磺酰脲类除草剂分子印迹聚合物制备及其应用

采用沉淀聚合法,以甲磺隆和氯磺隆为双模板分子,4-乙烯基吡啶为功能单体,二乙烯基苯为交联剂,乙腈为致孔剂,合成对29 种磺酰脲类农药具有高选择性的分子印迹聚合物。通过扫描电镜、平衡吸附实验等对制备的印迹聚合物进行表征和测定。结果表明：分子印迹聚合物对29 种磺酰脲类农药具有特异性吸附作用,其最大表观结合量为13.21 mg/g。以此合成的聚合物作为吸附材料制备固相萃取柱,进一步建立了分子印迹固相萃取-高效液相色谱-串联质谱法,用于测定农产品中29 种磺酰脲类农药残留。该方法在2～100 μg/L 范围内,磺酰脲类除草剂峰面积与质量浓度呈良好的线性关系,相关系数（R2）大于0.999,定量限为10 μg/kg。在不同添加水平下,样品中磺酰脲类除草剂的加标回收率在74.8%～110.5%之间,相对标准偏差不高于5.3%。     

有机氟防水剂的合成研究

以丙烯酸十二氟庚酯(G04)、甲基丙烯酸甲酯(MMA)、丙烯酸丁酯(BA)作为主要单体,壬基酚聚氧乙烯醚(NP40)和十二烷基苯磺酸钠(SDBS)为复配乳化剂,过硫酸铵(APS)为引发剂,分析了不同聚合方式制备的含氟丙烯酸酯共聚物乳液性能。实验表明,合成有机氟防水剂的优化工艺为:BA与MMA的比例为3∶2,含固量为30%,引发剂用量为0.6%时所制备的含氟丙烯酸酯共聚物具有最优的性能。     

Analysis of the volatile constituents of black chokeberry (Aronia melanocarpa Ell.)

The volatile constituents of black chokeberry were analysed by gas chromatography and mass spectrometry. Concentrations of the 48 compounds identified were in general below their individual threshold values. The main compounds were benzaldehyde cyanohydrin, hydrocyanic acid and benzaldehyde. Among other benzene derivatives identified in the press juice were benzylalcohol, 2-phenylethanol, phenylacetaldehyde, salicylaldehyde, acetophenone, 2′-hydroxyacetophenone, 4′-methoxyacetophenone, phenol, 2-methoxyphenol and methyl benzoate.     

新型聚丙烯酸浆料黏度和黏附性影响因素

为满足在纺织上浆中对浆液黏度热稳定性和黏附力的要求,选用丙烯酸、丙烯酰胺、甲基丙烯酸甲酯、丙烯酸乙酯和丙烯酸丁酯为原料,十二烷基硫酸钠(SDS)和OP-10为复合乳化剂,过硫酸铵(APS)为引发剂,采用乳液聚合法制备了一种新型聚丙烯酸类浆料。讨论乳化剂、引发剂、反应温度、反应时间以及搅拌转速对浆液黏度和黏附性能的影响。得到制备的最佳工艺条件:乳化剂质量分数为3%,引发剂质量分数为0.9%,反应温度为85℃,反应时间为3 h,搅拌转速为140 r/min。     

自交联性聚丙烯酸酯纸张增强剂的合成及应用研究

以丙烯酸丁酯、甲基丙烯酸甲酯、甲基丙烯酸和N-羟甲基丙烯酰胺为原料,采用半连续滴加的乳液聚合方式制备了纳米级的具有自交联性的聚丙烯酸酯乳液增强剂,并讨论了引发剂用量、复合乳化剂用量、反应单体配比、交联单体用量等对聚丙烯酸酯乳液性能的影响.结果表明:该乳液具有良好的稳定性,乳液的粒子粒径分布从85.9nm到110nm,能与水以任意比例互溶;将其用于阔叶木硫酸盐浆抄纸试验,可有效改善纸张的抗张指数、耐破指数和撕裂指数.     

Tetramethylsuccinonitrile in polyvinyl chloride products for food and its release into food-simulating solvents

The content of tetramethylsuccinonitrile (TMSN), the main decomposition product of 2,2'-azobis-isobutyronitrile, in polyvinyl chloride (PVC) products used for food packaging, were examined as well as food-simulating solvents. The TMSN concentration in 17 PVC products ranged from below the detection limit, 0.05 mg/kg, up to 523 mg/kg. The release of TMSN from two PVC products into five kinds of food-simulating solvents at 60 degrees C for 30 min was observed, except for 1 +/- 1 micrograms/kg of TMSN in n-heptane from a PVC bottle containing 523 +/- 30.4 mg/kg of TMSN. The detection limit of TMSN in the food-simulating solvents was 1 micrograms/kg. When pieces of the bottle were stored in olive oil at 40 degrees C for 120 days, 5 +/- 1 micrograms/kg of TMSN was detected in the oil. The release of TMSN from the pieces of the bottle into olive oil between 80 and 140 degrees C depended on the formula ln y = 0.08786x-5.696, r = 0.9927, where y is the concentration (microgram/kg) of TMSN in olive oil, x is the temperature (degrees C), and r is the correlation coefficient.     

Composition of Montmorency Cherry Essence. 2. High-boiling Components

SUMMARY: Volatile components of commercial Montmorency cherry essence boiling above ethanol were extracted from the essence by ether and concentrated by distillation. This concentrate was fractionated by gas chromatography. Individual components were identified using the methods of functional group analysis, gas co-chromatography, infrared analysis and mass spectrometry. The concentrations of the components in the original essence were estimated. The major components identified were n-propyl alcohol, isobutyl alcohol, isoamyl alcohol, and benzaldehyde. Minor components identified include n-butanol, n-hexanol, a hexenol, benzyl alcohol, α-terpineol, furfural, isoprene, myrcene and numerous higher terpenes, methyl benzoate, ethyl benzoate, benzyl acetate, ethyl caprylate, ethyl caprate, n-propyl benzoate, isobutyl benzoate, isoamyl benzoate and di-butyl phthalate.     

高分子微球免疫吸附剂的制备及其对黄曲霉毒素M1的吸附性能

制备用于牛乳中吸附黄曲霉毒M1的免疫吸附剂。以乙醇和水溶液为反应介质,聚乙烯吡咯烷酮为分散 剂,偶氮二异丁腈为引发剂,采用分散聚合法制备苯乙烯-甲基丙烯酸缩水甘油酯共聚物微球。利用微球表面的环 氧基团将抗黄曲霉毒M1的单克隆抗体固定在微球表面,获得免疫吸附剂。制备的微球粒径约为1.7 μm,微球中环氧 基量在67.2%～71.6%之间,制备的免疫吸附剂对乳中黄曲霉毒素M1的吸附量达1.2 μg/g以上。该免疫吸附剂对乳中 黄曲霉毒素M1的选择性吸附较好,是去除乳中黄曲霉毒素M1较理想的免疫吸附材料。     

Plant protection product residues in red grapes and Teran PTP wine

Between 2011 and 2013, a total of 73 grape and 82 wine samples from winegrowing district Kras (Karst) were analysed for plant protection product (PPP) residues. The samples were analysed for the presence of 215 different active compounds using two multiresidual analytical methods: gas chromatography coupled with mass spectrometry and liquid chromatography coupled with tandem mass spectrometry. Residues were found in 91.8% of all grape samples and in 67.1% of all wine samples. In all grape samples, residues were below maximum residue levels (MRLs) and 58.9% of all grape samples contained active substances at a level of less then 10% of the MRL. Nearly 33% of all Teran PTP wines did not contain PPP residues at all. Residues diminish during processing of grapes to wine, so their content in wine was low. Therefore, it could be concluded that grapes and wine in the winegrowing district Kras are safe for consumers.     

CPAM乳液的制备及其对漂白麦草浆助留助滤性能的影响

以丙烯酰胺(AM)和丙烯酸乙酯基三甲基氯化铵(DAC)为共聚单体,采用分散聚合法在无机盐水溶液中得到了性能稳定的聚合物乳液。产物的红外光谱、DSC曲线及粒径分析表明,这种分散聚合法在制备阳离子聚丙烯酰胺(CPAM)乳液上是成功的。将所得CPAM用于漂白麦草浆,实验结果表明,自制的CPAM能显著提高浆料中填料的留着率并改善浆料的滤水性能。     

含氟丙烯酸酯防水剂的合成及应用

以甲基丙烯酸甲酯（MMA）、丙烯酸丁酯（BA）为单体,脂肪醇聚氧乙烯醚（AEO-9）和十二烷基硫酸钠（SDS）为复合乳化剂,过硫酸铵（APS）为引发剂,采用乳液聚合方法制备含氟防水整理剂乳液。结果表明：当m（BA）：m（MMA）=3：2,乳化剂用量为6％,引发剂用量为0．6％（均为对单体总质量）,制得的聚合物乳液外观透亮、细腻、稳定性好。经该防水整理剂整理后的棉织物对水的接触角可达140°。     

造纸用苯乙烯-丙烯酸丁酯-甲基丙烯酸甲酯三元共聚乳液的合成

介绍了以苯乙烯、丙烯酸丁酯和甲基丙烯酸甲酯为反应单体,过硫酸铵为引发剂,十二烷基磺酸钠/OP-10为乳化剂的三元共聚乳液的合成工艺。对单体、引发剂、乳化剂及温度对乳液性能的影响进行了讨论。结果表明,引入适量的甲基丙烯酸甲酯,能有效地提高成膜的硬度、透光性、抗水性,同时还可赋予膜一定的韧性。     

阳离子聚丙烯酰胺乳液的制备及其助滤性能

以丙烯酰胺（AM）和丙烯酰氧乙基三甲基氯化铵（DAC）为共聚单体．采用分散聚合法在无机盐水溶液中得到了性能稳定的聚合物乳液。对所得产物进行红外光谱和粒径分析，并将所得阳离子聚丙烯酰胺（CPAM）用于漂白麦草浆试验，结果表明，自制的CPAM能显著提高浆料中填料的留着率并改善浆料的滤水性能。     

阳离子聚丙烯酰胺乳液的制备及其助留助滤性能

以丙烯酰胺(AM)和丙烯酰氧乙基三甲基氯化铵(DAC)为共聚单体,采用分散聚合法在无机盐水溶液中得到了性能稳定的聚合物乳液。对所得产物进行红外光谱和粒径分析,并将所得阳离子聚丙烯酰胺(CPAM)用于漂白麦草浆试验,结果表明,自制的CPAM能显著提高浆料中填料的留着率并改善浆料的滤水性能。     

Synthesis and utilisation of molecular imprinting polymer for clean-up of propachlor in food and environmental media

The molecularly imprinted polymers (MIPs) are used as the base material of solid phase extraction (SPE) for the separation and concentration of the propachlor herbicide (Prop) in different environmental matrix. Accordingly, we prepared MIPs on the surface of modified silica gel using propachlor as a template, acrylamide (AA) as functional monomers, ethylene glycol dimethacrylate (EGDMA) as a cross-linker and 2,2-azo-bis-isobutyronitrile (AIBN) as an initiator. The MIP structure was characterised using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR). Synthesised MIPs had a specific ability to detect the template Prop. The high selectivity solid phase extraction cartridges of molecularly imprinted polymers (MISPE) containing MIP Prop particles were prepared. The optimised Prop-MISPE procedure was developed for enrichment or clean-up of propachlor residues in water, soil and rice samples. Concentrations of propachlor in the samples were analysed by high performance liquid chromatography. Overall, the newly developed technique provides an analytical platform to quantify the trace amount of propachlor residues in multi or complex environmental and food media.     

Identification of organic contaminants in disposable aluminium foil containers

A series of disposable aluminium foil containers designed for cooking and packaging foods and available on the Italian market were investigated. Using different analytical techniques (near infrared (NIR), High Resolution Gas Chromatography (HRGC), gas chromatography/mass spectrometry (GC/MS)), organic substances used as lubricants in the manufacturing of the containers were detected on the aluminium layer in contact with the food. These contaminants were not mineral hydrocarbon fractions used for the shaping of can lids and bodies, but had an organic structure identifiable as esters derived by synthesis between fatty acids C8 and C10 with glycerine, and between C16 and C18 with butyl alcohol. Mixtures of higher esters were also identified as contaminants. Twelve samples were analysed, and the total amount of contaminant substances was found to range from 900 to 1200 µg dm^-2. It is recommended, for safety and compliance with European Community (EC) Regulation No. 1935/2004 (27 October 2004), that the use of aluminium foil containers be subject to appropriate regulation concerning substances adopted for technological purposes.     

核壳型马来酸酐改性苯丙乳液纸张湿强剂

采用半连续种子乳液聚合技术结合预乳化工艺,以苯乙烯、丙烯酸乙酯、甲基丙烯酸甲酯为聚合单体,马来酸酐为功能单体进行改性,采用阴/非离子型复配乳化剂(十二烷基硫酸钠SDS/壬基酚聚氧乙烯醚Tx-100)、复配型引发剂(过硫酸钾/亚硫酸氢钠)合成了具有核壳型结构的纸张湿强剂。采用TEM表征证明成功合成了核壳型的苯丙乳液;SDS与Tx-100之比为2:1时反应得到的乳液稳定性好,不产生凝聚物;从纸张成本及纸张物理强度综合考虑,建议选择浓度为3%的浸渍液。     

同位素内标UPLC -MS/MS法测定婴儿配方奶粉中性激素苯甲酸雌二醇残留

建立测定婴儿配方奶粉中性激素苯甲酸雌二醇的超高效液相色谱-串联质谱方法。样品前处理采用酶解、甲醇提取,经LC-C18和LC-NH2基固相萃取柱净化。苯甲酸雌二醇由超高效液相色谱-串联质谱(UPLC-MS/MS)分离、在正离子电离模式(ESI+)及多反应监测模式(MRM)下,以氘代诺龙-d3为内标进行定量检测。方法对婴儿配方奶粉中苯甲酸雌二醇的检出限(LOD)0.39μg/kg,定量限(LOQ)为0.95μg/kg。在4μg/kg和10μg/kg两个加标水平下,婴儿配方奶粉中苯甲酸雌二醇的回收率在76.5%～86.3%的范围内,相对标准偏差在9.7%～15.2%范围内。     

Volatile aroma constituents of kiwifruit

The volatile constituents of kiwifruit (Actinidia chinensis Planch.) have been investigated. The volatiles were collected and concentrated using vacuum steam distillation and freeze concentration. The concentrated distillate was analysed by gas chromatography, gas chromatography-mass spectrometry and reaction gas chromatography. Apart from methyl benzoate, all the components identified were alkyl and alkenyl esters, alcohols, aldehydes and ketones. The most abundant component was trans hex-2-enal. Odour evaluation of the components at the exit port of the gas chromato-graph indicated that ethyl butanoate, hexanal and trans hex-2-enal are important contributors to the aroma of kiwifruit. One other component which does not show a peak in the chromatogram and which is not yet completely characterised may have particular significance.     

乳清酒发酵过程中细菌群落演替与风味物质变化的相关性分析

采用气相色谱-质谱联用分析乳清酒中重要香气成分的变化规律，运用高通量测序技术分析乳清酒的细菌群落变化，并进行相关性分析。结果表明：乳清酒发酵过程中风味物质的数量整体增加，共检测出102种挥发性风味物质，其中酯类含量最高。通过计算香气活力值可以得出苯甲酸乙酯、乙酸苯乙酯、丁酸乙酯等15种香气物质构成了乳清酒的重要香气成分。发酵前期乳杆菌属（Lactobacillus）为绝对优势菌属，随着发酵的进行，Lactobacillus和乳球菌属（Lactococcus）成为绝对优势菌属。细菌功能预测表明，乳清酒代谢活动主要以氨基酸代谢和碳水化合物代谢为主。进一步展开关联分析，发现大多数的风味物质与Lactococcus和拉乌尔菌属（Raoultella）呈正相关，其中Lactococcus和Raoultella与乙酸苯乙酯、癸酸乙酯、己酸乙酯、乙酸乙酯呈显著正相关。Lactobacillus与柠檬醛、辛酸、癸酸、4-乙基苯酚、庚酸乙酯、癸酸甲酯、油酸乙酯等呈正相关。本研究可为乳清酒发酵剂的筛选及风味调控提供理论依据。