Determination of macro and trace element in multivitamins preparations by inductively coupled plasma optical emission spectrometry with slurry sample introduction

A slurry sampling technique has been utilised for elemental analysis of multivitamins preparations using inductively coupled plasma-emission spectrometry (ICP-OES). For results comparison, samples were mineralised. Slurry concentration 0.1–0.2% m/v in 6% v/v HNO₃, was used. The calibration by water standard solutions, slurry standards and standard additions were tested for determination above-mentioned elements in slurries. The method offers good precision for macro elements (RSD ranged from 5% to 10%). For in-home control sample, the measured concentrations are in satisfactory agreement with independent laboratories. For the analysed multivitamin preparations, the found element concentration is compared to amount declared by producer. The concentrations of Ca, Mg, P, K, Fe, Mn, Zn, Cu and Cr, Ni, V were determined in the range 1000–100,000 and 5–50 μg g⁻¹, respectively. The slurry ICP-OES analysis was found to be suitable for quality control monitoring of multivitamin preparations and could be useful as a routine procedure.     

Elemental analysis of flour-based ready-oven foods by slurry sampling inductively coupled plasma optical emission spectrometry

A slurry sampling technique has been utilised for the determination of Na, K, Ca, Mg, S, P, Fe, Mn, Cu and Zn in wheat-flour and flour-based ready-oven foods using ICP-OES and a direct aqueous calibration technique. For 0.1% w/v suspension of flour in 0.1% w/v Triton X-100 and 6% v/v HNO₃, the procedural limits of detection (all in mg kg⁻¹) for Na, K, Mg, Ca, P, S, Fe, Zn, Mn and Cu were 7.51, 61.1, 0.645, 1.59, 5.25, 4.58, 1.50, 1.07, 0.867 and 1.58, respectively. The precision was expressed as the relative standard deviation (RSD) of 5–10% (n = 10) for 0.1% w/v suspension of wheat-flour. The accuracy was confirmed by the analysis of reference materials wheat-flour GBW 08503 and rice flour NIST 1568a.     

Toxic and nutrient elements in yerba mate (Ilex paraguariensis)

Toxic and nutrient elements were investigated in yerba mate (Ilex paraguariensis) from South America. Fifty-four brands of commercialised yerba mate from Argentina, Brazil, Paraguay and Uruguay were analysed for Al, Ba, Ca, Cu, Fe, K, Mg, Mn, P, Sr, and Zn, using inductively coupled plasma optical emission spectrometry (ICP-OES), and Li, Be, Ti, V, Cr, Ni, Co, As, Se, Rb, Mo, Ag, Cd, Sb, La, Ce, Pb, Bi and U using inductively coupled plasma mass spectrometry (ICP-MS). Antimony, Se, Ag and Bi were not detected in any sample whereas the limits of detection (LODs) of these elements were 0.19, 0.40, 0.003 and 0.001 μg g^?1, respectively. Analysis of variance (ANOVA) revealed that the concentrations of Cd, Ti, Ni, As, Mo, U, Li and Be in yerba mate were not statistically different with regard to the country of origin, while those of the other investigated elements differed.     

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。      

多方法测定明胶中铬含量

为了比较明胶中铬含量多种测定方法的优劣性和适用性,分别采用二苯碳酰二肼分光光度法、火焰原子吸收法、石墨炉原子吸收法、电感耦等离子体原子发射光谱法和电感耦合等离子体质谱对特殊样品A和B、实际样品进行测定。结果表明,分光光度法、火焰原子吸收光谱法会受样品中铬元素存在形态的影响,而导致测定结果的不准确;石墨炉原子吸收光谱法、电感耦等离子体原子发射光谱法和电感耦合等离子体质谱法有较好的检出限,不受干扰,稳定性能满足检测要求,准确度好,相互间测定结果的对照良好,均可在日常检测中使用。     

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。      

微波消解—ICP-OES/ICP-MS法测定桂花中46种元素

为建立采用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)测定桂花中46种元素的方法。将样品经HNO_3—H_2O_2微波消解后,以ICP-OES测定桂花中Na、Mg、Al、P、S、K、Ca和Fe,ICP-MS测定桂花中Ag、As、Ba、Cd、Co、Cr、Cs、Cu、Hg、Li、Mn、Mo、Ni、Pb、Rb、Se、Sn、Sr、Th、Ti、Tl、V、Zn和15种稀土元素。结果表明:ICP-OES检出限为0.68~18.10μg/L,ICP-MS检出限为0.001~0.093μg/L。方法精密度(RSD)为0.84%~8.42%,回收率为87.2%~113.6%。国家标准物质灌木枝叶[GBW07603(GSV-2)]的检测结果与参考值基本一致。桂花测定结果表明桂花中富含多种微量元素,其中含量在10mg/kg以上的有13种。测定的元素中含量较高的有益元素为Na、Mg、P、S、K、Ca、Fe和Zn,而含量较高的有害元素有Al、Ni、Ba和Pb。该方法具有快速、简便、准确等优点,适用于桂花中多种元素的同时测定。     

酱香型白酒中金属元素的分析研究

采用电感耦合等离子体光度发射光谱法（ICP-OES）和电感耦合等离子体质谱法（ICP-MS）测定酱香型白酒中的常量金属元素、重金属元素及稀土元素。结果表明,茅河酒中铝（Al）、钡（Ba）、锌（Zn）、镍（Ni）、铈（Ce）含量相对较高,分别为17.37 mg/L、19.20 μg/L、21.41 μg/L、27.25 μg/L、2.72 μg/L;茅渡酒中钙（Ca）、钡（Ba）、锌（Zn）、锶（Sr）、铈（Ce）含量相对较高,分别为12.21 mg/L、12.30 μg/L、53.03 μg/L、14.37 μg/L、2.01 μg/L;两种酒中均未检测出铕（Eu）、铽（Tb）。回收率实验结果表明,常量金属元素回收率为96.91%～107.80%,相对标准偏差（RSD）为2.1%～2.9%;重金属元素回收率为80.0%～109.0%,RSD为2.3%～3.9%。表明ICP-OES和ICP-MS法准确度高,采用该方法测定白酒中的金属元素是可行的。     

微波消解结合ICP-OES和ICP-MS测定奇亚籽中多种矿物质元素的含量

建立奇亚籽中K (钾)、Na (钠)、Ca (钙)、Mg (镁)、Fe (铁)、Mn (锰)、Zn (锌)、Cu (铜)、P (磷)、B (硼)、Pb (铅)、Cd (镉)、As (砷)、Cr (铬)、Al (铝)、Ni (镍)16种矿物质元素的方法。样品经微波消解,以电感耦合等离子发射光谱(ICP-OES)测定K、Na、Ca、Mg、Fe、Mn、Zn、Cu、P、B含量,电感耦合等离子质谱(ICP-MS)测定Pb、Cd、As、Cr、Al、Ni含量。结果表明,此方法的ICP-OES检出限范围在0.00850~0.10200 mg/L,定量限范围在0.0283~0.3400 mg/L;ICP-MS检出限范围在0.00471~0.11330 mg/L,定量限范围在0.0157~0.3777 mg/L。线性相关系数均为r＞0.999,加标回收率为90.4%~99.8%,相对标准偏差为0~4.1%。同时用国家标准物质大米(GBW10045(GSB-1))和小麦(GBW10011(GSB-2))评价了方法的准确性,测定结果在标准值范围内。奇亚籽中含有丰富的P、K、Ca、Mg,其中P含量最高,为6860 μg/g,Ca含量为4085 μg/g,K含量为2798 μg/g,Mg含量为2515 μg/g;Fe、Zn、Al、Mn、Cu、Na、B含量(由高到低)在5~100 μg/g。同时检测出重金属危害元素Pb、Cd、Cr、Ni,其中Pb含量符合食品安全国家标准GB 2762-2017的限量要求,未能检测出As。该方法污染小、简便、高效、准确度高,适用于奇亚籽等植物类样品中多种化学元素的测定。     

The cryogenic grinding as the important homogenization step in analysis of inconsistent food samples

Some homogenisation approaches have been investigated to make easier and overcome troublesome preparation of inconsistent food samples. Contents of Na, Ca, Mg, P, Fe, Mn and Zn in muesli, seed and instant food samples were determined by inductively coupled plasma optical emission spectrometry after their grinding with an agate mortar, a kitchen coffee grinder and a cryogenic mill.     

Improvement of a sample preparation procedure for multi-elemental determination in Brazil nuts by ICP-OES

Various sample preparation procedures, such as common wet digestions and alternatives based on solubilisation in aqua regia or tetramethyl ammonium hydroxide, were compared for the determination of the total Ba, Ca, Cr, Cd, Cu, Fe, Mg, Mn, Ni, P, Pb, Se, Sr and Zn contents in Brazil nuts using inductively coupled plasma optical emission spectrometry (ICP-OES). For measurement of Se, a hydride generation technique was used. The performance of these procedures was measured in terms of precision, accuracy and limits of detection of the elements. It was found that solubilisation in aqua regia gave the best results, i.e. limits of detection from 0.60 to 41.9 ng ml^?1, precision of 1.0–3.9% and accuracy better than 5%. External calibration with simple standard solutions could be applied for the analysis. The proposed procedure is simple, reduces sample handling, and minimises the time and reagent consumption. Thus, this can be a vital alternative to traditional sample treatment approaches based on the total digestion with concentrated reagents. A phenomenon resulting from levels of Ba, Se and Sr in Brazil nuts was also discussed.     

Elemental fingerprint of wines from the protected designation of origin Valencia

Inductively coupled plasma optical emission (ICP-OES), in combination with different chemometric approaches, has been used to verify the origin of different red wine samples from Utiel-Requena, Jumilla, Yecla and Valencia protected designation of origin (PDO). The ability of multivariate analysis methods, such as hierarchical cluster analysis (HCA), principal component analysis (PCA), classification and regression trees (CARTs) and discriminant analysis (DA), to achieve wine classification from their elemental contents has been investigated. The calculations were performed using 38 variables (contents of Al, Ba, Be, Ca, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu, Fe, Gd, Ho, K, La, Li, Lu, Mg, Mn, Mo, Na, Nd, Ni, Pb, Pr, Sc, Se, Sm, Sr, Tb, Ti, Tm, V, Y, Yb and Zn, at mg l⁻¹ level, determined by ICP-OES).     

元素含量分析应用于进口四产区香米产地鉴别

利用元素分析建立四个产地香米的鉴别方法。利用电感耦合等离子体质谱法和电感耦合等离子体光谱法对来自泰国、越南、柬埔寨、巴基斯坦四个地区的220份香米进行包括钙、铁、钾、镁、锌、硼、铝、铬、锰、钴、镍、铜、砷、锶、硒、镉、铯、钡、铅19种元素在内的含量分析。通过判别分析建立判别模型。判别模型自校验交叉校验准确率100%,拥有极高的准确率。     

糖尿病住院患者营养状况评价和分析

目的:用NRS2002评价糖尿病患者的营养状况,分析影响糖尿病患者营养状况的可能危险因素。方法:以2012年7月—2013年6月在航天中心医院住院治疗的糖尿病患者为研究对象,入院后用NRS2002对其进行营养评价,记录其饮食、体重变化及入院后首次血清白蛋白(ALB)值。结果:178例糖尿病住院患者中,NRS2002≥3分者53例,占29.8%;其中3例(5.7%)BMI18.5kg/m2,10例(18.9%)ALB≤35g/L。24例(13.5%)患者出现不同程度的体质量减轻;3例(1.7%)患者出现食量大幅度下降。性别与BMI分布有关(P=0.001),男性超重比例远高于女性(P0.001)。糖尿病患者有无合并症与BMI分布也有关(P0.001),有合并症的糖尿病患者超重和肥胖的比例较高(P0.001)。年龄与糖尿病患者是否有合并症有关(P=0.002),45岁的糖尿病患者合并症比例较少,60岁的糖尿病患者合并症比例较高。结论:NRS2002适用于糖尿病患者营养风险筛查;糖尿病人超重和肥胖比例较高,老年糖尿病患者有合并症的比例较高;应加强糖尿病患者营养健康宣教及干预。     

Chemical composition and characterisation of seeds from two varieties (pure and hybrid) of Aesculus hippocastanum

Investigations have been conducted on some samples of naturally desiccated horse-chestnuts (Aesculus hippocastanum), representative of the two most common mediterranean varieties: the pure species (AHP, giving white flowers), and a hybrid (AHH, giving pink flowers). Different experimental techniques have been used to gain more information on morphological structure and chemical composition of these complex matrices. Surface analysis by SEM showed no differences in such floured samples (wild type), while thermal behaviour (DSC) outlines some significant differences between them. Chemical composition reveals some differences in residual moisture (AHP = 6.97%; AHH = 6.59%), proteins (AHP = 2.64%; AHH = 1.82%), lipids (AHP = 4.13%; AHH = 5.10%), glucides (AHP = 15.2%; AHH = 14.3%), and ashes (AHP = 2.51%; AHH = 2.19%). Most likely, these characters modulate other undifferentiated chemical parameters, such as cold water solubility (CWS:AHP = 53.9%; AHH = 48.6%), and total inorganic soluble salts (TISS:AHP = 2.18%; AHH = 1.92%). Principal component analysis was applied to differentiate the two horse-chestnuts varieties. In particular, the first principal component effectively distinguish and discriminates AHH and AHP samples in two well-separated categories, giving, at the same time, some information on the influence of the whole set of chemical compositional parameters.     

黑小麦营养成分分析及其深加工制品前景展望

对漯珍一号黑小麦（secalecerealeL）作了蛋白质、氨基酸及矿物元素等方面的营养素分析,结果表明：黑小麦蛋白质含量高,达17%,氨基酸种类齐全、比例模式优于普通小麦,必需氨基酸含量高,特别是赖氨酸含量比普通小麦高60%,提高了黑小麦蛋白质的质量;黑小麦矿质元素丰富,Fe、Mn、Mg、K、Ca、Zn等元素分别比普通小麦高1348.6%、460.9%、152%、137.4%、89.4%和45%。黑小麦为高蛋白、低脂肪、高纤维、低热能的新型食品加工原料,其开发前景广阔。     

Multivariate analyses of major and trace elements in 19 species of herbs consumed in Yunnan,China

This study aimed to analyze the concentrations of 10 elements in 19 species of herbs related to medical and edible purpose in Yunnan, China. Microwave-assisted acid digestion was used for all of the dried herbs and element contents were determined by inductively coupled plasma atomic emission spectrometry. The accuracy of this method was validated by analyzing GBW07605 certified reference material. The results indicated that the distributions of element contents were varied over a wide range in the specimens tested. The decreasing sequence of average element content expressed as dry weight was presented as follows: calcium (1740–22,246 µg/g dry weight), magnesium (634–6367 µg/g dry weight), iron (52.8–5707 µg/g dry weight), barium (9.19–465 µg/g dry weight), zinc (10.7–82.1 µg/g dry weight), strontium (8.25–69.8 µg/g dry weight), copper (4.10–36.6 µg/g dry weight), chromium (0.26–13.3 µg/g dry weight), nickel (0.57–14.7 µg/g dry weight), and cadmium (0.11–2.66 µg/g dry weight). The element contents of samples were different depending on several species. However, the accumulations of toxic elements (cadmium, chromium, and nickel) were above the international safety standards limit in most samples. Principal component analysis generated three principal components that explained 77% of the total variance in the data. Similar samples may get together by cluster analysis and could correspond to the result of principal component analysis.