[Application of polarography and oscillographic polarography with alternating current to food analysis].
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The calcium-, magnesium-, phosphorus-, nitrogen- and water-contents have been estimated in raw and processed foods (bread and sausages). These results were then compared with the data in food tables. Surprisingly small differences were recorded, since content-deviations of processed foods are equalized in a whole day menu. Thus, food tables proved to be reliable for the calculation of balance and test diets.
The formation of D-amino acids (D-aa's) in many fermented foods depends, among other factors, on the particular fermentation conditions, the action and autolysis of the microorganisms involved. In this sense, the analysis of chiral amino acids is an interesting analytical strategy for food scientists, since these compounds can be used as bacterial markers and can help, e.g., to detect adulterations, microbiological contaminations, etc. In this work, a fast and sensitive method based on MEKC-LIF has been developed to analyze and quantitate L-amino acid (L-aa) and D-aa in vinegars. The chiral MEKC-LIF procedure uses 100 mM sodium tetraborate, 30 mM SDS, and 20 mM beta-CD at pH 9.7 as running buffer, obtaining a good separation of the main vinegar L-/D-aa previously derivatized with fluorescein isothiocianate. Namely, L/D proline, alanine, arginine, glutamic, and aspartic acid, plus the nonchiral amino acid gamma-aminobutyric acid are separated in less than 20 min with high efficiency (up to 720,000 plates/m) and good sensitivity (LODs lower than 16.6 nM were achieved). Several D-aa's were detected and quantified in balsamic, sherry, white wine, and cider vinegars using this MEKC-LIF procedure, observing interesting differences in their L-aa and D-aa profiles and contents.
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Fast temperature-programmed gas chromatography (FTGC) is evaluated. A modified capillary column allowing temperature-program rates as high as 20 degrees C/s is operated with mass spectrometric detection (MSD). FTGC methods are developed for the analysis of off-flavors in water, derivatized sugars, and fatty acid methyl esters. Liquid injection and solid-phase microextraction are evaluated. Although the resolution can be somewhat lower than analysis with a traditional column, time savings are significant. Analysis times range from 2 to 4.5 min compared with 20 to 60 min for conventional methods. MSD allows for the analysis of some coeluting peaks, which allows for quantitation even when peaks coelute.
The 4 major driving forces that are expected to lead to increased use of affinity biosensors that meet crucial industrial test specifications, e.g., fast, reliable, cost-effective, and use of low-skilled personnel, are (1) strict legislative framework, e.g., recent changes proposed to the European food safety and hygiene legislation, EC No. 178/2002; (2) industrial shift from quality control to quality assurance procedures, e.g., Hazard Analysis Critical Control Point, ensuring effective positioning in the global competitive trade; (3) just-in-time production resulting in 'right' product every time; and (4) consumer demand for safe and wholesome products. The affinity biosensors field has expanded significantly over the past decade, with a projected global biosensors market growth from $6.1 billion in 2004 to $8.2 billion in 2009, representing major industrial sectors (e.g., Pharma, Medicare, and Food). This brief review is targeted to affinity biosensors developed for the food industry and includes research and development leading to biosensors for microbiological and chemical analytes of industrial concern, commercial biosensors products on the market, and examples of future prospects in this diagnostic field.
A simple, rapid, and reliable method for the determination of residual sulphonamide antibacterials (SAs) (sulfadiazine, sulfamerazine, sulfadimidine, sulfamethoxypiridazine, sulfisozole, sulfamonomethoxine, sulfamethoxazole, sulfisoxazole, sulfadimethoxine, and sulfaquinoxaline) in animal liver and kidney was developed using a combination of clean-up on a Bond Elut PSA cartridge and HPLC with UV detection. The SAs were extracted with ethyl acetate and then dissolved in 5 ml of 50 v/v% ethyl acetate-n-hexane after being evaporated to dryness. For clean-up of the crude sample, the resuspended extract was applied to a Bond Elut PAS (primary/secondary amine cartridge), and then SAs were eluted from the cartridge using 5 ml of 20 v/v% acetonitrile-0.05 M ammonium formate before being analysed by HPLC. Recoveries of the SAs at the levels of 0.5 and 0.1 microg/g were 70.8-98.2%, the rerative standard deviation were less than 7.0%, and the detection limits were 0.03 microg/g. The present analysis method of SAs in animal kidney and liver using HPLC with a clean-up procedure was demonstrated to be highly applicable to the direct LC-MS-MS analysis without any modification.
A multiresidue analytical method was developed for the confirmation of benzylpenicillin (PCG), phenoxymethylpenicillin (PCV), oxacillin (MPIPC), cloxacillin (MCIPC), nafcillin (NFPC) and dicloxacillin (MDIPC) in bovine tissues using electrospray ionization liquid chromatography-tandem mass spectrometry (LC-ESI-MS-MS) with a product ion scan mode. All penicillins gave [M-H]-, [M-H-CO2]- and [M-H-141]- as the product ion, when [M-H]- was selected as the precursor ion. Combination of an ion-exchange cartridge clean-up and the LC-ESI-MS-MS method can reliably identify all of these penicillins fortified at a concentration of 0.05 mg/kg in bovine tissues, including liver, kidney and muscle. The limits of confirmation satisfy the maximum residue limits for each of the penicillins established by the World Health Organization, US Food and Drug Administration, European Union and Japan.
Furnace atomic absorption is a very sensitive method for determination of lead and other trace metals in a variety of samples, but it is prone to matrix interferences. A major improvement in the method is achieved by the use of a L'vov platform, a small piece of graphite placed inside the furnace tube, onto which the sample solution is pipetted. The temperature of the platform rises more slowly than that of the tube wall during the atomization cycle, and sample vaporization is delayed until the furnace atmosphere is at a high and nearly constant temperature. The resulting atomization behavior is more consistent and less matrix-dependent for numerous analyte elements, including lead. Results are further improved by addition of ammonium phosphate to all samples and standards as a matrix modifier. For example, in comparing analyte sensitivity (slope of the absorbance vs concentration curve) in a variety of food sample types to the sensitivity in dilute HNO3, the average lead response showed 60 +/- 15% suppression due to the sample matrices. Use of the L'vov platform and matrix modifier virtually eliminated the suppression and improved the precision.
The review covers over 230 papers published mostly in the last 5 years. The goal of the review is to attract the attention of researchers and users to stripping voltammetry in particular, its application in environmental monitoring and analysis of foodstuffs. The sensors employed are impregnated graphite, carbon paste, thick film carbon/graphite and thin film metallic electrodes modified in-situ or beforehand. Hanging mercury drop electrodes and mercury coated glassy carbon electrodes are also mentioned. Strip and long-lived sensors for portable instruments and flow through systems are discussed as devices for future development and application of stripping voltammetry.
This paper introduces a facile method to determine the amount of mono- and diglycerides in virgin olive oils. This method is based on the phosphorylation of the free hydroxyls of the mono- and diglycerides with 2-chloro-4,4,5,5-tetramethyldioxaphospholane and the integration of the appropriate peaks in the (31)P NMR spectrum. Quantitative (31)P NMR spectroscopy can be extended to the quantification of other constituents of olive oils bearing functional groups with labile protons.
Trace metals such as mercury, especially its organic compounds, are an important risk to the environment and to man due to their accumulation in the food chain. For this reason, the routine determination of the very toxic methylmercury, and of other organic and inorganic mercury compounds in marine and land animals, vegetables, fruits and fresh water is of increasing importance in health and environmental control programmes throughout the world. The majority of speciation methods for organomercurials involve a series of fundamental steps for the identification and quantification of samples of biological origin: extraction or isolation from the matrix; derivatisation and concentration; detection; separation of different species of interest and of interference. Each of these steps, as part of the chromatographic analysis of MeHg and of other organomercurials is revised in this study using food samples.
This paper describes an inexpensive and relatively simple procedure to prepare high-performance size-exclusion columns from laboratory-packed or commercially pre-packed high-performance liquid chromatography columns by chemical deactivation of the surface of the silica packing material. The columns can be prepared quickly and reproducibly, they are chromatographically as efficient as high-performance size-exclusion columns commercially available, and are prepared at a fraction of the cost. Examples of the separation of proteins, peptides and polysaccharides on laboratory-prepared columns with differing permeation characteristics are illustrated and discussed.
Twelve laboratories participated in a collaborative study to evaluate precision parameters of a liquid chromatographic method for analysis of the glycoalkaloids alpha-solanine and alpha-chaconine in potato tubers. Samples consisted of frozen potato tuber homogenates distributed as 3 blind duplicates and 3 split-level pairs. The analytical method included aqueous extraction, workup on disposable solid-phase extraction cartridges, and reversed-phase chromatography with photometric detection at 202 nm. Results for alpha-solanine and alpha-chaconine were received from 10 and 9 laboratories, respectively. Relative standard deviations for reproducibility for alpha-solanine and alpha-chaconine were similar, ranging from 8 to 13% in the applied concentration range of 12 to 260 mg/kg fresh weight.
Near-Infrared Spectroscopy (NIRS) is the most rapidly developing and the most noticeable spectrographic technique in the 90's (the last century). Its principle and characteristics were explained in this paper, and the development of NIRS instrumentation, the methodology of spectrum pre-processing, as well as the chemical metrology were also introduced. The anthors mainly summarized the applications to agriculture and food, especially in-line analysis methods, which have been used in production procedure by fiber optics. The authors analyzed the NIRS application status in China, and made the first proposal to establish information sharing mode between central database and end-user by using network technology and concentrating valuable resources.
The triacylglycerol (TAG) profiles present in real world lipidic samples are usually quite complex and, as such, monodimensional high-performance liquid chromatographic (HPLC) techniques are inadequate when challenged with such matrices. In this respect, the complementary use of silver-ion (Ag) and non-aqueous (NA) reversed-phase (RP) HPLC can be exploited if thorough TAG separations are required. The present investigation reports the employment of a newly developed comprehensive LC (LC x LC) system, based on the different separation mechanisms of the aforementioned techniques, and applied to a rice oil sample. The approach was successful in the separation of a high number of solutes, otherwise unachievable through monodimensional LC. Furthermore, the use of atmospheric pressure chemical ionization mass spectrometry (APCI-MS), as detection system, provided a third analytical dimension boosting the identification power of the comprehensive chromatographic method.
A new physically adsorbed capillary coating for capillary electrophoresis-mass spectrometry (CE-MS) of basic proteins is presented, which is easily obtained by flushing the capillary with a polymer aqueous solution for two min. This coating significantly reduces the electrostatic adsorption of a group of basic proteins (i.e., cytochrome c, lysozyme, and ribonuclease A) onto the capillary wall allowing their analysis by CE-MS. The coating protocol is compatible with electrospray inonization (ESI)-MS via the reproducible separation of the standard basic proteins (%RSD values (n = 5) < 1% for analysis time reproducibility and < 5% for peak heights, measured from the total ion electropherograms (TIEs) within the same day). The LODs determined using cytochrome c with total ion current and extracted ion current defection were 24.5 and 2.9 fmol, respectively. Using this new coating lysozymes from chicken and turkey egg white could be easily distinguished by CE-MS, demonstrating the usefulness of this method to differentiate animal species. Even after sterilization at 120 degrees C for 30 min, lysozyme could be detected, as well as in wines at concentrations much lower than the limit marked by the EC Commission Regulation. Adulteration of minced meat with 5% of egg-white could also be analysed by our CE-MS protocol.