石墨炉原子吸收光谱法测定食品级磷酸中铅

通过加入基体改进剂硝酸钯及采用氘灯作背景校正,直接用石墨炉原子吸收光谱法测定食品级磷酸中铅,回收率在94.0%～104.3%之间,RSD(n=6)≤3.90%,方法的检出限为0.15 pg,经与国家标准方法及电感耦合等离子发射光谱法测定结果对照,方法的准确度优于国家标准方法,检出限低于ICP-AES法.     

食品室内实物标样的制作

对食品室内实物标样的定义、特点和应用进行了介绍，提出了食品室内实物标样的具体制作步骤和测试方法，并提供了室内实物标样制作和应用的实例。     

Genotoxic properties of 2-dodecylcyclobutanone, a compound formed on irradiation of food containing fat

When food containing fat is treated by ionizing radiation, a group of 2-alkylcyclobutanones is formed. These components contain the same number of carbon atoms as their precursor fatty acids and the alkyl group is located in ring position 2. Thus, from palmitic acid 2-dodecylcyclobutanone is derived. To date, there is no evidence that the cyclobutanones occur in unirradiated food. Therefore, these components cannot be considered inherent to food, and for questions pertaining to risk assessment of irradiated food it would be advisable to determine the genotoxic and toxic potentials of cyclobutanones. Measurements of DNA damage in cells exposed to 2-dodecylcyclobutanone, employing the single cell microgel electrophoresis technique, have been carried out. In vitro experiments using rat and human colon cells indicate that 2-docylcyclobutanone in the concentration range of about 0.30 – 1.25 mg/ml induces DNA strand breaks in the cells. Simultaneously, a concentration related cytotoxic effect is observed as was determined by trypan blue exclusion. To which extent these in vitro findings are of relevancy for the in vivo human exposure situation needs to be investigated in further studies. In vivo tests in rats are in progress.     

High-performance liquid chromatography with evaporative light-scattering detection for the determination of phospholipid classes in human milk,infant formulas and phospholipid sources of long-chain polyunsaturated fatty acids

We developed and validated a new high-performance liquid chromatographic method for the separation of phospholipid classes in human milk, infant formulas and phospholipidic sources of long-chain polyunsaturated fatty acids (LC-PUFAs) used in paediatric nutrition. Phosphatidylcholine, phosphatidylethanolamine, phosphatidylinositol, phosphatidylserine and sphingomyelin were separated in less than 25 min using an Extrasil silica column (150 x 4.0 mm I.D., 3-microm particle size) by isocratic elution with a mixture of isopropanol-hexane-water. Phospholipids were determined by an evaporative light-scattering detector. Several chromatographic conditions were assayed to optimise the method, whose suitability is shown by the detection limits, linearity ranges and precision rates obtained. The main advantages of the proposed method are its speed and the direct determination of the main phospholipids present in human milk, infant formulas and the phospholipid sources of LC-PUFAs used in paediatric nutrition.     

Voltammetric Detection of Free Sulfhydryl Compounds in Food Flours

Cyclic voltammetry has been applied to the rapid measurement of free SH‐compounds in food flours samples. The protocol is based on the electrochemical adaptation of the Ellman's test, where the DTNB reacts with SH‐compounds present in food flour extracts, resulting in the equimolar production of the electroactive compound TNBA which, in turns, reacts with phenylendiamine. The reaction is found to provide an analytical signal from which to quantify indirectly free sulfhydryl compounds in flours extracts.     

Direct determination of sulfite in food samples by a biosensor based on plant tissue homogenate

In the work described here, a biosensor was developed for the determination of sulfite in food. Malva vulgaris tissue homogenate containing sulfite oxidase enzyme was used as the biological material. M. vulgaris tissue homogenate was crosslinked with gelatin using glutaraldehyde and fixed on a pretreated Teflon membrane. Sulfite was enzymatically converted to sulfate in the presence of the dissolved oxygen, which was monitored amperometrically. Sulfite determination was carried out by standard curves, which were obtained by the measurement of consumed oxygen level related to sulfite concentration. Several operational parameters had been investigated: the amounts of plant tissue homogenate and gelatin, percentage of glutaraldehyde, optimum pH and temperature. Also, some characterization studies were done. There was linearity in the range between 0.2 and 1.8 mM at 35 °C and pH 7.5. The results of real sample analysis obtained with the biosensor agreed well with the enzymatic reference method using spectrophotometric detection.     

Behaviour of organic pollutants in paper and board samples intended to be in contact with food

This paper deals with the study of volatile compounds present in a set of three paper and board (P&B) samples of different composition, surface treatment, grammage and thickness. The volatile compounds released by the packaging material (P&B) can be trapped on the food and may then affect the safety and health of consumers. To evaluate if the recycled P&B could be used as food packaging material, adsorption studies have been performed with a selection of chemical substances. The adsorption isotherms are provided. Partition coefficients between paper and air have been calculated for a series of volatile compounds used as model compounds to represent different families of contaminants commonly present in P&B. Values from 4 to 3243 were obtained at different temperatures. The analysis of volatile compounds have been carried out by automatic headspace coupled on-line with GC/MS in SIM mode. The results obtained are shown and discussed.     

Development of solid-phase extraction and solid-phase microextraction methods for the determination of chlorophenols in cork macerate and wine samples

Tri-, tetra- and pentachlorophenol (TCP, TeCP and PCP) can be considered the precursors in the formation of corresponding chloroanisoles, known to be powerful odorants in corks and wine. Determining the presence of these chlorophenolic compounds in cork soaking solutions (ethanol/water mixtures, 12% (v/v) ethanol used for cork quality control testing), or in wine can be achieved by acetylation/gas chromatography electron-capture detection. In order to reach the required sensitivity, a previous preconcentration step is necessary. Solid-phase extraction (SPE) and headspace solid-phase microextraction (HS-SPME) have given good results for the preconcentration of TCP, TeCP and PCP in such matrices. The use of Oasis HLB cartridges gives acceptable recoveries for the three compounds when different volumes (50-250 mL) of cork macerate with concentrations ranging from 20 to 150 ng/L are processed. Preconcentration based on HS-SPME has also been optimised with a 100 microm polydimethylsiloxane fibre and in situ derivatization. The HS-SPME method allows chlorophenols in a cork soaking solution and in wine to be determined with a limit of detection of 1 ng/L for each compound (in cork macerate) and a repeatability of around 0.5%-5% (n=8) for a concentration level of 30 ng/L.     

离子色谱柱切换技术同时测定食品中的多种成分

采用离子色谱柱切换技术同时测定了保留性质差别较大的有机酸以及不同价态的无机阴离子。由于柱切换基本不影响色谱基线,该法有较高的灵敏度。同时测定了食品中的乙酸,山梨酸、苯甲酸、糖精、氯离子和磷酸根。     

Formulation–composition map of a lecithin-based emulsion

Formulation–composition map is an interesting tool to predict the nature of an emulsion, stability, viscosity and nevertheless to decide the mixing protocol of its ingredients. Information based on optimum formulation (environmental conditions at which the affinity of an emulsifier for oil and for aqueous phase is same), which is depicted through hydrophilic–lipophilic deviation (HLD) concept, is necessary to make a formulation–composition map of an emulsion. In order to apply this concept in food emulsions, it is necessary to determine characteristic constants of each component of the system, i.e. the aqueous phase, the oil phase and the emulsifier at equilibrium. In this work formulation–composition map of a sunflower oil–water–lecithin system, based on the knowledge of phase behavior of lecithin at equilibrium and emulsification, was made. The shape of inversion line on formulation–composition map was not the classical stair type rather an almost vertical inversion line at water-fraction (f_w) near 0.20 was observed. It was supposed to be linked to the viscosity of oil phase which was 50 times the viscosity of aqueous phase. Additionally, emulsions were of oil-in-water (O/W) type for f_w higher than 0.20, but their viscosity and the drop size behavior with respect to salt concentration as formulation variable did not show the existence of transitional inversion line on formulation–composition map. Such map in advance can certainly facilitate the guidelines for dynamic emulsification.