Low temperature cleanup combined with magnetic nanoparticle extraction to determine pyrethroids residue in vegetables oils

To quantify trace pesticide residue in vegetable oil rapidly, low temperature cleanup combined with magnetic nanoparticle based solid phase extraction was developed to determine eight pyrethroids in vegetable oils, including tetramethrin, fenpropathrin, cypermethrin, decamethrin, fenvalerate, acrinathrin, permethrin and bifenthrin. Polystyrene coated magnetic nanoparticles were synthesised by a modified chemical coprecipitation combined with emulsion polymerisation method. The nanoparticles were afterwards characterised by Fourier transform-infrared spectroscopy, X-ray diffraction, transmission electron microscopy as well as vibrating sample magnetometer, and successfully employed as adsorbents for the magnetic solid phase extraction of pyrethroids which were cleaned up using low temperature approach in advance. Critical impact factors on the efficiency of the extraction method such as the mass of adsorbents used, volume and type of eluent solvent, extraction time as well as elution time were optimised subsequently. Regression analysis of the calibration curves of the eight pyrethroids yielded satisfactory correlation coefficients within the range of 0.980–0.998. Limit of detection and limit of quantification were calculated to be between 0.0290-0.0658 and 0.0890–0.1994 ng g⁻¹, respectively. Intra-day and inter-day reproducibility at different concentration levels also produced satisfactory recovery rates of 83.18–112.79% with relative standard deviations not exceeding 10.84% and 12.01%, respectively, suggesting desirable stability of the proposed method.     

牛肉中孕酮的气相色谱/燃烧炉/同位素比质谱检测

建立了牛肉中孕酮的气相色谱/燃烧炉/同位素比质谱(GC/C/IRMS)检测方法。牛肉样品用乙腈振荡和超声辅助提取,经Na Cl脱水,有机相离心和旋转蒸发后以Zn Cl2脱脂,然后用LC-C18、LC-Si、LC-NH2固相萃取柱净化,过滤液经半制备液相色谱(Pre-HPLC)的C18柱纯化,最后分析物以GC/C/IRMS系统分析。牛肉中加标外源性孕酮δ13C值为-30.64±0.24‰(n=6),牛肉内源性孕酮δ13C值为-25.70±0.13‰(n=6),单因素方差分析(ANOVA,p值=2.23×10-140.05)显示,内源性孕酮和外源性孕酮的δ13C值存在显著差异性,且牛肉中加标外源性孕酮δ13C值与孕酮标准溶液的δ13C值无差异性。同时,经模拟实验可知,实际样品中内外源性孕酮混合物的δ13C值与外源性孕酮的δ13C值具有同源性。结果表明,本方法特异性和准确性好,GC/C/IRMS是鉴别激素来源的有效工具,该方法填补了国内鉴别激素来源技术空白。     

Polarized light microscope method for the determination of asbestos fiber of textile

ABSTRACT

Optical spectrogram and optical characteristic parameters of six kinds of asbestos standard products were established by polarizing microscope to analyze the asbestos fiber, and utilized horizon estimation to get the semi-quantitative asbestos content in the samples. The sample had been observed form, refractive index, interference color, dispersion, ductility, color, pleochroism, cleavage, contour lines, bumps, rough, baker characteristics under different refractive index of oiled, to compare with standard optical spectra and characteristic parameters. Comparison between the situation of asbestos fiber particles and the standard map of mineral chips in the field of view, the percentage of asbestos fibers in the sample is estimated. The results showed that this method is accurate, simple and fast.     

Raman investigation of optical phonons in the ion implanted Hg1−xCdxTe

Raman scattering is studied here for Hg_1−xCd_xTe (x = 0.3) samples implanted with 180-keV of B¹¹ ions with various doses up to 1 × 10¹⁵ cm⁻². Considering disorder in the implanted HgCdTe material, the correlation length of Raman active optical phonons is determined as a short range order in the nanocrystals. Phonon softening and asymmetric broadening are investigated for HgTe like LO and TO phonon modes in the Raman spectrum while CdTe like modes almost disappeared for the dose greater than 5 × 10¹³ cm⁻². Disorder is measured quantitatively for wide ranges of doses on the basis of phonon confinement model. Nanostructures of the near-surface implantation-induced damage layer are known to consist of a mixture of amorphous HgCdTe and its nanocrystals. A significant reduction of the nanocrystallites size is reported here with increasing dose i.e. L = 34–46 A⁰ at dose of 1 × 10¹⁵ cm⁻².     

蒜制品中二氧化硫4种检测方法的比较研究

目的研究比较蒜制品中二氧化硫的检测方法。方法通过应用碘量法、比色法、柱后衍生-高效液相色谱法以及离子色谱法检测蒜制品中二氧化硫的结果进行比较分析。结果鲜蒜和脱水蒜制品的比色法检测结果差异较大。采用比色法(盐酸副玫瑰苯胺法)检测鲜蒜和脱水蒜制品中二氧化硫的结果普遍较高,蒜罐头类的检测结果与其他检测方法的值接近。采用滴定法、高效液相色谱法和离子色谱法的检测结果都较为接近。结论 4种方法都可用于蒜制品中二氧化硫的检测,但比色法不适用于鲜大蒜及脱水蒜制品中二氧化硫的检测。     

Carbon fiber/epoxy composite property enhancement through incorporation of carbon nanotubes at the fiber–matrix interphase – Part I: The development of carbon nanotube coated carbon fibers and the evaluation of their adhesion

A new method to realize the uniform coating of carbon nanotubes (CNTs) to carbon fibers (CFs) has been developed, which enables the scalable fabrication of CNT containing CF/epoxy composites. In this method, CNTs are treated by cationic polymers, then, the CNTs are coated to CFs by immersion into a CNT/water suspension. Good dispersion is achieved by repulsive force between positively charged CNTs and uniform coating of the CNTs is achieved by attractive forces between positively charged CNTs and negatively charged CFs. It is found that the use of specific cationic polymers including polyethyleneimine (PEI) results in stable CNT/water suspensions, and uniform coating of the CNTs. Single fiber fragmentation tests of the CF/epoxy composites were conducted to evaluate the strength of interface and interphase under shear loading. The results show that the combination of epoxy resin sizing and PEI treated CNT coating to CFs results in high interfacial shear strength.     

微生物挥发性有机化合物及其在线数据库

微生物挥发性有机化合物是微生物代谢产物的重要组成部分,是了解微生物生命活动本质规律的重要窗口,也是提高微生物利用价值的重要物质基础。虽然通过测序方法可以检测病原微生物,但是检测其标志性或指纹挥发物将会更快、更容易。微生物挥发性有机化合物目前被用来作为标记物检测人类疾病、食物腐败和霉菌。细菌和真菌的挥发物信息目前分散在国内外文献中,没有公共的、可更新的数据库可以查询,为满足需要,科学家研制了一套微生物挥发性代谢产物在线数据库,为微生物代谢产物的研究提供参考。本文还举例介绍了微生物挥发性代谢产物检测技术在医学、食品和植物病害防治方面等方面的应用。     

进口鸡翼中单核细胞增生李斯特菌的鉴定及其 挥发性产物分析

目的对从进口鸡翼中分离的菌株F7-10进行种属鉴定,并通过顶空气相色谱-质谱联用法(headspace gas chromatography-mass spectrometry,HS-GC-MS)分析其液态培养代谢的挥发性产物。方法通过VITEK 2 Compact全自动微生物鉴定系统分析菌株的生理生化特征,结合16S r RNA基因和prf A基因PCR扩增测序鉴定分离菌株,通过HS-GC-MS分析分离菌株F7-10代谢的挥发性产物,并与单核细胞增生李斯特菌ATCC 13932、格氏李斯特菌ATCC 700545和英诺克李斯特菌ATCC 33090的代谢挥发性产物进行比较分析。结果菌株F7-10为革兰氏阳性菌,生理生化特征与单核细胞增生李斯特菌(Listeria monocytogenes)的相似性为98%,协同溶血实验在靠近金黄色葡萄球菌的接种端溶血增强;16S r RNA基因序列与单增李斯特菌标准菌株的相似性为99%,prf A基因特异性扩增出现预期大小的目的片段。菌株F7-10在营养肉汤中代谢的挥发性产物主要有乙醇、3-羟基-2-丁酮、乙酸、丁酸、3-甲基戊酸、十二醇等,与单增李斯特菌标准菌株的代谢挥发性产物种类相似,但含量有差别。结论进口鸡翼中分离的菌株F7-10鉴定为单核细胞增生李斯特菌,该菌产生的挥发性产物可为单核细胞增生李斯特菌的鉴定提供参考。     

Optimum dispersion conditions and interfacial modification of carbon fiber and CNT–phenolic composites by atmospheric pressure plasma treatment

Electric resistance measurements were used to determine the optimal dispersion conditions for carbon nanotubes (CNTs) in phenolic resins. Plasma treatment is frequently used to modify carbon fiber surfaces to improve adhesion of the fibers to matrices. Such treatment might also influence carbon fiber tensile strength. In order to determine the effect of atmospheric pressure plasma treatment on carbon fiber tensile strength and interfacial bonding strength, change in tensile strength of the fiber was studied at different gage lengths before and after the plasma treatment. The wettability of carbon fibers was improved significantly after only 10 s of plasma treatment. Such plasma treatment resulted in a decrease in the advancing contact angle from 65° to 28°. Surface energies of carbon fiber and CNT–phenolic composites were measured using the Wilhelmy plate technique, indicating that the work of adhesion between plasma treated carbon fibers and CNT–phenolic composites was higher than it before plasma modification. The interfacial shear strength (IFSS) and apparent modulus were also increased by plasma treatment of the carbon fibers.     

凝胶渗透色谱净化-气相色谱-质谱法测定黄油中6种激素的残留

建立了凝胶渗透色谱(GPC)-气相色谱-质谱(GC/MS)同时测定黄油中雄酮(A)、脱氢表雄酮(DHEA)、睾酮(T)、孕酮(P)、雌酮(E1)、17β-雌二醇(β-E)6种类固醇激素残留的方法。黄油样品用乙酸乙酯/环己烷(1:1,V/V)振荡辅助提取,提取液经GPC柱净化除脂,GPC浓缩液用氮气吹至尽干,然后用乙酸酐和吡啶衍生化,最后,衍生化物经GC色谱柱(HP-5MS,30 m×0.25mm,0.25μm)分离,在SIM模式下进行定性和定量分析。6种类固醇激素以外标法定量,在10~500μg/kg线性范围内相关系数(r)均大于0.999;方法的定量限LOQs(S/N≥10)为4~10μg/kg;添加水平为10μg/kg、50μg/kg、200μg/kg时,加标回收率范围为77.2~112%,相对标准偏差为4.2~10%。结果表明,所建方法准确、可靠,已成功用于黄油中6种类固醇激素的检测分析。