Methods of analysis for toxic elements in food products. 2. Review of USSR standards on determinations of heavy metals and arsenic

Methods of analysis prescribed by USSR standards for Hg, Pb, Zn, As, Cd, Cu, Fe, and Sn in foods are described: for Hg--colorimetry of tetraiodide mercurate and atomic absorption spectroscopy (AAS); for Pb, Cd, Zn, and Cu--polarography; for Cu--colorimetry with sodium diethyldithiocarbamate and zinc dibenzyldithiocarbamate; for As--colorimetry with silver diethyldithiocarbamate; for Sn--colorimetry with quercetin; and for Fe--colorimetry with o-phenanthroline. All of the methods have the necessary metrological characteristics, including intralaboratory repeatability value (r), interlaboratory reproducibility value (R), minimum quantity of the element to be determined in the analytical test portion (MQSM), and the coefficients that account for mercury and arsenic losses during analysis. Establishing constant r- and R-values for the methods under consideration is expedient because (a) the methods suggested are used for safety purposes; and (b) the optimum amount of the element studied in the test sample is determined, to a certain degree, by the mass of the test portion.     

Zur Verwendung von Gesteinsmehlen in der Landwirtschaft. I. Chemisch-mineralogische Zusammensetzung und Eignung von Gesteinsmehlen als Düngemittel

The use of rock powders in agriculture. I. Chemical and mineralogical composition and suitability of rock powders for fertilization Five different rock powders were investigated in order to test their suitability for agricultural fertilization. The fertilization effect of rock powders is greatly influenced by the mineralogical composition and the intensity of grinding, but less by the total content of nutrients. The low content of soluble nutrients (less than 1%) and the high portion of elements without any importance for plant nutrition (more than 70% oxigen-bound Si, Al and Fe) raises the question if rock powders can be successfully applied as fertilizers, at least in annual cropping systems. Because of the enormous differences between the investigated rock powders the term “rock powder” does not describe any specific characteristics for the user.     

Thin layer chromatographic determination of aflatoxins, ochratoxins, sterigmatocystin, zearalenone, citrinin, T-2 toxin, diacetoxyscirpenol, penicillic acid, patulin, and penitrem A.

A general method is described for determining 16 mycotoxins in mixed feeds and other food products used in the manufacture of these feedstuffs. The mycotoxins are extracted and cleaned up by extracting with solvents of different pH. Thin layer chromatography is used to separate the toxins; toxins are then quantitated by the limit detection method. The minimum detectable concentration of mycotoxins in various products is: aflatoxin B1 or G1, 4--5 micrograms/kg; ochratoxin A or ethyl ester A 140--145 micrograms/kg; citrinin 600--750 micrograms/kg; zearalenone, 410--500 micrograms/kg; sterigmatocystin, 140--145 micrograms/kg; diacetoxyscirpenol, 2400--2600 micrograms/kg; T-2 toxin, 800--950 micrograms/kg; patulin, 750--800 micrograms/kg; penitrem A 14,000--14,500 micrograms/kg; penicillic acid 3400--3650 micrograms/kg.     

Precision parameters of methods of analysis required for nutrition labeling. Part I. Major nutrients

Major components of foods and feeds are fat, protein, and carbohydrates. Fat and protein are determined by direct measurements that are interpreted as the quantity of the constituent. Carbohydrates are usually calculated by difference. For this calculation, values for moisture/solids, ash, and "fiber" are also needed. The readily available collaborative studies for the determination of these major components are reviewed in an attempt to assign precision parameters to validated methods of analysis. When a number of studies for the same analyte, in the same food, by the same method are available, it is seen that the precision parameters among laboratories (standard deviations, SR; relative standard deviations, RSDR) and the ISO maximum tolerable difference functions (repeatability value, r; reproducibility value, R) are not characterized by any conventional distribution. The precision data are best summarized as a median or average parameter and the interval containing the centermost 90% of reported values. Typically, the precision of methods of analysis can be expressed as a function of concentration only, independent of analyte, matrix, and method. The average RSDR value from each collaborative data set can then be used as the numerator in a ratio containing, as the denominator, the value calculated from the Horwitz equation: RSDR = 2 exp (1 - 0.5 log C) where C is the concentration as a decimal fraction. A series of ratios consistently above 1, and especially above 2, probably indicates that a method is unacceptable with respect to precision. By this criterion, only the protein (Kjeldahl) determination is unqualifiedly acceptable with a 90% interval for RSDR of 1 to 3% at C values above about 0.01 (1 g/100 g). Fat, moisture/solids, and ash are acceptable down to limiting concentrations in the region of 1 to 5 g/100 g, if a test portion large enough to provide at least 50 mg of weighable residue or volatiles is specified. Measurements of individual carbohydrates and fiber-related analytes have unexpectedly poor precisions among laboratories. The variability, although high, may still be suitable for nutrition labeling. Reliability of analyses for the control of labeling of the primary nutrients must be achieved through quality assurance programs that require strict adherence to the directions of empirical methods and the use of suitable reference materials for absolute methods.     

Sensitive and rapid reversed-phase liquid chromatography-fluorescence method for determining bisphenol A diglycidyl ether in aqueous-based food simulants.

A method has been developed for determination of bisphenol A diglycidyl ether (BADGE) in 3 aqueous-based food simulants: water, 15% (v/v) ethanol, and 3% (w/v) acetic acid. BADGE is extracted with C18 cartridges and the extract is concentrated under a stream of nitrogen. BADGE is quantitated by reversed-phase liquid chromatography with fluorescence detection. Relative precision at 200 micrograms/L was 3.4%, the detection limit of the method was 0.1 micrograms/L, and recoveries of spiking concentrations from 1 to 8 micrograms/L were nearly 100%. Relative standard deviations for the method ranged from 3.5 to 5.9%, depending on the identity of the spiked aqueous-based food simulant.     

Simple, rapid cleanup method for analysis of aflatoxins and comparison with various methods

A method is described for simple and rapid determination of aflatoxins in corn, buckwheat, peanuts, and cheese. Aflatoxins were extracted with chloroform-water and were purified by a Florisil column chromatographic procedure. Column eluates were concentrated and spotted on a high performance thin layer chromatographic (HPTLC) plate, which was then developed in chloroform-acetone (9 + 1) and/or ether-methanol-water (94 + 4.5 + 1.5) or chloroform-isopropanol-acetone (85 + 5 + 10). Each aflatoxin was quantitated by densitometry. The minimum detectable aflatoxin concentrations (micrograms/kg) in various test materials were 0.2, B1; 0.1, B2; 0.2, G1; 0.1, G2; and 0.1, M1. Recoveries of the aflatoxins added to corn, peanut, and cheese samples at 10-30 micrograms/kg were greater than 69% (aflatoxin G2) and averaged 91%, B1; 89%, B2; 91%, G1; 78%, G2; and 92%, M1. The simple method described was compared with the AOAC CB method, AOAC BF method, and AOAC milk and cheese method. These methods were applied to corn, peanut, and cheese composites spiked with known amounts of aflatoxins, and to naturally contaminated buckwheat and cheese. Recoveries were much lower for the BF method compared with our simple method and the CB method.     

Integration of ANP and Fuzzy set techniques for land suitability assessment based on remote sensing and GIS for irrigated maize cultivation

Land suitability assessment can inform decisions on land uses suitable for maximizing crop yield while making best use, but not impairing the ability of natural resources such as soil to support growth. We assessed the suitability of maize to be produce in 12,000 ha land of Dasht-e-Moghan region of Ardabil province, northwest of Iran. Suitability criteria included soil depth, gypsum (%), CaCO₃ (%), pH, electrical conductivity (EC), exchangeable sodium percentage (ESP), slope (%) and climate data. We modified and developed a novel set of techniques to assess suitability: fuzzy set theory, analytic network process (ANP), remote sensing and GIS. A map of suitability was compared a map created using a traditional suitability technique, the square root method. The coefficient of determination between the land suitability index and observed maize yield for square root and ANP-fuzzy methods was 0.747 and 0.919, respectively. Owing to greater flexibility to represent different data sources and derive weightings for meaningful land suitability classes, the ANP-fuzzy method was a superior method to represent land suitability classes than the square root method.     

Simplified cleanup and liquid chromatographic determination of oxamyl residues in potato tubers

A simple and efficient method is presented for the extraction, cleanup, and liquid chromatographic (LC) determination of oxamyl residues in potato tubers. Samples are extracted with methanol, partitioned into dichloromethane, and cleaned up using Sep-Pak Florisil cartridges. LC determination is performed using a Zorbax PSM 60 size exclusion column with an acetonitrile-water (1 + 9) mobile phase and UV detection at 254 nm. Recovery of oxamyl from spiked control tubers averaged 94.1 and 85.9% at fortification levels of 0.4 and 0.08 micrograms oxamyl/g tuber, respectively. The minimum detectable concentration of oxamyl by this method is 0.01 micrograms/g.     

Simplified cleanup and liquid chromatographic ultraviolet determination of linuron and three metabolites in potatoes

A simple and efficient method is presented for the extraction, cleanup, and liquid chromatographic (LC) determination of linuron and 3 of its metabolites, 3-(3,4-dichlorophenyl)-1-methyl urea (DCPMU), 3-(3,4-dichlorophenyl) urea (DCPU), and 3,4-dichloroaniline (DCA), in potatoes. Samples are extracted with acetone, partitioned into dichloromethane-hexane (1 + 1), and cleaned up using disposable silica cartridges. LC determination is performed using a LiChrosorb NH2 5 microns column, with an isopropanol-isooctane gradient mobile phase and UV detection at 248 nm. Recoveries of linuron and 2 of the metabolites from untreated samples fortified at 0.02-2 micrograms/g ranged from 80 to 102%, while recoveries for the metabolite DCA ranged from 60 to 78%. The detection limit was 0.015 micrograms/g for linuron and each metabolite; the minimum quantitation level was 0.5 micrograms/g. The developed method was applied to potato samples from a field experiment.     

Rapid thin layer chromatographic determination of zearalenone in corn, sorghum, and wheat

A rapid method is described for determining zearalenone in corn, sorghum, and wheat. The mycotoxin is extracted with a mixture of acetonitrile and 4% KCl in HCl. The extract is cleaned up with isooctane, evaporated, and redissolved in chloroform. Zearalenone is separated by thin layer chromatography; identity is confirmed with various developing solvents and spray reagents. Zearalenone is then quantitated by the limit detection method. The minimum detectable concentration is 140-160 micrograms/kg when aluminum chloride solution is used as spray reagent, and 85-110 micrograms/kg when Fast Violet B salt is used as spray reagent.     

Application of two-dimensional gel electrophoresis to interrogate alterations in the proteome of genetically modified crops. 1. Assessing analytical validation

Current tools used to assess the safety of food and feed derived from modern biotechnology emphasize the investigation of possible unintended effects caused directly by the expression of transgenes or indirectly by pleiotropy. These tools include extensive multisite and multiyear agronomic evaluations, compositional analyses, animal nutrition, and classical toxicology evaluations. Because analytical technologies are rapidly developing, proteome analysis based on two-dimensional gel electrophoresis (2DE) was investigated as a complementary tool to the existing technologies. A 2DE method was established for the qualitative and quantitative analysis of the seed proteome of Arabidopsis thaliana with the following validation parameters examined: (1) source and scope of variation; (2) repeatability; (3) sensitivity; and (4) linearity of the method. The 2DE method resolves proteins with isoelectric points between 4 and 9 and molecular masses (MM) of 6-120 kDa and is sensitive enough to detect protein levels in the low nanogram range. The separation of the proteins was demonstrated to be very reliable with relative position variations of 1.7 and 1.1% for the pI and MM directions, respectively. The mean coefficient of variation of 254 matched spot qualities was found to be 24.8% for the gel-to-gel and 26% for the overall variability. A linear relationship (R2 > 0.9) between protein amount and spot volume was demonstrated over a 100-fold range for the majority of selected proteins. Therefore, this method could be used to interrogate proteome alterations such as a novel protein, fusion protein, or any other change that affects molecular mass, isoelectric point, and/or quantity of a protein.     

Rapid pentachlorophenol evaluation in solid matrixes by second derivative UV spectroscopy for application to wood and leather samples

A method for the quail-quantitative evaluation of pentachlorophenol (PCP) in solid matrixes has been developed. The procedure is based on solid-liquid extraction of solid samples (leather or wood), followed by purification on a cyanopropyl column and determination of the preservative by second derivative UV spectroscopy considering the PCP A peak-through value (304-297 nm). The method allows rapid PCP determination in the concentration range 1-40 micrograms/mL; any matrix interference is avoided by the purification step and recoveries of the preservative were 99.12% (RSD% 0.13) for the leather matrix and 98.03 (RSD% 0.17) for the wood matrix.     

基于GIS的皖南山区茶叶种植适宜性评价

以石台县为例,运用ArcGIS地理信息系统以及县域耕地资源管理信息系统,利用石台县测土配方施肥项目的采样调查分析结果,该研究通过确定评价单元,建立了具有区域特色的评价指标体系,并采用耕地自然要素评价综合指数法对石台县茶叶种植适宜性进行定量评价分析。     

Determination of carbon and nitrogen in samples of various soils by the dry combustion

Abstract

Carbon and nitrogen (N) content of various soils in the world were analyzed using a CNS‐2000 (LECO, Corp., St. Joseph, MI) analyzer. The results were in good agreement with those obtained by a laboratory proficiency test at the International Soil‐Analytical Exchange, organized by Wageningen Agricultural University, Wageningen, The Netherlands. The best agreement for both elements was observed at a combustion temperature of 1000°C. Results of organic carbon (C) determined by the Tyurin method were closely related to results of C determination at this temperature. Higher C contents were obtained with samples rich in carbonates when analyzed at higher temperatures >1000°C. These results confirm the suitability of automated dry combustion in soil analysis for C and N.     

Validity of photographs for food portion estimation in a rural West African setting

OBJECTIVE: To validate food photographs for food portion size estimation of frequently consumed dishes, to be used in a 24-hour recall food consumption study of pregnant women in a rural environment in Burkina Faso. This food intake study is part of an intervention evaluating the efficacy of prenatal micronutrient supplementation on birth outcomes. SUBJECTS: Women of childbearing age (15-45 years). DESIGN: A food photograph album containing four photographs of food portions per food item was compiled for eight selected food items. Subjects were presented two food items each in the morning and two in the afternoon. These foods were weighed to the exact weight of a food depicted in one of the photographs and were in the same receptacles. The next day another fieldworker presented the food photographs to the subjects to test their ability to choose the correct photograph. RESULTS: The correct photograph out of the four proposed was chosen in 55% of 1028 estimations. For each food, proportions of underestimating and overestimating participants were balanced, except for rice and couscous. On a group level, mean differences between served and estimated portion sizes were between -8.4% and 6.3%. Subjects who attended school were almost twice as likely to choose the correct photograph. The portion size served (small vs. largest sizes) had a significant influence on the portion estimation ability. CONCLUSIONS: The results from this study indicate that in a West African rural setting, food photographs can be a valuable tool for the quantification of food portion size on group level.     

Bacillus stearothermophilus disk assay for determining ampicillin residues in fish muscle.

The Bacillus stearothermophilus disk assay for penicillin in milk (AOAC official method) was adapted for the determination of ampicillin in fish muscle. The method was evaluated in 2 species of cultured fish: channel catfish and striped bass. Recoveries of ampicillin ranged from 99 to 104% when muscle specimens from both species were spiked at concentrations of 0.025-1.00 micrograms/g. The lower limit of determination (LOD) was 0.025 micrograms/g. The assay was applied to monitor the elimination of ampicillin from the muscle of striped bass after intravascular administration (dosage of 10 mg/kg body weight). The mean concentrations in the muscle declined from 1.160 micrograms/g at 2 h to 0.063 micrograms/g at 18 h. The half-life of ampicillin in the muscle was 3.6 h. Ampicillin concentrations were below LOD at 24 h. No inhibitory activity was observed in the muscle of control fish.     

Maintaining estuary quality for shorebirds: towards simple guidelines

It is increasingly important to be able to monitor and maintain the quality of estuaries for overwintering shorebirds. Bird numbers alone are not sufficient to indicate quality nor, as recent research shows, can it be assumed that site quality is being maintained simply because there is enough food to meet the birds’ physiological demands; i.e., the amount of food available per bird in autumn needs to be greater than the amount eaten. But how much greater? We used a simple individuals-based and behaviour-based model to explore the factors that affect the relationship between overwinter mortality and the amount of food available per bird in autumn (the food:bird ratio). The aims were to explore how the natural history characteristics of a shorebird species affected the shape of this relationship, in order to identify characteristics of the system that should be included in any monitoring programme of site quality. In all cases there was a minimum threshold food:bird ratio above which mortality did not vary and below which mortality increased steadily. The amount of food per bird required at the threshold varied from one to six times the amount actually consumed by each bird during winter, depending on the amount of realism included in the model. The minimum threshold ratio was most strongly influenced by the shape of the relationship between intake rate and prey density - the functional response - and, when interference competition occurred, by the distribution of the birds’ main food supply. Simulations with realistic spatial distributions of prey predicted that the minimum required amount of food per bird would be between two and five times the amount actually consumed. The threshold approach could provide a simple method of monitoring estuary quality based on food supply and bird numbers. It also provides a potentially clearly-defined and unambiguous measure of the carrying capacity of a site. If applied to a sufficient number of real estuaries, general guidelines for maintaining estuary quality based on estuary characteristics, food supply and bird species might be established.     

A quantitative stable-isotope LC-MS method for the determination of folic acid in fortified foods

A stable-isotope liquid chromatography-mass spectrometry (LC-MS) assay was developed for the quantitative determination of folic acid in fortified foods. Folic acid was extracted from food samples into a phosphate buffer, purified on a C-18 Sep-Pak cartridge, and analyzed by LC-MS in the negative ion mode using electrospray ionization. The analyte was quantified using (13)C(5)-folic acid as an internal standard. The coefficient of variation for the precision of the method was 5.6% based on the analysis of four sample replicates. The accuracy of the method was assessed using a standard method of addition of folic acid to a shredded whole-wheat cereal. The quantitative determination of folic acid in this matrix was linear over 1 order of magnitude having a concentration range of 2.4 to 24 microg/g of food (or 0.05 to 0.5 microg of analyte injected into the LC-MS). The overall quantitative efficiency of the method was evaluated using a standard reference material (infant formula SRM 1846). The method was applied to the determination of folic acid in several test samples (fortified breakfast cereals), and the values were in accord with the manufacturer's claim. This method advances a LC-MS technique for the determination of folic acid in fortified foods based on stable-isotope dilution methodology. The specificity of the technique and quantitative accuracy of the method in various food substrates suggests that the method may be adapted for routine analysis in other fortified foods.     

Ion chromatographic determination of perchlorate in foods by on-line enrichment and suppressed conductivity detection

Systemic uptake of perchlorate anion, a rocket fuel component and potential thyroid function disruptor, by leafy vegetables and other crops grown in contaminated waters is a public health concern. A column-switching anion-exchange chromatographic method with suppressed conductivity detection, described in this paper, achieved a 3-6 microg/kg method limit of quantitation in analysis of the wet weight edible portion of cantaloupe, carrots, lettuce, and spinach samples with field-incurred perchlorate. A test portion was blended with dilute nitric acid, and the extract was filtered under vacuum. A portion of the measured filtrate was acidified to pH approximately 2 by addition of cation-exchange resin, 4 mL was passed through a graphitized carbon cleanup column, and an aliquot of a collected fraction was pushed through a short precolumn for anion extraction, enrichment, and injection onto the analytical column. Statistical comparison with determination by tandem mass spectrometry-ion chromatography analysis of untreated filtrate revealed that the difference between means was not significant at the 95% confidence level (P value > or = 0.12) for crops tested. In addition, the method was applied to cooked vegetables processed as baby food.     

过硫酸钾氧化-间苯二酚光度法测定地表水中总氮的探讨

参考间苯二酚光度法测定水中硝酸根，探讨和试验了过硫酸钾氧化－间苯二酚光度法测定地表水中总氮。该法共存离子干扰少，精密度与准确度较好，最低检出限0．08mg／l。