Monitoring survey of patulin in a variety of fruit-based products using a sensitive UHPLC–MS/MS analytical procedure

The mycotoxin patulin is known to be the predominant natural contaminant of apples, apple-based products and a variety of other fruits. Because of its high incidence and harmful health effects, patulin is included with mycotoxins, which are strictly monitored. In this study, a sensitive and reliable ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS) method was developed and validated for determination of patulin in a variety of fruit matrices. A combination of the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) procedure along with a solid phase extraction (SPE) clean-up strategy enabled an effective removal of sample matrix and pre-concentration of patulin. This resulted in low limits of quantification ranging from 1 to 2.5 μg/kg, depending on fruit type. In our study, quantification of patulin was based on a stable isotope dilution assay (SIDA) using ¹³C₇-patulin as the internal standard. Data showed that the procedure described, in combination with neat solvent internal calibration, can be used for accurate quantification of patulin regardless the type of fruit. Although the SIDA method allowed omission of matrix-matched calibration, matrix-effects were estimated in order to assess suppression of the patulin signal caused by a variety of fruit samples. The method was fully validated for apples, apple baby food, apple juice, peaches, strawberries and blueberries. The recovery values were in the range from 92 to 109%. Repeatability of the method was below 10% for all tested matrices. The method was applied to the monitoring of patulin in 135 samples of fresh fruits and fruit products and can also be used as an efficient tool for routine monitoring of this contaminant in a variety of fruit-based foods.     

Vanadium-ceria catalysts for H2S abatement from biogas to feed to MCFC

Vanadium-based catalysts supported on ceria were studied for the direct and selective oxidation of H₂S to sulphur and water at low temperature.Catalysts with two vanadium loading (20–50 wt% of V₂O₅) were prepared, characterized and tested at temperature of 150–200 °C in order to identify the best catalytic formulation. The most promising catalyst was the sample with the 20 wt% of V₂O₅ that showed 99% of sulphur selectivity and equilibrium H₂S conversion at 150 °C.The effect of the components of a typical biogas stream (CH₄, CO₂ and H₂O) was studied at 150 °C in order to investigate the possible formation of secondary products such COS, CS₂. No significant effect was observed in terms of H₂S conversion (99%) and selectivity to SO₂ (<1%) by adding CH₄ and CO₂ to the feed stream. Furthermore, the effect of the H₂S inlet concentration, temperature, contact time and molar feed ratio (O₂/H₂S) were also investigated at a reaction temperature of 80 °C.Finally, time on stream tests of 30 h were performed at 80 and 120 °C, in order to examine the catalyst stability.     

我国食品接触材料标准新体系构建

食品接触材料标准为食品安全国家标准的重要组成部分,通过标准清理整合等工作,我国食品接触材料标准新体系基本建成。本文主要介绍了我国食品接触材料新标准体系的构成,对比分析了新标准体系发生的主要变化,科学梳理了行业面临的挑战以及新标准体系存在的问题,提出了下一步工作建议。     

Low temperature catalytic oxidation of H2S over V2O5/CeO2 catalysts

CeO₂ supported vanadium catalysts at different V₂O₅ loads (2.55–20.00 wt%) were tested for the selective catalytic H₂S oxidation to sulfur at low temperature.The aim of the work is to investigate the effect of temperature and contact time in order to realize in one step a very high H₂S conversion, minimizing SO₂ formation.Catalytic activity tests showed in the range 2.55–20.00 wt% the effect of the vanadium loading plays a major role on sulfur selectivity. In particular, the 20.00 wt% V₂O₅/CeO₂ catalyst was the most interesting sample with a selectivity to sulfur of 99%. The H₂S conversion calculated experimentally at 150 °C is 98.7%, very close to that obtained by thermodynamic equilibrium calculations, corresponding to 99%.Interesting results were also obtained from the preliminary tests on the effect of the contact time, suggesting information relating to the reaction behavior as well as helping to identify the optimal operating conditions capable of minimizing SO₂ selectivity.     

Aflatoxin contamination and exposure in processed cereal-based complementary foods for infants and young children in greater Accra,Ghana

In the study, aflatoxin levels were assessed in thirty five (35) cereal-based food products intended for infants and young children. Additionally, the results showed that 71% of the processed foods intended for infants contained AFB₁ (0.18 ± 0.01 to 36.10 ± 0.32 μgkg⁻¹) levels higher than the European Union permissible limits of 0.1 μg kg⁻¹. Aflatoxin intake was estimated using aflatoxin levels in the food products and the estimated individual consumption rates. The study also revealed mixed cereals as having the highest intake of aflatoxin B₁ contaminants (0.005–0.852 μgkg⁻¹bw d⁻¹; 0.004–0.657 μgkg⁻¹bwd⁻¹) with mean estimated daily intake (EDI) of 0.23 ± 0.16 μgkg⁻¹bwd⁻¹ and 0.153 ± 0.13 μgkg⁻¹bwd⁻¹ for infants and young children respectively. The estimated AFT intake recorded for infants and young children for all the cereal-based food ranged from 0.005 to 1.054 μgkg⁻¹bwd⁻¹ and 0.004–0.838 μgkg⁻¹bwd⁻¹ respectively.     

免疫亲和柱净化-高效液相色谱法测定红曲制品中桔霉素的含量

目的建立免疫亲和柱净化-高效液相色谱法测定红曲制品中桔霉素含量的分析方法。方法试样经甲醇-水提取,稀释过滤后经含桔霉素特异性抗体的免疫亲和柱净化,洗脱液经Merk Hibar RP-18e色谱柱分离,以乙腈:0.1%磷酸水溶液作为流动相,采用荧光检测器测定(激发波长350 nm,发射波长500 nm),以外标法定量。结果桔霉素在1~50 ng/m L范围内有良好的线性关系,相关系数为0.99991,方法检测限为50μg/kg,在50、100和200μg/kg 3个水平的加标回收率为67.55%~89.12%,相对标准偏差为5.43%~11.25%。结论该方法操作简便、准确,可适用于红曲制品中桔霉素的测定。     

Assessment of thermal aging embrittlement in a cast stainless steel valve and its effect on the structural integrity

This paper analyzes the thermal aging embrittlement occurred in a cast stainless steel valve, which is part of the reactor water clean-up (RWCU) system of a Spanish boiling water reactor (BWR) nuclear power plant. The aim is to estimate the current and future state of the material and the corresponding structural integrity of the valve. Given that there is no data available for the experimental characterization of the material, the evolution of the mechanical properties (fracture toughness, yield stress, flow stress and Ramberg-Osgood parameters) has been estimated using the ANL procedure.With the obtained estimations, the critical crack size has been calculated using the European procedure FITNET FFS and the ASME Code.This analysis considers not only the evolution of the mechanical properties up to now but also its future evolution in case there is a life extension of the plant until year 2029.     

Rapid multi-class multi-residue method for the confirmation of chloramphenicol and eleven nitroimidazoles in milk and honey by liquid chromatography-tandem mass spectrometry (LC-MS)

A confirmatory method was developed to allow for the analysis of eleven nitroimidazoles and also chloramphenicol in milk and honey samples. These compounds are classified as A6 compounds in Annex IV of Council Regulation 2377/90 (European Commission 1990) and therefore prohibited for use in animal husbandry. Milk samples were extracted by acetonitrile with the addition of NaCl; honey samples were first dissolved in water before a similar extraction. Honey extracts underwent a hexane wash to remove impurities. Both milk and honey extracts were evaporated to dryness and reconstituted in initial mobile phase. These were then injected onto a liquid chromatography-tandem mass spectrometry (LC-MS/MS) system and analysed in less than 9 min. The MS/MS was operated in multiple reaction monitoring (MRM) mode with positive and negative electrospray ionization. The method was validated in accordance with Commission Decision 2002/657/EC and is capable of analysing metronidazole, dimetridazole, ronidazole, ipronidazole and there hydroxy metabolites hydroxymetronidazole, 2-hydroxymethyl-1-methyl-5-nitroimidazole, and hydroxyipronidazole. The method can also analyse for carnidazole, ornidazole, ternidazole, tinidazole, and chloramphenicol. A recommended level of 3 µg l^?1/µg kg^?1 for methods for metronidazole, dimetridazole, and ronidazole has been recommended by the Community Reference Laboratory (CRL) responsible for this substance group, and this method can easily detect all nitroimidazoles at this level. A minimum required performance level of 0.3 µg l^?1/µg kg^?1 is in place for chloramphenicol which the method can also easily detect. For nitroimidazoles, the decision limits (CCα) and detection capabilities (CCβ) ranged from 0.41 to 1.55 µg l^?1 and from 0.70 to 2.64 µg l^?1, respectively, in milk; and from 0.38 to 1.16 µg kg^?1 and from 0.66 to 1.98 µg kg^?1, respectively, in honey. For chloramphenicol, the values are 0.07 and 0.11 µg l^?1 in milk and 0.08 and 0.13 µg kg^?1 in honey. Validation criteria of accuracy, precision, repeatability, and reproducibility along with measurement uncertainty were calculated for all analytes in both matrices.     

Indirect determination of aflatoxin B1 in beer via a multi-commuted optical sensor

This paper reports the determination of aflatoxin B₁ (AFB₁), one of the most carcinogenic substances known. A multi-commuted flow injection–solid phase spectroscopy (FI–SPS) system combined with photochemically induced fluorescence (PIF) was developed, for the first time, for its quantitative determination. A strongly fluorescent degradation product was obtained on-line by irradiation with ultraviolet light. The determination was carried out by measuring the fluorescence intensity of the photo-product at 353/424 (λ _ex/λ _em), once retained on C₁₈ silica-gel filling the flow-cell. A linear dynamic range of 0.09–12?µg?l^?1, detection limit as sensitive as 29?ng?l^?1 and a relative standard deviation (RSD) of 1.4% were obtained. The method proposed was satisfactorily applied to the determination of AFB₁ in different types of beer (normal and non-alcoholic). Hydrophobic compounds were eliminated from beer samples and AFB₁ was extracted with acetonitrile by solid-phase extraction on C₁₈ sorbent. Recoveries of the target compound from spiked beers were between 94 and 106%. The results obtained in the analysis of real samples are in good agreement with those provided by a reference chromatographic method.