免疫亲和柱净化/柱前衍生化-高效液相色谱荧光检测法测定粮谷中的T-2毒素

建立了免疫亲和柱净化/柱前衍生化-高效液相色谱荧光检测器测定粮谷中T-2毒素含量的方法。样品经甲醇-水(体积比为80∶20)混合溶剂提取,通过免疫亲和柱(IAC)净化,以氰酸蒽(1-AN)为衍生化试剂、4-二甲基氨基吡啶(DMAP)为催化剂进行衍生,以ZORBAX Eclipse XDB-C18 柱为分离柱,乙腈-水(体积比为80∶20)为流动相进行高效液相色谱分离及荧光检测，荧光检测的激发波长为381 nm，发射波长为470 nm。T-2毒素的质量浓度为0.01~1.5 mg/L时与峰高呈良好的线性,相关系数为0.9985。在0.01~1.5 μg/g添加水平下，回收率为79.7%~94.5%,相对标准偏差小于7%；检出限（S/N＝3）为0.01 μg/g。该方法净化效果好,灵敏度高,操作简便快速。     

Synthesis of [18F]F-γ-T-3, a Redox-Silent γ-Tocotrienol (γ-T-3) Vitamin E Analogue for Image-Based In Vivo Studies of Vitamin E Biodistribution and Dynamics

Vitamin E, a natural antioxidant, is of interest to scientists, health care pundits and faddists; its nutritional and biomedical attributes may be validated, anecdotal or fantasy. Vitamin E is a mixture of tocopherols (TPs) and tocotrienols (T-3s), each class having four substitutional isomers (α-, β-, γ-, δ-). Vitamin E analogues attain only low concentrations in most tissues, necessitating exacting invasive techniques for analytical research. Quantitative positron emission tomography (PET) with an F-18-labeled molecular probe would expedite access to Vitamin E’s biodistributions and pharmacokinetics via non-invasive temporal imaging. (R)-6-(3-[¹⁸F]Fluoropropoxy)-2,7,8-trimethyl-2-(4,8,12-trimethyltrideca-3,7,11-trien-1-yl)-chromane ([¹⁸F]F-γ-T-3) was prepared for this purpose. [¹⁸F]F-γ-T-3 was synthesized from γ-T-3 in two steps: (i) 1,3-di-O-tosylpropane was introduced at C6-O to form TsO-γ-T-3, and (ii) reaction of this tosylate with [¹⁸F]fluoride in DMF/K₂₂₂. Non-radioactive F-γ-T-3 was synthesized by reaction of γ-T-3 with 3-fluoropropyl methanesulfonate. [¹⁸F]F-γ-T-3 biodistribution in a murine tumor model was imaged using a small-animal PET scanner. F-γ-T-3 was prepared in 61% chemical yield. [¹⁸F]F-γ-T-3 was synthesized in acceptable radiochemical yield (RCY 12%) with high radiochemical purity (>99% RCP) in 45 min. Preliminary F-18 PET images in mice showed upper abdominal accumulation with evidence of renal clearance, only low concentrations in the thorax (lung/heart) and head, and rapid clearance from blood. [¹⁸F]F-γ-T-3 shows promise as an F-18 PET tracer for detailed in vivo studies of Vitamin E. The labeling procedure provides acceptable RCY, high RCP and pertinence to all eight Vitamin E analogues.     

铸型尼龙端面扭动与滑动摩擦学行为研究

为研究端面扭动摩擦特性,研制了端面扭动摩擦特性测量装置,进行了玻璃纤维增强铸型尼龙（MC尼龙）复合材料与45#钢在123 N法向载荷下的扭动与滑动摩擦学试验,扭动角位移幅值为60°和90°,使用扫描电镜观察MC尼龙复合材料磨损表面形貌,采用光学显微镜观察45#钢偶副表面转移膜形貌.结果表明：扭动摩擦的扭矩-角位移（T-θ）曲线随着循环次数的增加保持平行四边形,而摩擦扭矩随之升高;扭动状态下的摩擦系数高于滑动摩擦系数,扭动磨损后MC尼龙试样质量增加;滑动状态下的磨损机理主要为塑性变形和疲劳磨损,扭动状态下的磨损机理为更为严重的黏着磨损和疲劳磨损;滑动摩擦状态下,45#钢偶副表面形成了大面积连续的转移膜,扭动状态下,45#钢偶副表面只在接触中心区域有少量条块状转移物质.     

Bestimmung von T-2-Toxin in pflanzlichen Nahrungsmitteln

Zusammenfassung Ein Verfahren zur quantitativen Bestimmung von T-2-Toxin in verschimmeltem Reis bzw. Mais durch Extraktion, dünnschicht-chromatographische Trennung und Fluorescenzintensitätsmessung der mit H₂SO₄ behandelten DC-Platte wird vorgestellt. Fluorescenzabsorptions- und Fluorescenzemissionsspektrum werden angegeben. Die Abhängigkeit der Mycotoxinkonzentration von der Fluorescenzintensität wird durch eine Gleichung beschrieben. Die analytische Detektion von T-2-Toxin läßt sich durch ein 4-(p-Nitrobenzyl)pyridin-Derivat und dessen Absorptionsspektrum bestätigen. Versuche mit zugesetztem T-2-Toxin zeigten einen Analysenfehler von weniger als 10%.

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Determination of T-2-toxin in vegetable foodstuffs1. T-2-toxin in mouldy rice and maize

Summary A procedure is described for the determination of T-2 toxin in extracts from mouldy rice and maize by thin-layer chromatography (TLC) and subsequent fluorescence intensity measurement of the H₂SO₄-treated TLC plates. The fluorescence absorption and emission spectra are presented. The dependence of the concentration of the mycotoxin on fluorescence intensity is described by an equation. The detection of T-2 toxin can be confirmed by colour reaction with 4-(p-nitrobenzyl)pyridine yielding a blue derivative. Experiments with added toxin revealed an analytical error smaller than 10%.

     

Filling polygonal holes with minimal energy surfaces on Powell-Sabin type triangulations

In this paper we present two different methods for filling in a hole in an explicit 3D surface, defined by a smooth function f in a part of a polygonal domain D⊂R². We obtain the final reconstructed surface over the whole domain D. We do the filling in two different ways: discontinuous and continuous. In the discontinuous case, we fill the hole with a function in a Powell-Sabin spline space that minimizes a linear combination of the usual seminorms in an adequate Sobolev space, and approximates (in the least squares sense) the values of f and those of its normal derivatives at an adequate set of points. In the continuous case, we will first replace f outside the hole by a smoothing bivariate spline s_f, and then we fill the hole also with a Powell-Sabin spline minimizing a linear combination of given seminorms. In both cases, we obtain existence and uniqueness of solutions and we present some graphical examples, and, in the continuous case, we also give a local convergence result.     

农产品与饲料中T-2毒素免疫亲和柱净化-液相色谱串联质谱检测技术研究

利用T-2毒素单克隆抗体2G7和CNBr活化的Sepharose 4B研制出T-2免疫亲和柱,考察了T-2免疫亲和柱的最佳应用条件。利用免疫亲和柱,建立了农产品与饲料中T-2毒素免疫亲和柱净化/液相色谱-串联质谱(IAC/LC-MS/MS)确证性检测技术,并考察该方法的准确度和精密度。结果表明,T-2毒素在0.5~500.0 ng/g范围内线性关系良好,相关系数为0.999 7,检出限为0.05 ng/g,定量下限为0.17 ng/g。大米、玉米、饲料样品在T-2毒素10,50,100 ng/g的加标水平下,回收率为92.9%~109.7%,相对标准偏差为2.1%~8.3%。对市售36份农产品与饲料样品进行测定,检测结果的相对标准偏差均小于10.0%。     

Antitumor activity on human bladder cancer T-24 cells and composition analysis of the core of Camellia osmantha fruit

Abstract

In this study, antitumor activity and composition analysis of the core of Camellia osmantha fruit were investigated. The cores were extracted by 80% ethanol to obtain the crude extract (TF), which was successively distributed by different concentrations of ethanol with MCI resin to obtain three different parts (Frs 1 to 3). Cytotoxicity activities showed that TF, Fr-2, and Fr-3 exhibited good inhibition against T-24 with IC₅₀ values of 6.7 ± 1.3, 6.9 ± 0.9, and 6.7 ± 1.7 μg/mL, respectively. Fr-3 has a strong inhibitory activity on T-24 cells, mainly due to effectively increasing the release of intracellular calcium ions and reactive oxygen species. In addition, Fr-3 can inhibit T-24 cells migration and invasion. Further composition analysis on Fr-3 was detected by LC-Q-TOFMS implying the main components to be ellagic acid and its derivatives.     

Characterization of (<Superscript>13</Superscript>C<Subscript>24</Subscript>) T-2 toxin and its use as an internal standard for the quantification of T-2 toxin in cereals with HPLC–MS/MS

In this paper, the structure and the identity of fully ¹³C-substituted T-2 toxin were confirmed using high-resolution mass spectrometry, ¹H-NMR, ¹³C-NMR, tandem mass spectrometry and HPLC–DAD. The purity of this compound was estimated to be at least 98.8% according to UV data. The isotopic distribution of (¹³C₂₄) T-2 toxin indicated a total isotopic enrichment of 98.2 ± 1.0 atom% ¹³C, and the application of different MS measurement modes revealed the MS/MS fragmentation pattern of T-2 toxin. Furthermore, a stable isotope dilution mass spectrometry method for the quantification of T-2 toxin was developed using (¹³C₂₄) T-2 toxin as internal standard. The method was evaluated with and without conventional clean-up and validated for maize and oats. Both cereals showed strong matrix enhancement effects, which could be compensated for through the application of the isotope-substituted internal standard.     

2-(Diphenylacetyl)-1,3-Indanedione-1-Hydrazone (Dipain) Derivatives for Detection of Trichothecene Mycotoxins

Abstract

2-(Diphenylacetyl)-1,3-indanedione-1-hydrazone and its derivatives where the NH₂ has been replaced by a substituted NH or an imino group give fluoresence enhancement with trichothecene mycotoxins. Absolute amounts of T-2 toxin as low as 50 ng are detectable. Detection limits for HT-2, Diacetoxyscirpenol, Neosolaniol, and Fusarenon-X range from 0.1 to 4μg.

The advantage in using 2-(diphenylacetyl)-1,3-indanedione-1-hydrazone (DIPAIN) derivatives for the detection of trichothecene mycotoxins is that response time is based on the rate of formation of a molecular association complex between the toxin and the detector reagent rather than on the chemical reactivity of the toxin. Hence, sensitive detection or mycotoxins can be achieved simply and rapidly at 25°C.

Since DlPAlN derivatives have been found to be direct-acting reagents capable of detecting droplets of dissolved trichothecenes, it is speculated that they may be useful as coatings in optical waveguide devices or in other devices that are developed as field detectors for aerosols that contain trichothecene mycotoxins. The DlPAlN reagents may also be used in kits that are designed to detect surface contamination by trichothecene mycotoxins.     

Acceleration statistics of inertial particles in turbulent flow

Turbulent transport of material inclusions plays an important role in many natural and industrial situations. Being able to accurately model and predict the dynamics of dispersed particles transported by a turbulent carrier flow, remains a challenge. One critical and difficult point is to develop models which correctly describe the dynamics of particles over a wide range of sizes and densities. Our measurements show that acceleration statistics of particles dispersed in a turbulent flow do exhibit specific, and so far unpredicted, size and density effects and that they preserve an extremely robust turbulent signature with lognormal fluctuations, regardless of particles size and density. This has important consequences in terms of modeling for the turbulent transport of dispersed inclusions.