UPLC-MS/MS法同时测定减肥食品中55种非法添加物

目的 建立超高效液相色谱-串联质谱同时测定减肥类食品中55种非法添加物的分析方法。方法 样品经甲醇超声提取后,采用Agilent Eclipse Plus C₁₈ RRHD色谱柱(2.1 mm×100 mm,1.8μm)分离,以乙腈-0.1%甲酸为流动相进行梯度洗脱。在正负离子扫描条件下,采用动态多反应监测模式监测。结果 55种非法添加药物在相应的线性范围内均呈现良好线性关系,相关系数大于0.995,平均回收率75.2%～121.6%,相对标准偏差<12%,各化学药物的检测限在0.02～1.25μg/g。应用该方法对50批样品进行了检测,其中有38批次样品检出托拉塞米、大黄素、西布曲明、N-单去甲基西布曲明、N,N-双去甲基西布曲明、比沙可啶、麻黄碱、甲基麻黄碱、氢氯噻嗪、氟西汀等非法添加物。结论 该方法简单、快速、灵敏、准确、高效,兼具定性定量检测的优点,可用于食品中减肥类化学药物的高通量检测。     

The synthesis,electrochemical and theoretical nonlinear optical properties of push–pull chromophores for photorefractive composites

Four chromophores, of different dipole moment and polarizable anisotropy and which comprised conjugation bridges of both benzene and polyene with strong electron-donor and electron-acceptor groups, were characterized using ¹H NMR, FT-IR, UV–vis, and electrochemical analyses. The electric dipole moment (μ), polarizability (α) and the first hyperpolarizability (β) values of the chromophores were examined using computational methods. The contribution of orientational birefringence to total birefringence was estimated from the calculated molecular parameters of the chromophores; these parameters are important factors for predicting photorefractive efficiency.     

枸杞多糖特性和单糖组成及木糖醇含量的分析

目的 多种分析方法联合分析枸杞多糖特性和单糖组成及木糖醇含量。方法 枸杞干果采用水提醇沉的方法提取枸杞多糖,计算提取率。建立凝胶渗透色谱-示差检测-多角度激光光散射法测定枸杞多糖分子量及分子量分布;再将提取的枸杞多糖经三氟乙酸水解为单糖,建立高效阴离子色谱-积分脉冲安培法测定水解后的阿拉伯糖、鼠李糖、半乳糖、葡萄糖、甘露糖、果糖、木糖、岩藻糖、核糖9种单糖和木糖醇。结果 采用本法检测宁夏地区的10批枸杞,枸杞多糖得率为1.86%～3.21%;10批枸杞多糖的重均相对分子量为9.12×10⁵～3.65×10⁶ Da,离子色谱法检测10批枸杞中单糖和木糖醇含量从高到低依次为阿拉伯糖、葡萄糖、鼠李糖、半乳糖、甘露糖、果糖、木糖醇及岩藻糖。结论 本文对枸杞多糖的重均分子量及单糖组成、含量进行初步研究,与现行质量标准中检测方法相比,控制指标更加全面、客观、准确,为建立枸杞多糖的质量控制方法提供技术参考。     

Review of the structural characterization,quality evaluation,and industrial application of Lycium barbarum polysaccharides

BackgroundLycium barbarum polysaccharides (LBPs) are considered to be the major bioactive components in L. barbarum. Due to the considerable health benefits of LBPs, and the significant research interest in LBPs, quality evaluation of LBPs and their related products is imperative for ensuring their efficacy and safety. The bioactivities of polysaccharides are closely associated with their physicochemical properties, which can be easily monitored via chemical techniques. Therefore, analysis of physicochemical properties is a more straightforward and viable approach for the quality control of polysaccharides.Scope and approachIn this review, special techniques for the structural characterization of LBPs are summarized and discussed. In addition, quality evaluation approaches of LBPs that have never been emphasized are highlighted herein. Furthermore, industrial applications of LBPs are reviewed and discussed.Key findings and conclusionsHigh-performance anion-exchange chromatography coupled with pulsed amperometric detection is one of the most effective techniques for analysis of both acidic and neutral LBPs. Size-exclusion chromatography coupled with multi-angle laser light scattering and refractive index detection is able to determine absolute molecular weights, chain conformations, and contents of LBPs. Fingerprinting analysis and saccharide mapping analysis are effective approaches for quality evaluation of LBPs. However, the lack of appropriate quality evaluation approaches indicates an unreliable regulation of LBPs and their related products. This reveals the deficiency in the quality control of commercial products. Thus, the development of reliable approaches for pharmacological activity-based quality control of LBPs and their related products must be extensively investigated.     

Minimizing the effect of density in determination of particle aerodynamic diameter using a time of flight instrument

Particle aerodynamic diameter measurement using an aerosizer (a time-of-flight (TOF) particle size measurement instrument) requires assuming the density of particle being measured. In this paper, a relationship between TOF of spherical particles with different densities through three laser beams, and the lumped parameter, Log[d_aeC_D^−1/2], is found. This allows the effect of density in particle aerodynamic diameter measurement to be minimized.     

Effect of malt pretreatment on phytic acid and in vitro protein digestibility of sorghum flour

Sorghum seeds of cultivar Wad Ahemed (phytate: 2.7 mg/g, tannin: 0.96% and 2 h pepsin digestion: 18%) were germinated for three days to obtain 1-, 2- and 3- days old sorghum malts. Sorghum malt was added in concentrations of 1, 2.5, 5, 7.5 or 10% to sorghum flour. The mixtures were incubated with shaking for 0, 30, 60, 90 or 120 min. Phytic acid and in vitro protein digestibility were assayed for all treatments. The results revealed that phytate content was significantly reduced. The 10% 3-day-old malt after 120 min incubation, reduced the phytate content by 83%. The in vitro protein digestibility (IVPD) was significantly improved as a result of malt pretreatment. The rate of reduction of phytate content and the rate of increment in IVPD increased with time of incubation, age and concentration of the malt.     

丁香酚在水产品中的残留及风险评估研究进展

受我国南北气候、地理环境和养殖条件的限制,鲜活水产品为满足不同市场的需求,需要经过长途运输。而运输过程中鲜活水产品受应激胁迫、机体受伤感染、水质恶化等因素影响,不仅引起水产品存活率降低,而且造成产品质量下降。丁香酚有较强的麻醉作用,广泛应用于口腔牙科麻醉,现也作为渔用麻醉剂应用到鲜活水产品运输过程中。虽然我国逐渐开展丁香酚应用、残留检测、风险评估等方面的研究,但关于水产品中麻醉剂丁香酚从应用到残留风险评估的综合性研究综述较少。本文旨在通过对丁香酚国内外标准规定、使用现状、麻醉机理和应用、残留检测方法、残留风险评估以及前景展望等方面进行说明和探讨,以期为我国丁香酚在水产养殖运输环节中的合理使用提供依据和参考。     

An immunoassay for ochratoxin A without the mycotoxin

Phage display peptide libraries allow the selection of new molecules capable of mimicking the structural and functional features of native proteins or chemicals. This technology can be applied to developing new reagents, which may serve as the surrogate of the original objects. In order to screen peptides capable of mimicking ochratoxin A (OTA) in the interaction with anti-OTA monoclonal antibody (McAb) and establish the immunoassay for OTA, an anti-OTA McAb was used as the target for panning-elution selection from a phage random seven-peptide library. After four rounds of panning, 11 phages were found to be able to mimic OTA in binding with the antibody. Enzyme-linked Immunosorbent Assay (ELISA) for detecting OTA was established with the phages. In the most sensitive assay, the linear range of the inhibition curve was 200–8000 pg/ml; the detection limit was 150 pg/ml. The inserted peptide sequences were deduced by DNA sequencing. The common amino acid residue sequence was IR(V)PMV(L)XX (X is any amino acid residues), which was verified by two synthesized peptides. The results demonstrated that those phage peptides could be used as the surrogate of OTA to establish the immunoassay.     

Efficient separation and quantitative detection of Listeria monocytogenes based on screen-printed interdigitated electrode,urease and magnetic nanoparticles

Rapid screening of pathogenic bacteria contaminated foods is the key to prevent and control the outbreaks of foodborne illness. In this study, an impedance biosensor was developed using immunomagnetic nanoparticles for efficient separation and concentration of the Listeria monocytogenes cells, urease for amplifying the weak signal, and screen-printed interdigitated electrode for quantitative measurement of the impedance change of the catalysate. The magnetic nanoparticles (MNPs) coated by the monoclonal antibodies (MAbs) were used to separate the Listeria cells from the background and concentrate them in small volume of PBS. Then, the gold nanoparticles (GNPs) modified with the urease and the polyclonal antibodies (PAbs) were used to react with Listeria to form the MNP-Listeria-GNP sandwich complexes. The complexes were re-suspended with the urea to catalyze the hydrolysis of the urea into ammonium ions and carbonate ions, which were measured by the electrode. A new equivalent circuit was designed for simulation of the biosensor with a good fitting result. Under the optimized conditions, a linear relationship between the impedance changes and the concentrations of Listeria from 1.9 × 10³ to 1.9 × 10⁶ CFU/mL was obtained. The limit of detection of this biosensor was 1.6 × 10³ CFU/mL and the recovery of the spiked lettuce sample ranges from 94.7% to 103.8%. This proposed biosensor was developed at much lower cost than our previous studies and could be more applicable for in-field detection of foodborne pathogens.