Raman spectroscopy based analysis of milk using random forest classification

The development of a classification system based on the Raman spectra of milk samples is proposed in present study. Such development could be useful for nutritionists in suggesting healthy food to infants for their proper growth. Previously, molecular structures in milk samples have been exploited by Raman spectroscopy. In the current study, Raman spectral data of milk samples of different species is utilized for multi-class classification using a dimensionality reduction technique in combination with random forest (RF) classifier. Quantitative and experimental analysis is based on locally collected milk samples of different species including cow, buffalo, goat and human. This classification is based on the variations (different concentrations of the components present in milk such as proteins, milk fats, lactose etc.) in the intensities of Raman peaks of milk samples. Principal component analysis (PCA) is used as a dimensionality reduction technique in combination with RF to highlight the variations which can differentiate the Raman spectra of milk samples from different species. The proposed technique has demonstrated sufficient potential to be used for differentiation between milk samples of different species as the average accuracy of about 93.7%, precision of about 94%, specificity of about 97% and sensitivity of about 93% has been achieved.     

Trace elements in food reference materials: compositional and analytical perspectives

Selection criteria for production of food reference materials need to simultaneously consider realistic proximate matrix compositions, emerging trends for the nutritional and toxicological effects of less-emphasized trace elements (e.g., B, Li, Si, and V), chemical speciation (especially for As, Hg, Se, and Sn), and analyte certification requirements from the analyst's point of view. For the most part, currently available Certified Reference Materials (CRMs) do not meet many of these needs. Candidate CRMs with relevant concentrations of trace elements could be chosen from similar foods with different proximate compositions (e.g., fat content of milk products, meat, or soya flour). Explicit guidance must accompany CRMs so that variations in measured trace element concentrations arising from procedural lapses and basis weight are avoided.     

Selenium and vitamin E concentrations in human milk and formula milk from Hungary

The metabolic roles of vitamin E and selenium are closely related, and to a very great extent, each can compensate for the deficiency of the other. The aim of the study was to determine and compare the Se and vitamin E (α- and γ-tocopherol) contents of breast milk and commercially available infant formulas in Hungary. The Se content was measured by instrumental neutron activation analysis (INAA), while the α-, and γ-tocopherol concentrations were determined by high performance liquid chromatography (HPLC). The mean Se concentration was 17.4±2.8 μg/L in transitional and 13.8±2.3 μg/L in mature milk. It was found that, all of the starter (ST), the follow-on (FO) and the specialized formulas (SF) had lower Se content than breast milk. Transitional breast milk resulted in a higher Se intake (14 μg/day) than mature milk (11 μg/day). The daily Se intakes in Hungarian infants were within the Recommended Dietary Allowance (RDA) range. The natural vitamin E contents of human milk were similar during the early and late lactation. Mature breast milk had 3.30±1.13 mg/L α-TE concentration and this was significantly higher than that of in ST (1.98±1.57), and FO (1.77±0.78), or in SF ready to feed preparations (1.03±0.74). The present study suggests that the formulas for the optimal development of young infants, should contain concentrations of these antioxidants on a level which is comparable to that of the human milk.     

A study of some trace elements in infant foods

Seven trace elements were determined in milk formulas, powder milk and infant food. Instrumental neutron activation analysis was used for the analysis of Fe, Zn, Co, Cr and Rb, while As and Cu content was determined using radiochemical neutron activation analysis. Differences were found in the trace element content of foods of the same type. Milk formulas are comparable with human milk according to the results obtained for the elements analyzed. The samples of powder cow's milk presented similar concentrations of the elements studied. Liver with vegetables was found to have the highest Cu content. A meal prepared at home, made of beef and fresh vegetables showed a higher trace element content than its similar commercial one. An estimation of the daily intake of the elements analyzed was made and compared with minimum recommended daily ingestion.     

1152例婴儿血中6种元素检测结果的分析

为探讨婴儿体内铜、锌、钙、镁、铁和铅微量元素的含量及其与年龄、性别的关系,测定了1 152例湖南长沙地区1岁内婴儿指末梢全血中6种元素铜、锌、钙、镁、铁和铅的含量,对其结果进行了统计分析。结果表明,所测婴儿元素铁、锌缺乏最显著,其次是钙缺乏;铜、镁无明显失衡;血铅超标的水平较低;不同性别之间6种元素含量的差异无统计学意义。提示在长沙地区的孕婴保健中,应加强锌、钙与铁的合理补充。     

Automated on-line column-switching HPLC-MS/MS method with peak focusing for measuring parabens, triclosan, and other environmental phenols in human milk

Parabens (esters of p-hydroxybenzoic acid) and triclosan are widely used as preservatives and antimicrobial agents, respectively, in personal care products, pharmaceuticals, and food processing. Because of their widespread use and potential risk to human health, assessing human exposure to these compounds in breastfed infants is of interest. We developed a sensitive method, using a unique on-line solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry system with peak focusing feature, to measure in human milk the concentrations of five parabens (methyl-, ethyl-, propyl-, butyl-, and benzyl parabens), triclosan, and six other environmental phenols: bisphenol A (BPA); ortho-phenylphenol (OPP); 2,4-dichlorophenol; 2,5-dichlorophenol; 2,4,5-trichlorophenol; and 2-hydroxy-4-methoxybenzophenone (BP-3). The method, validated by use of breast milk pooled samples, shows good reproducibility (inter-day coefficient of variations ranging from 3.5% to 16.3%) and accuracy (spiked recoveries ranging from 84% to 119% at four spiking levels). The detection limits for most of the analytes are below 1 ng mL(-1) in 100 microL of milk. We tested the usefulness of the method by measuring the concentrations of these twelve compounds in four human milk samples. We detected methyl paraben, propyl paraben, triclosan, BPA, OPP, and BP-3 in some of the samples tested. The free species of these compounds appear to be the most prevalent in milk. Nevertheless, to demonstrate the utility of these measures for exposure and risk assessment purposes, additional data about sampling and storage of the milk, and on the stability of the analytes in milk, are needed.     

Determination of Mineral Elements in Milk Products by Inductively Coupled Plasma-Optical Emission Spectrometry

The determination of mineral elements in milk products is of great importance since their excess or deficiency may affect human health. In this study, calcium, magnesium, potassium, sodium, phosphorus, and iron were determined in milk products from South Korea. The samples were wet-digested by microwave-assisted combustion using nitric acid and hydrogen peroxide, and analyzed by inductively coupled plasma-optical emission spectrometry. The method was validated by sensitivity, linearity, precision, recovery checks, and the analysis of a milk powder certified reference material. The elemental concentrations were similar in the milk products. Calcium and potassium were the most abundant, followed by phosphorus, sodium, magnesium, and iron. All concentrations were comparable to previous values and were within the limits of recommended dietary allowances and tolerable upper levels.     

A quantitative and comprehensive method to analyze human milk oligosaccharide structures in the urine and feces of infants

Human milk oligosaccharides (HMOs), though non-nutritive to the infant, shape the intestinal microbiota and protect against pathogens during early growth and development. Infant formulas with added galacto-oligosaccharides have been developed to mimic the beneficial effects of HMOs. Premature infants have an immature immune system and a leaky gut and are thus highly susceptible to opportunistic infections. A method employing nanoflow liquid chromatography time-of-flight mass spectrometry (MS) is presented to simultaneously identify and quantify HMOs in the feces and urine of infants, of which 75 HMOs have previously been fully structurally elucidated. Matrix-assisted laser desorption/ionization Fourier transform ion cyclotron resonance MS was employed for high-resolution and rapid compositional profiling. To demonstrate this novel method, samples from mother–infant dyads as well as samples from infants receiving infant formula fortified with dietary galacto-oligosaccharides or probiotic bifidobacteria were analyzed. Ingested oligosaccharides are demonstrated in high abundance in the infant feces and urine. While the method was developed to examine specimens from preterm infants, it is of general utility and can be used to monitor oligosaccharide consumption and utilization in term infants, children, and adults. This method may therefore provide diagnostic and therapeutic opportunities.

Capillary electrophoresis of acidic oligosaccharides from human milk

Interest in defining the array of oligosaccharides of human milk has been increasing. Pathogens that bind glycans on their host mucosal surfaces may be inhibited by human milk oligosaccharides. It has been postulated that acidic oligosaccharides in human milk may inhibit binding by pathogens that bind acidic glycans in the gut, but testing this hypothesis requires their reliable quantification in milk. Sialyloligosaccharides of human milk have been quantified by HPLC and CE. A recent CE technique uses the MEKC mode with direct detection at 205 nm to resolve and quantify, in the native form, the 12 most dominant sialyloligosaccharides of human milk in a single 35-min run. The method gives a linear response from 39 to 2500 microg/mL with a coefficient of variation between 2 to 9% and accuracy from 93 to 109%. This was used to detect variation in expression of specific sialyloligosaccharides in milk. Individual sialyloligosaccharide concentrations in milk differ among individual donors and between less and more mature milk. Thus, CE can be used to measure variation in sialyloligosaccharide expression in milk, and thereby test the relationship of this variation-to-variation in risk of specific diseases in breastfed infants.     

Detection of milk oligosaccharides in plasma of infants

Human milk oligosaccharides (HMO) are one of the major components of human milk. HMO are non-digestible by the human gut, where they are known to play important functions as prebiotics and decoys for binding pathogens. Moreover, it has been proposed that HMO may provide sialic acids to the infant that are important in brain development, however this would require absorption of HMO into the bloodstream. HMO have consistently been found in the urine of humans and other mammals, suggesting systemic absorption. Here, we present a procedure for the profiling of milk oligosaccharides (MO) in plasma samples obtained from 13 term infants hospitalized for surgery for congenital heart disease. The method comprises protein denaturation, oligosaccharide reduction, and porous graphitized carbon solid phase extraction for purification followed by analysis using nHPLC-PGC-chip-TOF-MS. Approximately 15 free MO were typically observed in the plasma of human infants, including LNT, LDFP, LNFT, 3′SL, 6′SL, 3′SLN, and 6′SLN, of which the presence was confirmed using fragmentation studies. A novel third isomer of SLN, not found in human or bovine milk was also consistently detected. Differences in the free MO profiles were observed between infants that were totally formula-fed and infants that received at least some part breast milk. Our results indicate that free MO similar in structure to those found in human milk and urine are present in the blood of infants. The method and results presented here will facilitate further research toward the possible roles of free MO in the development of the infant.     

Comparative measurements of mineral elements in milk powders with laser-induced breakdown spectroscopy and inductively coupled plasma atomic emission spectroscopy

Mineral elements contained in commercially available milk powders, including seven infant formulae and one adult milk, were analyzed with inductively coupled plasma atomic emission spectrometry (ICP-AES) and laser-induced breakdown spectroscopy (LIBS). The purpose of this work was, through a direct comparison of the analytical results, to provide an assessment of the performance of LIBS, and especially of the procedure of calibration-free LIBS (CF-LIBS), to deal with organic compounds such as milk powders. In our experiments, the matrix effect was clearly observed affecting the analytical results each time laser ablation was employed for sampling. Such effect was in addition directly observed by determining the physical parameters of the plasmas induced on the different samples. The CF-LIBS procedure was implemented to deduce the concentrations of Mg and K with Ca as the internal reference element. Quantitative analytical results with CF-LIBS were validated with ICP-AES measurements and nominal concentrations specified for commercial milks. The obtained good results with the CF-LIBS procedure demonstrate its capacity to take into account the difference in physical parameters of the plasma in the calculation of the concentrations of mineral elements, which allows a significant reduction of the matrix effect related to laser ablation. We finally discuss the way to optimize the implementation of the CF-LIBS procedure for the analysis of mineral elements in organic materials.     

Multielemental analysis of Brazilian milk powder and bread samples by neutron activation

The concentrations of Na, Cl, Mn, Br, Fe, Zn, Rb, Sb, Sc, Cr, Al and Mg were determined in some types of bread and in some brands of milk powder consumed in the city of São Paulo (SP—Brasil), by instrumental neutron activation analysis. Radiochemical separations were carried out by means of retention of²⁴Na on hydrated antimony pentoxide (HAP) from a 8N HCl solution, after digestion of the organic matter. It was possible in this way to determine the radioisotopes⁶⁴Cu,^69mZn and¹⁴⁰La in the effluent solution. The detection limits of the trace elements analyzed in bread and milk powder samples were determined using the Currie and Girardi criterions.From a dissertation submitted by V. A. MAIHARA to the University of São Paulo in partial fullfillment of the requirements for a Master of Science Degree in Nuclear Technology.     

Determination of Lead and Cadmium in Milk by Electrothermal Atomic Absorption Spectophotometry

Abstract

The concentrations of lead and cadmium in different kinds of milk samples (powdered, infant formula, market, buffalo, condensed and human) were determined using electrothermal atomic absorption spectrophotometric technique. Among all the varieties of milk analysed, condensed milk was found to contain much higher amount of lead. Human milk as expected was found to have lowest concentration of these elements. The results were compared with the reported values of other countries. Daily intake of these toxic elements by adults and babies up to the age of six months through the consumption of various types of milk was estimated and compared with the tolerance levels.     

Characterization of Brazilian commercial milks by instrumental neutron activation analysis

Aiming at the determination of toxic and essential elements in Brazilian commercial bovine milk, 25 ultra high temperature (UHT) milk samples were acquired in the local market of Piracicaba, SP. The samples were freeze-dried and analyzed by instrumental neutron activation analysis (INAA) allowing the determination of Br, Ca, Co, Cs, Fe, K, Na, Rb and Zn. When the results were expressed as concentration (mg·l⁻¹) no significant differences were found. However, considering the dry matter, results showed a clear difference between the mass fractions (mg·kg⁻¹ d.w.) of skim milk and whole milk for the elements Br, Ca, K, Na, Rb and Zn, indicating that the removal of fat caused a concentration effect in the dry matter of skim milks. Discrepancies were found between the concentrations of Ca and Na measured by INAA and the values informed in the labels. Ca showed variations within 30% for most samples, while concentrations of Na were up to 190% higher than informed values. The sample preparation and the INAA procedure were appropriate for the determination of Br, Ca, Co, Cs, Fe, K, Na, Rb and Zn in milk samples.     

Study of the Nutritional Status of Maternal Breast Milk in Preterm Infants in Nigeria

Instrumental neutron activation analysis (INAA) and proton induced X-ray emission (PIXE) analysis were used to determine the concentration of 13 elements in the breast milk collected within the first week of lactation and after morning feed from 16 pre-term mothers and 20 term mothers. The results of the study show that pre-term milk has a significantly higher concentration of Cl, Cu, Fe, K, Mg, Mn, Na and Zn while term mothers have a significantly higher concentration of P and Br. No significant differences were, however, found in the mean concentration of Al, Ca, I and Rb. Furthermore, the mean concentration for most of the elements found in the breast milk fall within the range of the concentrations obtained for the commercial infant milk formulae.     

Variations in trace element concentrations in breast milk with stages of lactation

The influence of stages of lactation on the mineral and trace elementconcentrations of breast milk collected from 20 healthy lactating women ina Nigeria population was investigated using instrumental neutron activationanalysis (INAA) and proton induced X-ray emission (PIXE) analysis. The breastmilk samples were divided into colostrum (day 1–5), transitional (day6–13) and mature milk (day 14–28). The result of the study showthat colostrum milk has a significantly higher mean concentration of Ca, Cl,Cu, Fe, Mg, Na and Zn than the transitional and mature milk. Furthermore,the mean concentrations of Fe, Mg, Na and Zn in transitional milk were foundto be significantly higher when compared with the mature milk. It was alsoobserved from the semi-log plot of the concentration of the elements againstdays of lactation that the concentration of all the elements decreased significantlythroughout the lactation period studied with Cu, Fe and Zn concentration showingthe greatest decline, particularly in the early stages of lactation.     

Modified Baby Milk—Bioelements Composition and Toxic Elements Contamination

Breast milk has the most suitable composition for the proper development in the first year of a child’s life. However, it is often replaced with artificial milk. The aim of the study was to analyze the composition of essential elements: Na, K, Ca, P, Mg, Fe, Zn, Cu, and Mn as well as toxic elements: Ni, Pb, Sr, Li, and In in 18 formulas available in Poland. The daily supply was also estimated. The study was performed by Inductively Coupled Plasma Optical Emission Spectrometry method. The results showed the presence of all essential elements tested, but the content of P and Mn significantly differed from the concentrations declared. Such discrepancies can have significant impact on the daily dose of the bioelements taken. However, the content of elements was within the reference standards established by the EU Directive with exception of P, the amount of which exceeded the norms 5.23–18.80-times. Daily supply of P in tested milk as well as Fe and Mn provided with first and hypoallergenic formula exceeded the adequate intake. Analysis revealed the contamination with harmful elements—Pb, Sr, Li, and In were detected in almost all products. The study confirms the data concerning some discrepancies in composition and the contamination of food and may provide information on the feeding quality of children and estimation of health risk associated with exposure to toxic elements.     

Determination of elemental concentrations in environmental plant samples by instrumental neutron activation analysis

The intake of leafy vegetables in daily diet is very important to meet our nutritional needs. Vegetables provide the essential elements which are necessary and recommended for human growth. However, due to rapid industrialization and urbanization our environment becomes polluted and this affects the normal growth of agricultural products and composition of environmental species. The elemental concentrations present in the environmental samples are good indicators to assess the toxicological levels due to pollution affects. In the present work we have analysed several vegetable plant samples by instrumental neutron activation analysis to determine the elemental concentrations at major, minor and trace levels. The leafy vegetables like spinach, red leafy veagetable, pui, gourd leaf, lettuce and katoua were chosen as these are extensively consumed by local peple in eastern part of India. We have determined 15 elements in the above mentioned vegetable samples and some of these are essential elements and some are toxic elements. It was found that Na and K were present as major elements, Fe and Zn as minor elements and As, Ce, Cr, Co, La, Mo, Rb, Sc, Sm, Sr as trace elements. The concentration level of Cr was found to be higher than that of recommended value certified by WHO and National environment quality control for human consumption. The validation of our analytical results have been performed by the Z-score tests through the determination of concentrations of the elements of interest in certified reference materials.     

Relationship among iodine, bromine and chlorine concentrations in cow's milk in Japan

In order to know the relationship among some elements in biological materials, iodine, bromine and chlorine concentrations in cow's milk samples in Japan were determined by the thermal neutron activation analysis using a low power research reactor and a Van de Graaff accelerator. The iodine contents in cow's milk samples ranged from 0.041 to 0.316 ppm with an average of 0.096 ppm. The bromine and chlorine in these samples ranged from 2.3 to 11.1 ppm and from 475 to 1650 ppm, respectively. The average concentration of the bromine was calculated to be 5.6 ppm and that of the chlorine was 853 ppm. The relationship among iodine, bromine and chlorine concentrations in cow's milk samples in Japan was studied with a regression analysis. It was suggested that the correlation has a power function as follows; Y = K(Z)-A where, Y is elemental concentration in ppm, Z is atomic weight [corrected] of element, A (= 7.4) is exponent and K (= 14.7) is a constant.