Development and validation of a new LC–MS/MS method for the simultaneous determination of six major ergot alkaloids and their corresponding epimers. Application to some food and feed commodities

A liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for the simultaneous determination of six major ergot alkaloids, ergometrine, ergosine, ergotamine, ergocornine, ergokryptine and ergocristine, as well as their corresponding epimers in food and feed samples. The method involves extraction under alkaline conditions and subsequent clean-up by applying a simple and rapid liquid–liquid partitioning procedure prior to LC–MS/MS analysis. Evaluation of the method revealed good linearity, accuracy and precision. The limits of quantification varied from 0.1 to 1 μg/kg depending on the analyte and matrix. The average extraction and clean-up recoveries in different matrices were between 45 (only for ergometrine in biscuit) and 90%. The uncertainty associated with the analytical method was not higher than 51% and 30%, at concentration levels of 2.5 and 150 μg/kg respectively. Analyte epimerization proved to be minimal during the analytical procedure. The method has been successfully applied to the determination of ergot alkaloids in some Belgian food and feed commodities. Ergot alkaloids were found in 104 out of 122 samples investigated. Ergosine was the most frequently occurring alkaloid, while the highest levels were observed for ergotamine, ergocristine or ergosine, depending on the product type. The total alkaloid content in positive samples varied from 1 to 1145 μg/kg.     

城市家具中的无障碍设计

＂城市家具＂是城市中的重要组成部分,是城市文明与形象的具体体现,是城市人性化设计的展示平台。城市家具无障碍设计是一个复杂而系统的工程,是所有人平等参与城市活动的平台,是城市公共环境发展的方向。文章深入分析我国现有＂城市家具＂设计中存在的问题,总结无障碍设计的价值,影响因素和基本原则,为无障碍城市家具设计指明了发展趋势。     

2012—2014年青岛、深圳、大连三口岸282份进口水果和蔬菜中农药残留监测

目的掌握和了解进口水果和蔬菜中农药残留污染状况,为国家制定和完善相关标准和采取相关措施提供科学依据。方法本文采用GB/T 19648—2006《水果和蔬菜中500种农药及相关化学品残留量的测定气相色谱-质谱法》和GB/T 20769—2008《水果和蔬菜中450种农药及相关化学品残留量的测定液相色谱-串联质谱法》分析方法,对2012—2014年从青岛、深圳、大连三个主要水果和蔬菜进口口岸采集的282份水果和蔬菜样品进行了666种农药残留的检测。结果对282份水果和蔬菜样品进行农药残留测定和技术分析:未检出农药残留样品31份,占11.0%;检出农药残留样品251份,占89.0%。共检测出农药52种,频次702次。结合中国、欧盟、日本的农药最大残留限量标准,对获得的数据进行了科学的分析:进口香蕉、榴莲、火龙果、草莓的农药残留水平整体处于安全水平,应加强进口龙眼、樱桃、葡萄中农药残留的检测和监管。结论进口水果和蔬菜的农药残留检出率较高,达到89.0%,但超出中国最大残留限量标准的样品较少,只占1.1%,说明进口水果和蔬菜中农药残留整体处于安全水平。     

Application of hybrid image features for fast and non-invasive classification of raisin

A new approach for the non-invasive classification of raisins is presented based on the hybrid image features, namely morphological, color and texture features. A total of 74 features (8 morphological, 30 color, and 36 textural) were extracted from RBG images. Seven kinds of models were established based on different feature sets. They were three kinds of models established based on single feature set, three kinds of models established based on the combination of two feature sets, and one kind of model established based on the combination of all feature sets. Five kinds of classifiers, namely partial least squares (PLS), linear discriminant analysis (LDA), soft independent modeling of class analogy (SIMCA), and least squares support vector machine (LS-SVM) with linear and radial basis function (RBF) kernels were used for the model establishment based on different feature sets. The best correct answer rates (CAR) of 99% was obtained when LDA was used to establish the classification model based on the combination of all feature sets, which was higher than those of the models established based on single feature set or the combination of two feature sets. The results show that the feature combination is helpful to improve the accuracy of raisin classification. It was concluded that the varieties of raisin could be accurately classified based on RGB image features and the combination of morphological, color and texture features was an accurate way to improve the accuracy of classification.     

新型表面活性剂柠檬酸单酯的溶液性能研究及其在凝胶油中的应用

凝胶油不仅在功能食品中得到广泛应用,而且在药物制剂、化妆品领域也有重要应用前景。本文通过直接酯化法合成了两种柠檬酸单酯,并对其作为凝胶因子性能进行了研究。利用表面张力仪、电导率仪以及动态光散射仪等方法对两种柠檬酸酯的溶液聚集行为和胶束形成热力学进行了分析。结果表明,25℃下,柠檬酸月桂醇单酯和柠檬酸异癸醇单酯的临界胶束浓度分别为3.30mmol/L和6.40 mmol/L。同时,研究了离子强度对胶束形成过程的影响,结果表明,无机盐不仅影响胶束聚集数,而且使得柠檬酸异癸醇单酯的胶束尺寸降低约100 nm,柠檬酸月桂醇单酯的胶束尺寸降低约200 nm。凝胶油性能研究结果表明,最低凝胶浓度为7%,溶胶-凝胶转变温度为45~53℃之间,两种柠檬酸酯均能与植物油形成凝胶。生物相容性研究结果表明,两种柠檬酸酯在浓度为200mg/L时对微生物生长没有显著影响,具有良好的生物相容性。     

利用有机凝胶因子提高花生酱稳定性的工艺研究

使用紫虫胶作为有机凝胶因子制备稳定型花生酱,并对其工艺条件进行优化。以析油率为指标,紫虫胶添加量、加热温度、加热时间和冷却温度为因素变量,进行响应面优化试验,得到了最优工艺条件,并进行了花生酱感官评鉴。结果表明,紫虫胶添加量为3.2%(w/w)、加热温度为90 ℃、加热时间为40 min、冷却温度为1 ℃时,制得的有机凝胶花生酱最稳定,此时析油率仅1.24%。在最优工艺条件下制备的有机凝胶花生酱与商品花生酱相比,析油率更低,感官品质更好。     

细菌纤维素合成菌株发酵条件的考察

菌株QAX0 2 1 9# 进行液态发酵可产生不溶性的凝胶膜 ,通过纤维素酶水解等实验确定其发酵产物为纤维素 ,同时研究了乙醇、溶氧含量、培养方式以及接种量对菌体合成纤维素的影响。结果为 :以 8%接种量 ,在发酵培养基中添加一定量的乙醇 ,可显著提高纤维素产量     

Pd/Ce0.6Zr0.4O2/Al2O3 as advanced materials for three-way catalysts: Part 1. Catalyst characterisation, thermal stability and catalytic activity in the reduction of NO by CO

Pd-loaded Ce_0.6Zr_0.4O₂ solid solutions supported on Al₂O₃ are investigated as catalysts for the reduction of NO by CO. The attention is focused on the role of the Ce_0.6Zr_0.4O₂ and of the Pd dispersion on the catalytic activity. The system shows a very high activity below 500 K, which is almost independent on the Pd dispersion. The high activity is attributed to a promoting effect of the Ce_0.6Zr_0.4O₂ on the NO conversion. Investigation of the influence of high temperature treatments disclosed a thermal stabilisation of both Ce_0.6Zr_0.4O₂ and Al₂O₃ in the Ce_0.6Zr_0.4O₂/Al₂O₃ system.     

The influence of nitrogen incorporation on the optical properties of anodic Ta2O5

Anodic oxides were grown on sputter-deposited Ta in different aqueous solutions. A photoelectrochemical investigation was performed in order to estimate the band gap of the films as a function of the anodizing bath composition and formation voltage, i.e. thickness. Photoelectrochemical results provided evidence of sub-band gap photocurrent for films formed in a bath containing ammonium ions at pH 9. Elemental depth profiles obtained by glow discharge optical emission spectroscopy revealed the presence of nitrogen species in the outer part of the anodic films, which is bonded to Ta according to XPS analysis. A mechanism of nitrogen incorporation is proposed in order to account for the pH dependence of film composition.     

APOB CRISPR-Cas9 Engineering in Hypobetalipoproteinemia: A Promising Tool for Functional Studies of Novel Variants

Hypobetalipoproteinemia is characterized by LDL-cholesterol and apolipoprotein B (apoB) plasma levels below the fifth percentile for age and sex. Familial hypobetalipoproteinemia (FHBL) is mostly caused by premature termination codons in the APOB gene, a condition associated with fatty liver and steatohepatitis. Nevertheless, many families with a FHBL phenotype carry APOB missense variants of uncertain significance (VUS). We here aimed to develop a proof-of-principle experiment to assess the pathogenicity of VUS using the genome editing of human liver cells. We identified a novel heterozygous APOB-VUS (p.Leu351Arg), in a FHBL family. We generated APOB knock-out (KO) and APOB-p.Leu351Arg knock-in Huh7 cells using CRISPR-Cas9 technology and studied the APOB expression, synthesis and secretion by digital droplet PCR and ELISA quantification. The APOB expression was decreased by 70% in the heterozygous APOB-KO cells and almost abolished in the homozygous-KO cells, with a consistent decrease in apoB production and secretion. The APOB-p.Leu351Arg homozygous cells presented with a 40% decreased APOB expression and undetectable apoB levels in cellular extracts and supernatant. Thus, the p.Leu351Arg affected the apoB secretion, which led us to classify this new variant as likely pathogenic and to set up a hepatic follow-up in this family. Therefore, the functional assessment of APOB-missense variants, using gene-editing technologies, will lead to improvements in the molecular diagnosis of FHBL and the personalized follow-up of these patients.