Elemental analysis of instant soups and seasoning mixtures by ICP–OES

A method for the determination of Na, K, Ca, Mg, P, Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn levels in high saline food products (instant soups and seasoning mixtures) using ICP–OES was developed. The results of the direct determination with multi-elemental water standards were compared with the internal standardisation, the standard addition methods and the allowable limits of the above mentioned elements in food. The method was shown to be sensitive with limits of detection: Na 1.50, K 12, Ca 0.32, Mg 0.13, P 1.1, Cd 0.16, Cr 0.21, Cu 0.32, Fe 0.30, Mn 0.17, Ni 0.42, Pb 2.1 and Zn 0.21 (in mg kg⁻¹). The method exhibited RSD 2–8%.     

Determination of elemental content in solid sweeteners by slurry sampling and ICP OES

Inorganic species (Ca, Cd, Cu, Co, Fe, Mg, Mn, Na, Ni, Pb, Se and Zn) were determined in solid sweeteners by ICP OES without employing a mineralization step. Robust conditions were used in the ICP equipment and the samples were analyzed as aqueous suspensions. The analysis of different kinds of sweeteners showed different concentration profiles. Some samples presented contamination by Cd but, in general, the samples were found to contain Ca, Fe, Mg, Mn, Na and Se in tolerable amounts. The method accuracy was evaluated and recovery values between 90% and 110% were attained for the recovery experiments, the RSD values were lower than 5% in most cases and the method was shown to be adequate for monitoring inorganic elements in this kind of sample.     

Dilute-and-shoot procedure for the determination of mineral constituents in vinegar samples by axially viewed inductively coupled plasma optical emission spectrometry (ICP OES)

Samples of commercial wine vinegar were introduced in an axially viewed inductively coupled plasma optical emission spectrometry instrument (AX-ICP OES) equipped with different sample introduction systems: a cross-flow nebulizer combined with a double-path spray chamber (CF-DP) and cone spray associated with a cyclone spray chamber (CS-CC). Samples of white and red wine vinegar were diluted with water before analysis. Higher magnesium Mg II/Mg I ratios (11 and 10 for CS-CC and CF-DP, respectively) were obtained using a nebulization gas flow rate of 0.6 l min^-1 and an applied power of 1.3 kW. The background equivalent concentrations (BEC) and signal-to-background ratio (SBR) of analytes were improved using scandium (Sc) as the internal standard. The limits of detection (LOD) and limits of quantification (LOQ) for mineral constituents were similar for both introduction systems. Best recoveries values were obtained using a plasma under robust conditions, CS-CC system and Sc as the internal standard. The concentration determined in 13 commercial samples of wine vinegars varied between 0.2 and 3.0, between 0.02 and 0.4, between 8.5 and 100.0, between 0.01 and 0.05, between 27.0 and 540.0, between 4.0 and 79.0, between 0.4 and 10.0, and between 0.01 and 2.0 for aluminium (Al), barium (Ba), calcium (Ca), copper (Cu), potassium (K), magnesium (Mg), manganese (Mn), and zinc (Zn), respectively.     

Optimization of a slurry dispersion method for minerals and trace elements analysis in infant formulae by ICP OES and FAAS

Infant formula developed by manufacturers requires a rigorous control of composition, particularly those elements added routinely in an attempt to mimic the mineral composition of human milk. A total of 97 different types of powdered infant formulae (preterm, adapted starter, adapted follow-up, toddler, specialised and soy-based formulae) commercially available in Spain were studied. It is noteworthy great differences in mineral (Ca, P, Mg) and trace element (Zn, Fe, Cu, Mn) contents found between analysed and listed in label information. The development of a fast, simple and direct slurry method for the determination of these essential micronutrients in infant formula by inductively coupled plasma optical emission spectrometry (ICP OES) and flame atomic absorption spectrometry (FAAS) was performed in order to help in quality control tasks. Infant formula samples were solubilised using different amounts of several different solvents. An addition of 250 μL of a solution 10% tetramethylammonium hydroxide and 25% ammonium hydroxide were required for the accurate quantification of Ca and P, Mg, Zn, Fe, Cu and Mn, respectively. The standard reference material 1549 non-fat milk powder was solubilised to compare the validity of assayed methodology following slurry nebulisation and traditional microwave-assisted acid digestion method. Good agreement of the analytical results by both ICP OES and FAAS, with the certified values was obtained. Method performance parameters (accuracy, precision and methodological detection limits) were determined for studied elements to check the quality and usefulness of the optimised slurry method. The analytical procedure was applied successfully to the analysis of a representative group of infant formulae. Levels of analysed elements were graphically represented, showing an acceptable comparability between slurry and acid-mineralisation method set by linear correlation coefficients and slopes close to the unit. The described simple and slurry method is appropriate, as an attractive alternative, for routine control analysis of added essential elements in infant formulae regardless of predominant protein type used in manufacture.     

Elemental analysis of nutritional preparations by inductively coupled plasma mass and optical emission spectrometry

This paper reports the development and using of ICP-MS and ICP-OES methods for determination of major, minor and trace elements in multivitamin preparations and dietary supplements and, based on results, their classification using multivariate statistical methods.The method was optimised and evaluated with the use of “in-house” reference material, commercial reference materials and spiked samples. Macroelements (Na, K, Ca, Mg, P), microelements (Cu, Fe, Mn, Zn, Se, Cr), toxic elements (As, Cd, Pb, Ni, V) and a whole series of other elements (e.g. REEs, Ti, Au, Pt, Pd, etc.) were detected with excellent limits of detection as well as other procedure parameters suitable for the purpose of the elemental analysis.As for physiologically significant elements, contents were found as follows (mg kg⁻¹): Ca 560-196,000, Mg 308-70,300, Na 289-74,000, K from undetectable to 28,200, Cu 28-1460, P from undetectable to 217,000, Zn 2.1-25,000, Fe 115-39,400, Mn 28-1860, Cr 0.486-26.6, Mo 0.0418-9.88, and Se 0.395-161. It was found out, if compared with recommended daily intakes, that maximally 50% Ca, 37% Mg, 3% K, 20% P, 14% Na, 100% Cu, 160% Mn, 190% Fe, 120% Zn, 24% Cr, 29% Mo and 79% Se can be obtained from one dose. Extreme samples presenting a possible health risk (Ni content nearly 200 mg kg⁻¹) were indicated. Most of the remaining elements (e.g. REEs) were analysed in order to get reference values for nutritional preparation.     

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.     

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.     

Chemometric evaluation of trace metal concentrations in some nuts and seeds

Seventeen trace metals in acid digests of nuts and seeds were determined using inductively coupled plasma-atomic emission spectrometry and inductively coupled plasma-mass spectrometry. The data were subjected to chemometric evaluation using principal component analysis (PCA), linear discriminant analysis (LDA) and cluster analysis (CA) in an attempt to classify the samples. Hazelnuts (raw and dry roasted), almonds (raw and dry roasted), sunflower seeds (black and white), peanuts (raw and dry roasted), cashew nuts, Brazil nuts, walnuts, chickpeas (raw and dry roasted), pumpkin seeds (raw and dry roasted), and pistachio nuts were used as samples. The samples were classified into seven groups by PCA and CA. All group members determined using PCA and CA were found by LDA to be correctly classified in the predicted groups. Interestingly, the chemometric evaluation indicated that the raw and roasted nuts are very close to each other even though some originated from different countries.     

Total antioxidant capacity of spices, dried fruits, nuts, pulses, cereals and sweets consumed in Italy assessed by three different in vitro assays

With the aim to expand the Italian total antioxidant capacity (TAC) database, the TAC values of 11 spices, 5 dried fruits, 7 sweets, 18 cereal products, 5 pulses, and 6 nuts were determined using three different assays and considering the contribution of bound antioxidant compounds in fiber-rich foods (i. e. cereals, legumes, and nuts). Among spices, saffron displayed the highest antioxidant capacity, whereas among dried fruits, prune exhibited the highest value. The TAC values of all the chocolates analyzed were far higher than the other sweet extracts measured. Among cereal products, whole meal buckwheat and wheat bran had the greatest TAC. Among pulses and nuts, broad bean, lentil and walnuts had the highest antioxidant capacity, whereas chickpeas, pine nuts and peanuts were less effective. The contribution of bound phytochemicals to the overall TAC was relevant in cereals as well as in nuts and pulses. The complete TAC database could be utilized to properly investigate the role of dietary antioxidants in disease prevention.     

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.     

Determination of major and minor elements in dairy products through inductively coupled plasma optical emission spectrometry after wet partial digestion and neutron activation analysis

A wet partial digestion procedure using hydrochloric acid was investigated to determine the concentration of Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P and Zn in dairy products by Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES) technique. The results of this partial digestion were satisfactory and no loss of analytes was observed. A comparison of the results obtained from this methodology was carried out with the other results from dry ashing digestion and Instrumental Neutron Activation Analysis (INAA) technique that do not require pre-treatment procedure.     

Rapid assessment of neoformed compounds in nuts and sesame seeds by front-face fluorescence

The potential of a rapid spectral method, based on front-face fluorescence, to monitor lipid neoformed compounds (NFC) during processing of nuts and sesame seeds was investigated. Fluorescence fingerprints were obtained from front-face fluorescence acquisition directly on crushed nuts and sesame seed samples obtained at different stages of processing. Fluorescence was very sensitive to physicochemical changes induced by the heat process, namely roasting. Parallel factor (PARAFAC) analysis of the fluorescence landscapes revealed four main fluorescence profiles in the nuts, and five in the sesame seeds. These were associated with peptidic tryptophan, tocopherols and process derived products. Various regression models between fluorescence spectra and NFC appearing during the process, carboxymethyllysine (CML) and trans fatty acids (tFA) showed good correlations (R > 0.89) and satisfactory prediction errors (RMSECV < 1.67). When applied to indicators of lipid peroxidation, good regression models were also obtained allowing prediction of the pAV (p-anisidine value) and TBARs (thiobarbituric acid reactive substances): R = 0.73 and 0.96 in nuts and sesame seeds, respectively, with prediction errors lower than 0.78. This study demonstrates the interest of front-face fluorescence as a promising tool for quality control of nuts and seeds roasting.     

元素分析-同位素比质谱法测定食醋总碳同位素比值

本文建立了一种利用元素分析-同位素比质谱法(Elemental analyzer-Isotope ratio mass spectrometry,EA-IRMS)测定食醋总碳同位素比值的方法,并对食醋进行聚类分析。优化了样品稀释倍数及进样量。2 g芳香醋用4 m L超纯水进行稀释,2 g糯米酿造食醋用2 m L超纯水进行稀释,苹果醋、配制白醋不稀释,进样量均为1μL,样品分析时间为670 s。结果显示:芳香醋、糯米酿造食醋、苹果醋及配制白醋的δ~(13)C值范围分别为-26.94‰~-23.46‰、-25.06‰~-22.40‰、-27.99‰~-22.76‰、-19.06‰~-13.74‰,聚类分析可将不同产地、不同原料、不同生产方式的食醋进行初步归类,并且该方法可鉴别出芳香醋和掺入≥4%糯米酿造食醋、≥6%苹果醋、≥2%配制白醋的芳香醋混合样品。食醋及质控样品(咖啡因)的测试精度(SD)在0.02‰~0.25‰(n=6)之间,均小于0.3‰,满足方法检测分析要求。结果表明,所建EA-IRMS方法结合聚类分析可用于食醋分类及掺假鉴别。     

微分脉冲催化极谱法及等离子发射光谱法测定奶粉中铬含量

研究了2种测定奶粉中铬含量的方法,微分脉冲催化极谱法和等离子发射光谱法,并对2种方法的特点及存在的问题进行了讨论。     

Compositional analysis and roasting behaviour of gevuina and macadamia nuts

This study compares the composition of macadamia and gevuina nuts following natural abscission and air-drying of intact nuts and compares chemical and sensory properties on roasting gevuina nuts using a reported macadamia roasting process. The markedly higher fat content of macadamia (75% vs. 43%) reflected a higher percentage of protein, moisture, ash and carbohydrate in gevuina nuts. Gevuina nuts also had lower energy and pH values than macadamia. Water activities were similar. Both oils were around 80% monounsaturated, but differed widely in positional isomerism. On roasting, macadamia nuts developed sweet, nutty, buttery notes along with brown colour development (measured using L *, a *, b * values) after 20 min at 135 °C while gevuina nut colour and aroma took at least 30 min, where the aroma was more hazelnut-like. Extractable volatiles were significantly higher for macadamias following roasting.     

Content,composition, and stereochemical characterisation of lignans in berries and seeds

In seed extracts of five oilseed species, in bran extracts of three cereal species, and in seed and/or whole berry extracts of 10 berry species, the concentrations of a large number of lignans and the enantiomeric composition of selected lignans were determined. In the case of sesame and hemp seeds, the lignan content and composition of the whole seeds was compared to that of the hulled seeds. The results showed that cloudberry seeds are the third most lignan-rich food source after linseeds and whole sesame seeds, and that most of the berry species analysed were more lignan-rich than the cereal brans. The lignans are concentrated in the hull of the oilseeds and in the seeds of the berries. In most samples, secoisolarici-, pino-, medio-, and syringaresinol were present as a mixture of two enantiomers.     

我国2016~2019年炒货食品及坚果制品质量安全状况及风险分析

目的 分析2016~2019年我国坚果炒货食品的安全形势。方法 结合2016~2019年国家和各省市场监督管理局公开发布的食品监督抽检信息, 对其不合格项目等信息进行分析。结果 炒货食品及坚果制品的主要不合格项目为品质指标(过氧化值、酸价等)、微生物指标(霉菌、大肠菌群等)和食品添加剂(二氧化硫、糖精钠等),主要不合格种类为花生、瓜子和豆类。酸价和过氧化值主要不合格原因为炒货原料质量不达标、生产过程控制不严、储存条件不当、包装密封性不好; 霉菌和大肠菌群主要不合格原因为原料、包装材料、生产过程中人员卫生、器具等生产设备、环境的污染 、熟制过程中杀菌不彻底; 二氧化硫和糖精钠主要不合格原因为超范围使用食品添加剂和添加量控制不当。结论 建议监管部门完善标准体系、加强原料监管和生产过程控制、严格食品添加剂管理、引导企业建立食品安全可追溯体系和加强企业食品安全意识和责任意识。     

超高效液相色谱—串联质谱法测定炒货中纽甜含量的不确定度评定

建立了一种测定炒货中纽甜含量的不确定度数学模型,分析了整个检测过程中各种不确定度影响因子并进行评定,确定有关分量并合成不确定度。结果表明,当样品中纽甜含量为7.69 mg/kg时,其扩展不确定度为0.71mg/kg(k=2),其中标准储备溶液的配制和测量重复性引入的不确定度影响较大。