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101.
建立了同时测定水产品中15种邻苯二甲酸酯类塑化剂残留的气相色谱-质谱(GC-MS)分析方法。样品经二氯甲烷-正己烷(1∶1)混合溶液超声萃取,中性氧化铝玻璃层析柱净化,用正己烷、二氯甲烷-正己烷(1∶9)混合液、乙酸乙酯-正己烷(1∶4)混合液和乙酸乙酯依次洗脱目标物,洗脱液经浓缩后正己烷定容,气相色谱-质谱测定。结果显示,15种邻苯二甲酸酯的线性范围为0.05~1.0 mg/L,相关系数(r)不小于0.999 1,检出限(LOD,S/N=3)为0.04~1.18μg/kg,定量下限(LOQ,S/N=10)为0.20~4.00μg/kg,不同水产品样品中添加2、50、200μg/kg的15种PAEs,平均加标回收率为81%~123%,相对标准偏差(RSDs,n=3)均小于15%。该方法稳定、可靠、操作简便,适用于鱼肉等水产品中多种PAEs的同时检测与确证。 相似文献
102.
103.
以甲基-2,3,4,6-四-O-苄基-α-D-吡喃型半乳糖为起始原料,通过对1-位和2-位进行结构修饰,6-位选择性脱除苄基后,再引入保护基Ms(或Ts)制得3,4-二-O-苄基-6-磺酰基(或对甲苯基磺酰基)-α-D-吡喃型半乳糖衍生物(2a~2f);在AcOK/DMSO体系中于80℃反应24 h,2发生分子内亲核取代反应合成了一系列新型的4,6-脱水-α-D-吡喃型半乳糖衍生物,产率78%~88%,其结构经1H NMR,13C NMR和ESI-HR-MS表征。 相似文献
104.
应用ICP-MS测定市售红葡萄酒中重金属元素的含量 总被引:1,自引:0,他引:1
目的随着对葡萄酒功效的认识,它逐渐成为普通人喜欢的饮品,所以对葡萄酒中各种成分的研究也成了热点。方法借助先进的ICP-MS技术对4种葡萄酒中的各种重金属和微量元素进行测定。结果金属元素质量浓度由高到低顺序为:As,Cr,Pb,Cd,As最高不超过0.5μg.mL-1,结论符合国家食品卫生标准。 相似文献
105.
目的对样品前处理、酸度及茶叶中共存元素干扰的影响等因素进行探讨,方法用微波消解前处理样品,ICP-AES法同时测定茶叶中铅(Pb)、砷(As)、镉(Cd)、镍(Ni)等元素含量。结果该法的回收率在84.5%~115%之间,精密度RSD均小于9%,结论该法能满足茶叶测定要求。 相似文献
106.
Der‐Lii M. Tzou Lin‐Kai Ni Mei‐Man Chen Min‐Chuan Chiou Li‐Chou Chen Shan‐Te Hsu Kuo‐Lung Ku Chien‐Chung Cheng 《中国化学会会志》2013,60(9):1107-1112
Solid‐state Nuclear Magnetic Resonance (ss‐NMR) 13C single‐pulse excitation spectroscopy in combination with the magic‐angle spinning (MAS) technique was applied to a series of Phalaenopsis tissues, including the leaf, sheath, stem, and root, at different growth and spiking periods. Compared with{1H}/13C cross‐polarization MAS spectra, the 13C single‐pulse excitation MAS spectra displayed very distinct spectral patterns, recognizable as fingerprints of the tissues studied. 1Here, we demonstrate that solid‐state 13C single‐pulse excitation NMR spectroscopy provides a direct and robust analytical tool for studying the various tissues of Phalaenopsis in different growth and spiking induction periods. 相似文献
107.
Bao-Min Wang Zhang Yuan Zhi-Qiang Guo Hai-Nan Ma Chuan Fook Lai 《Russian Journal of Physical Chemistry A, Focus on Chemistry》2013,87(13):2253-2259
As a new nano-scale functional material, it is necessary to achieve a uniform distribution in the composites for gaining the CNFs’ excellent reinforcing effect. In this paper, CNFs were purified by the method of high temperature annealing treatment. Six surfactants, methylcellulose (MC), hydroxypropyl methylcellulose (HPMC), sodium dodecyl sulfate (SDS), dodecylamine (DDA), N, N-dimethyl formamide (DMF) and cetyltrimethyl ammonium bromide (CTAB) were used individually and combinatorially in a certain concentration to disperse the CNFs in aqueous solution. To achieve a good dispersion of the CNFs, a method utilizing ultrasonic processing was employed. The CNFs treated by the method of high temperature annealing treatment were characterized by differential thermal analysis (DTA) and thermogravimetry analysis (TGA), and the ultrasonication-driven dispersion of CNFs in aqueous solutions were monitored by UVvis spectroscopy and transmission electron microscopy (TEM). The experiments reveal that the method of high temperature annealing treatment purified the CNFs and the maximum achievable dispersion of CNFs corresponds to the maximum UV absorbance of the solution. All results show that the surfactants mixture of MC and SDS in a certain concentration of 0.4 and 2.0 g/L has the maximum dispersion effect on CNFs in aqueous solution, the optimum concentration ratio of MC, SDS, and CNFs was 2: 10: 1. 相似文献
108.
A series of aryl hydroxylactams (2a, 2b, 2d–2g, 2i–2k, 2m, and 2n) was synthesized by partially reducing aryl cyclic imides in moderate to excellent yields with activated zinc dust alone in acetic acid. This method was regiospecific and can be employed as an alternative for reported methods to partially reduce aryl cyclic imides. 相似文献
109.
Two dinuclear succinato‐bridged nickel(II) complexes [Ni(RR‐L)]2(μ‐SA)(ClO4)2 ( 1 ) and [Ni(SS‐L)]2(μ‐SA)(ClO4)2 ( 2 ) (L = 5, 5, 7, 12, 12, 14‐hexamethyl‐1, 4, 8, 11‐tetraazacyclotetradecane, SA = succinic acid) were synthesized and characterized by EA, Circular dichroism (CD), as well as IR and UV/Vis spectroscopy. Single crystal X‐ray diffraction analyses revealed that the NiII atoms display a distorted octahedral coordination arrangement, and the succinato ligand bridges two central NiII atoms in a bis bidentate fashion to form dimers in 1 and 2 . The monomers of {[Ni(RR‐L)]2(μ‐SA)}2+ and {[Ni(SS‐L)]2(μ‐SA)}2+ are connected by O–H ··· O and N–H ··· O hydrogen bonds into a 1D right‐handed and left‐handed helical chain along the b axis, respectively. The homochiral natures of 1 and 2 are confirmed by the results of CD spectroscopy. 相似文献
110.
A series of heterometallic LnIII–SbIII edta‐containing compounds with the formulas [Sb2(edta)2Ln]NO3 · nH2O [edta = ethylenediaminetetraacetate; Ln = Eu, n = 7 ( 1 ); Gd, n = 7.5 ( 2 ) and Tb, n = 8 ( 3 )] were synthesized and characterized by elemental analyses (EA), powder X‐ray diffraction (PXDP), Fourier transform infrared spectroscopy (FT‐IR), and thermogravimetric analyses (TGA). Their fluorescence and magnetic properties were also studied. The thermal analysis demonstrates the compounds formation of the antimony, lanthanide ions, and edta4– ligands. FT‐IR spectra reveal that the antimony and lanthanide ions are connected through the carboxylate bridges. The studies of luminescence properties show that compounds 1 and 3 exhibit typical luminescence in the visible region. Furthermore, magnetic properties reveal compounds 2 and 3 have weak ferromagnetic behavior. 相似文献