结果与标准值一致.实验结果表明该法耗样少,准确度高,快速,测定结果令人满意.     

电感耦合等离子体质谱仪测定皮革中铬含量

用电感耦合等离子体质谱仪ICP-MS测定皮革中的铬含量,选择测定同位素52Cr与53Cr,其结果出现了差异,探讨了52Cr与53Cr测定结果出现差异的原因及解决方法,经过校正后,52Cr与53Cr测定结果满足了一致性的要求。     

电感耦合等离子体原子发射光谱法测定凉粉草不同部位中22 种无机元素的含量

为测定凉粉草根、枝和叶中无机元素的含量,采用HNO3-H2O2消解体系,通过微波消解彻底有效地消解样品中的有机物,应用电感耦合等离子体原子发射光谱法测定Al、As、Ag、Ba、Bi、Ca等22 种无机元素含量。结果表明,在优化条件下,待测各元素间相互干扰较小,22 种元素在一定范围具有良好的线性关系,相关系数（r）均不小于0.999 6,检出限范围为0.000 1～0.019 0 μg/mL,平均回收率为98.9%～103.4%,相对标准偏差为0.7%～5.2%（n=6）。实验方法快速、简便、准确、灵敏度高,能够准确测定凉粉草不同部位中22 种无机元素含量。     

ICP-OES法测定方便面中微量元素的研究

采用微波辅助消解样品,建立了轴向观测电感耦合等离子体发射光谱(ICP-OES)法同时测定方便面中Na、Mg、Al、K、Ca、Mn、Fe、Cu、Zn、Mo、Cd、Ba等12种微量元素的分析方法。确定了仪器的最佳工作条件,选择了各待测元素合适的分析谱线,采用Y为内标元素消除了测定过程中的干扰。结果表明方法的检出限为0.16～18.15μg/L,采用硬质小麦标准物质NIST 8436进行方法验证,结果准确可信。该法具有准确度高,精密度好等优点,可用于方便面的质量控制和安全评价。     

ICP-OES法测定密蒙花中多种元素

建立电感耦合等离子体发射光谱法测定密蒙花中Na、Mg、P、K、Ca、Mn、Fe、Cu、Zn、Sr人体必需元素和Ni、As、Cd、Pb毒理性元素的分析方法。样品经（硝酸＋双氧水）密闭微波消解后用超纯水稀释后进行测定,确定各待测元素的分析波长,通过加入内标元素Y补偿待测元素分析信号的漂移,校正基体效应,改善分析信号的稳定性。在选定的操作条件下,各待测元素的检出限在0.011～25.16 μg/L之间,利用标准参考物质（NIST SRM 1515）验证分析方法的准确度和精密度,结果表明,标准物质的分析结果与参考值基本一致,相对标准偏差为2.0%～8.3%。方法简便、快速、准确,能实现密蒙花中多元素的快速分析。     

Development of an Analytical Method for the Combined Determination of Water-Soluble Vitamins and Minerals Through High-Performance Liquid Chromatography–Inductively Coupled Plasma Atomic Emission Spectrometry Hyphenation

The capabilities of inductively coupled plasma atomic emission spectrometry (ICP-AES) for the determination of water-soluble vitamins after high-performance liquid chromatography (HPLC) separation have been evaluated for the first time in the present work. Thanks to the multielemental capability of ICP-AES, it has been possible to develop a method for the joint determination of several water-soluble vitamins and minerals. The vitamin chromatograms were obtained by plotting the carbon corrected emission intensity against time. Meanwhile, minerals were determined through the measurement of the emission intensity at their characteristic wavelengths. The established method was applied to the determination of thiamine, riboflavin, pantothenic acid, nicotinamide, ascorbic acid, Cr, Mo, Se, Mn, Zn, Fe, Mg, Ca, and K in multivitamin complexes. Good linearities were obtained, with correlation coefficients above 0.999 for all the vitamins and metals. The detection limits using ICP-AES for vitamins were lower than 10 mg L⁻¹ except for biotin (18 mg L⁻¹) and ascorbic acid (35 mg L⁻¹). Moreover, the limits of detection for metals ranged from 0.3 mg L⁻¹ for K and 0.02 mg L⁻¹ for Mo. Even though the ICP is less sensitive than PDA and MS for vitamin determination, the HPLC-ICP-AES allows determination of vitamins and minerals in a period of time not much higher than that required for the simple determination of the minerals, and it is less sensitive to interferences in trace quantities.     

微波消解_ICP-AES法同时测定膨化食品中的铅、铝、砷

建立快速消解并同时测定膨化食品中铅,铝,砷的检测方法。通过微波消解法进行前处理,用电感耦合等离子体发射光谱仪(ICP-AES)进行测定。方法简便,快速,准确,灵敏度高。对于所测元素,校正曲线的相关系数达0.999 0以上,回收率范围为90.2%～102.7%,相对标准偏差1.85%～8.35%。膨化食品中的铅,铝,砷可用微波消解ICP-AES法同时测定,适合检测行业对膨化食品的日常检验。     

微波消解/ICP-AES法测定蔬菜中重金属含量

采用微波消解处理样品,以电感耦合等离子体发射光谱(ICP-AES)法测定8 种蔬菜中的Zn、Pb、Cu、Cd 4 种重金属元素的含量。结果表明：此方法的检出限为0.006～0.018μg/mL,相对标准偏差0.17%～1.76%,加标回收率为99.00%～102.95%。叶类蔬菜吸收重金属的能力比茄果类蔬菜强。ICP-AES 法测定蔬菜中重金属元素的含量具有快速、灵敏、准确性较好的优点。