基于α-叔碳-β,γ-不饱和醛的制备全合成番茄红素

将一种α-取代-α,β-不饱和醛的制备方法应用于番茄红素(Ⅵ)的全合成中,通过该法以廉价的原料假性紫罗兰酮(Ⅰ)制备了2,6,10-三甲基-3,5,9-十一烷三烯-1-醛(Ⅱ),然后与四乙基亚甲基二磷酸酯(Ⅲ)经过Wittig-Horner反应得到关键中间体3,7,11-三甲基-1,4,6,10-四烯十二烷基膦酸二乙酯(Ⅳ),最终和2,7-二甲基-2,4,6-辛三烯-1,8-二醛(Ⅴ)进行Wittig-Horner反应、转位异构合成全反式番茄红素。反应共经历3步线性反应,总产率为37.0%。最终产物的结构采用IR、HRMS和NMR进行确证。     

Electrochemical growth of tin(II) oxide films: Application in photocatalytic degradation of methylene blue

We have investigated the semiconducting and photoelectrochemical properties of SnO films grown potentiostatically on tin substrate. The oxide is characterized by X-ray diffraction, scanning electron microscopy and Raman spectroscopy. The anodic process corresponds to the formation of SnO·nH₂O pre-passive layer that is removed upon increasing potential due to surface etching at the metal/oxide interface. SnO films deposited for long durations (>50 mn) are uniform and well adhered; they thicken up to ~50 nm by diffusion-controlled process and the growth follows a direct logarithmic law. The thickness is determined by coulometry and the X-ray diffraction indicates the tetragonal SnO phase (SG: P4/mmm) with a crystallite size of 32 nm. The Mott–Schottky plot is characteristic of n type conductivity with an electrons density of 5.72×10¹⁸ cm⁻³, a flat band potential of −0.09 V_SCE and a depletion width of ~10 nm. The valence band, located at 5.91 eV below, vacuum is made up of hybridized O²⁻:2p Sn²⁺:5s while the conduction band (4.45 eV) derives from Sn²⁺:5p orbital. The electrochemical impedance spectroscopy (EIS) measured in the range (10⁻²–10⁵ Hz) shows the contribution of the bulk and grain boundaries. The energy band diagram predicts the photodegradation of methylene blue on SnO films. 67% of the initial concentration (10 mg L⁻¹) disappears after 3 h of exposure to visible light (9 mW cm⁻²) with a quantum yield of 0.072.     

A reliable and sensitive time-resolved fluorescent immunochromatographic assay (TRFICA) for ochratoxin A in agro-products

Immunochromatographic assays (ICAs) are considered as a suitable diagnostic tool for the detection of mycotoxins. Mycotoxins and especially, ochratoxin A are analytes with more demanding sensitivity requirements. To enhance the sensitivity of current immunochromatographic assays for ochratoxin A (OTA), a novel sensitive ICA was developed in this study. In the assay, microspheres enclosing fluorescent europium (III) [Eu(III)] nanoparticles (EuNPs) were used as a label for OTA monoclonal antibody (OTA-mAb) conjugation. Accordingly, assay was called time-resolved fluorescent immunochromatographic assay (TRFICA). The test strip was composed of three parts: a sample pad, nitrocellulose membrane and an absorbent pad. As for detection, a proper concentration of conjugated microspheres was pipetted into the microtube and sample extract was added to it. Then the strip was inserted into the tube and the fluid flow along the strip. The TRFICA results were obtained in 8 min and read by a portable TRFICA strip reader. The established method allows quantitative determination of OTA with limit of detection as low as 1.0 μg kg⁻¹ in the samples. For validation, spiked samples including wheat, maize, soybean and rice were respectively assayed by TRFICA and a standard high performance liquid chromatography equipped with a fluorescence detector (HPLC-FLD), and good agreement of results was obtained between two methods.     

电感耦合等离子体质谱法测定小麦粉中铅及其不确定度评定

通过建立数学模型,对电感耦合等离子体质谱法测定小麦粉中的铅的进行不确定度评定。分析并计算了各不确定度分量,计算合成标准不确定度和扩展不确定度。结果表明,方法测量不确定度主要由曲线校正和样品测试重复性引入,而定容体积和称样过程的不确定度可忽略不计。     

Annular denuder method for sampling reactive gases and aerosols in the atmosphere

The annular denuder method (ADM), consisting of a denuder-filter pack assembly, has been developed to measure several gaseous and aerosol species without sampling artifacts. Its application to the determination of gaseous acids and ammonia in the atmosphere indicates that this aim is achieved, even though the ratio of analytes in the gas phase and particulate matter is extremely low. The procedure is particularly suitable for the measurement of trace levels (0.1 μg m⁻³) of HNO₃ and SO₂ (even in the presence of high levels of sulfate and nitrate) as well as of HNO₂ (by making correction for the positive interference of NO₂ and PAN).The ADM sampling and analysis precision for the examined gases does not exceed ±10% in the 0.1–10 μg m⁻³ range. By sampling at an air flow rate of 151 min⁻¹, the minimum detectable atmospheric concentrations is ∼0.1 μgm⁻³ for each species over a 3 h interval.     

基于GRA-ISM-HMM的广州市肉及肉制品安全风险评估

该研究旨在利用广州食品安全风险监测2015年至2020年针对肉及肉制品样本的检测数据,构建肉及肉制品的安全风险评估模型,从而了解广州市该段时间内肉及肉制品的食品安全风险及其时变特点。该研究采取灰色关联分析方法和解释结构模型建立风险指数,并基于该指标值作为隐马尔可夫模型的观测值探讨观测背后的隐含风险状态。分析结果显示,2015~2020年所有样本综合风险指数结果都在[0,0.45]之间,总体风险都较小,其中2019年风险最高;将风险指数进行等级划分,显示2015~2020年风险等级为[1, 2, 2, 2, 3, 1];通过HMM分析得到这六年的隐藏风险等级为[0, 1, 1, 1, 2, 0],与观测风险结果一致,且HMM预测2021年风险等级为1,即表明广州肉及肉制品风险往良好态势发展。最后,进行风险差异原因分析,发现各肉制品分类之间有差异,其中腊肠、鸡肉和腊肉的风险指数较高于其他种类,而2019年增加腊肠和腊肉的检测是风险增加的一个原因。总体来说,广州肉及肉制品风险较小,但依旧需要监督改善。     

电感耦合等离子体质谱鉴别潲水油方法研究

通过湿法消解和温水浸提处理样品市售合格食用油和不同来源潲水油样品后,采用电感耦合等离子体质谱检测样品金属元素含量。结果显示：不同来源潲水油和合格食用油Na、Al等金属元素含量检测结果比较差异有统计学意义（p〈0.05）;温水浸提法处理潲水油样品后用ICP-MS法检测Na、Al等金属元素含量,可满足不同来源潲水油样品和样品快速检测需求。     

2006-2008年广州市食源性疾病暴发监测分析

目的分析2006-2008年广州市食源性疾病暴发的特征,提出针对性的防控策略和措施。方法确定食源性疾病暴发的标准,利用食源性疾病暴发监测与报告系统收集2006-2008年暴发资料,建立excel食源性疾病暴发数据库,按季节、月份、致病因素、致病食品、就餐场所、引发因素等进行分析。结果2006-2008年食源性疾病暴发共189起,发病2678例,死亡6例,平均每起发病14.17例,罹患率13.47%,病死率0.22%。查明致病因素共166起,占总数的87.83%;微生物性暴发起数和发病人数最多,分别占总数的58.20%和70.95%;有毒动植物性暴发死亡人数最多,占总数的66.67%。微生物性(17.27例)平均每起患者数最多;化学性罹患率(91.83%)最高;有毒动植物性病死率(1.86%)最高。结论应提高食源性疾病暴发监测与报告系统的效率和质量,开展针对性防控,降低食源性疾病负担。     

食品中大肠杆菌0157: H7的几种检测方法的比较

目的 评估平板分离培养法、免疫磁珠分离(IMS)法、VIDAS全自动酶标免疫测试系统、BAX全自动病原菌检测系统及环介导等温扩增(LAMP)技术在食品中检验肠出血型大肠埃希菌0157:H7的特异性、敏感性.方法 使用平板分离培养法、免疫磁珠分离法、VIDAS法、BAX法及LAMP法对人工制备的染菌猪肉样本进行检测,并对这几种方法进行比较.结果 BAX法和LAMP法的检出率最高,分别是89.1％和85.9％,免疫磁珠法和VIDAS法检出率次之,分别是75.0％和78.1％,传统分离培养法为43.8％.结论 BAX法和LAMP法具有快速、高效、特异性好、敏感性高的特点,可快速筛选食品中可能存在的肠出血型大肠埃希菌0157∶H7.