Simultaneous Determination of 2- and 3-MCPD Esters in Infant Formula Milk Powder and Edible Vegetable Oils by Gas Chromatography-Mass Spectrometry

Esters of 2- and 3-monochloropropane-1,2-diol (MCPD) are significative contaminants of processed edible oils used as foods or food ingredients. The aim of this study was to develop and validate a new method by GC-MS for the simultaneous quantification of 2 and 3-MCPD esters in infant milk powder and edible vegetable oils. The developed protocol included fat fraction in infant milk powder and edible vegetable oils samples was extracted and treated with sodium methylate-methanol to cleave the ester bonds of the 2- and 3-MCPD esters, moreover, standard samples of deuterium isotope-labeled 2- and 3-MCPD palmitic acid double esters and stearic acid double esters were used as the internal standards. Furthermore, this method was validated when it was applied to food products, concrete manifestation in its good accuracy (the recovery of MCPD esters ranged from 86% to 114%), high sensitivity (the LOD of 3-MCPD and 2-MCPD esters were 0.025 and 0.020 mg/kg, LOQ were 0.075, 0.060 mg/kg, respectively) and satisfactory repeatability (RSD below 6.8%) for all analytes. In the 150 commercial edible vegetable oils and infant formula milk powder samples, we obtained a preliminary profile of MCPD ester contamination.

Synergistic extraction of rare earth by mixtures of 2-ethylhexyl phosphoric acid mono-2-ethylhexyl ester and di-(2-ethylhexyl) phosphoric acid from sulfuric acid medium

The extraction of Nd^3＋ and Sm^3＋, including the extraction and stripping capability as well as the separation effect of Nd^3＋ or Sm^3＋, from a sulfuric acid medium, by mixtures of di-（2-ethylhexyl） phosphoric acid （HDEHP, H2A2（0）） and 2-ethylhexyl phosphoric acid mono-2-ethylhexyl ester （HEH/EHP, H2L2（0）） were studied. The distribution ratios and synergistic coefficients of Nd^3＋ and Sm^3＋ in different acidities were also determined. A synergistic extractive effect was found when HDEHP and HEH/EHP were used as mixed extractants for Sm^3＋ or Nd^3＋. The chemical compositions of the extracted complex were determined as Nd.（HA2）2-HL2 and Sm.（HA2）2-HL2. The extraction equilibrium constants, enthalpy change, and entropy change of the extraction reaction were also determined.

Azalomycin F_(4a) 2-ethylpentyl ester,a new macrocyclic lactone,from mangrove actinomycete Streptomyces sp.211726

Azalomycin F4a 2-ethylpentyl ester,a new 36-membered macrocyclic lactone antibiotic,was isolated from mangrove actinomycete Streptomyces sp.211726.Its structure was elucidated on the basis of spectroscopic data.The compound showed broad-spectrum antifungal activity and moderate cytotoxicity against human colon tumor cell HCT-116.

Short communication Catalytic synthesis of butyric esters with TiSiW_(12)O_(40)/TiO_2

The catalytic activities of TiSiW_(12)O_(40)/TiO_2 in synthesizing ethylester; propyl ester, n-butyl ester; and amyl ester were reported. It was demonstrated thatTiSiW_(12)O_(40)/TiO_2 is an excellent catalyst. Various factors concerned with esterification wereinvestigated. The optimum conditions were found: the mole ratio of alcohol to acid is 1.3:1, themass ratio of catalyst to reactants is 1.5 percent, and the reaction time is 1.0 h. Under theoptimum conditions, the yields are 88.0 percent for ethyl ester, 94.5 percent for propyl ester, 98.6percent for n-butyl ester, 99.1 percent for n-amyl ester, and 96.7 percent for iso-amyl ester,respectively.

Caffeic acid phenethyl ester up-regulates antioxidant levels in hepatic stellate cell line T6 via an Nrf2-mediated mitogen activated protein kinases pathway

AIM To investigate the antioxidant effect of caffeic acid phenethyl ester (CAPE) in hepatic stellate cell-T6 (HSC-T6) cells cultured in vitro and the potential mechanisms. METHODS HSC-T6 cells were cultured in vitro and treated with various concentrations of CAPE for 24, 48 and 72 h, respectively. Cell proliferation was investigated using the MTT assay, and cell ultrastructural alterations were observed by transmission electron microscopy. Flow cytometry was employed to investigate the effects of CAPE on apoptosis and the levels of reactive oxygen species in HSC-T6 cells cultured in vitro. An enzyme immunoassay instrument was used to evaluate antioxidant enzyme expression. The effect on alpha-smooth muscle actin was shown using immunofluorescence. Gene and protein levels of Nrf2, related factors, and mitogen activated protein kinases (MAPKs), in HSC-T6 cells were detected using RT-PCR and Western blot, respectively. RESULTS CAPE inhibited the proliferation and activation of HSC-T6 cells cultured in vitro. CAPE increased the antioxidant levels and the translocation of Nrf2 from the cytoplasm to the nucleus in HSC-T6 cells. Moreover, the phosphorylation of MAPKs in cells decreased in response to CAPE. Interestingly, CAPE-induced oxidative stress in the cells was significantly attenuated by pretreatment with MAPKs inhibitors. CONCLUSION CAPE inhibits cell proliferation and up-regulates the antioxidant levels in HSC-T6 cells partly through the Nrf2-MAPKs signaling pathway.

Solvent extraction equilibrium of dysprosium(Ⅲ) from nitric acid solutions with 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester

In view of the importance of solvent extraction of rare earth metals with the acidic organophosphorous reagent,the development of a chemically based model applicable to high concentration is desired.In the present study,the equilibrium distribution of dysprosium(Ⅲ)between an aqueous nitric acid solution and 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester (PC88A)was measured in the range of an initial aqueous dysprosium(Ⅲ)concentration from 1.0×10-3to 1.0×10-1kmol/m 3and PC88A concentration from 0.16 to 0.65 kmol/m3in Shellsol D70 as the diluent.The obtained data were analyzed using the chemically based model in order to correlate the equilibrium distribution ratios.In this model,dysprosium(Ⅲ)was assumed to be extracted with the PC88A dimer as a 1:3 complex,the activities were considered for the aqueous species,and the effective concentration of the PC88A dimer was calculated using Alstad's empirical equation.As a result,the apparent extraction equilibrium constant was determined to be 253(kmol·m- 3)-2with an excellent correlation between the experiment and calculation results in the wide range of the logarithm of the distribution ratio from-2 to 3.5.In conclusion,the methodology in this model would be effective for quantitative description of solvent extraction behavior of general rare earth elements as well as dysprosium.

Potassium iodide catalyzed reductive dehalogenation ofα-halo-ketones using Hantzsch ester diethyl 1,4-dihydro-2,6-dimethylpyridine-3,5-dicarboxylate as reductant

In the presence of diethyl 1,4-dihydro-2,6-dimethylpyridine-3,5-dicarboxylate（DHP） and a catalytic amount of potassium iodide,severalα-halo ketones were easily reduced to the corresponding ketones in acetone media.The procedure presented here showed several merits such as short reaction time,practical experimental and isolated procedure,and excellent yields of products.

Synergistic extraction of praseodymium with 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester and 8-Hydroxyquinoline

The synergistic extraction of Pr^3＋ from hydrochloric medium using mixture of 2-ethylhexyl phosphonic acid mono- 2-ethylhexyl ester （P507, HL） and 8-Hydroxyquinoline （HQ） in heptane was investigated. The effect of equilibrium of aqueous acidity on extraction of Pr^3＋ was discussed. The effect of extractant concentraction, different diluents, equilibrium time and acetate ion concentration oil extraction reaction were also studied. With a method of double-logarithmic slope, composition of the extracted species on 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester and 8-Hydroxyquinoline was derived. The result shows that the synergistic extraction system not only overcomes emulsification of 8-Hydroxyquinoline, but also shows perfect capacity of synergistic extraction. The largest synergistic enhancement factor can be calculated to be 5.49 at pH 3.6 for Pr^3＋.

Synthesis, Crystal Structure and Inhibition of N-2-Thiophenesulfonyl-α-L-phenylalanine Ethyl Ester on K562 Cell Proliferation

The title compound N-2-thiophenesulfonyl-a-L-phenylalanine ethyl ester has been synthesized. Complete assignments were achieved by IR, MS, ^1H NMR and single-crystal X-ray diffraction analyses. Using MTT assay, the inhibitory rate of the title compound on K562 cells （chronic myeloid leukemic cells） was measured and the result of preliminary bioassay showed that the title compound possesses antiproliferation effects on K562 cells. In order to investigate the relationship between structure and activity of the target compound, we report its crystal structure and biological behavior in the present paper. Crystallographic data： C15H17NO4S2, Mr = 339.42, monoclinic, space group P21, flack = -0.15（12）, a = 5.7916（10）, b = 11.5078（19）, c = 12.924（2） A, β = 97.781（3）°, Z = 2, V = 853.4（2） A^3, De = 1.321 g/cm^3, F（000） = 356, -7≤h≤7, -10≤k≤14, -15 ≤ l≤15, R = 0.0628, wR = 0.1540 and μ（MoKa） = 0.327 mm^-1. The molecule comprises a benzene and a thiofuran rings, and the intramolecular N（1）-H（1A）…O（1） makes a five-membered ring of O（1）--C（6）-C（5）--N（1）--H（1A）.

Synthesis and Crystal Structure of 4-(4,6-dimethoxyl -pyrimidin-2-yl)-3-thiourea Carboxylic Acid Methyl Ester

The title compound 4-（4,6-dimethoxylpyrimidin-2-yl）-3-thiourea carboxylic acid methyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at the room temperature. The structure was characterized by elemental analysis and IR and determined by X-ray diffraction analysis＇ Crystallographic data： C9H12N4O4S, Mr = 272.29, monoclinic, space group C2/m with a = 1.6672（3）, b = 0.66383（12）, c = 1.1617（2） nm, β = 109.275（2）°, V = 1.2136（4） nm^3, Dc = 1.490 g/cm^3,μ = 0.281 mm^-1, F（000） = 568, Z = 4, R1 = 0.0341and wR2 = 0.1042.

New Method for Reducing 2，6－Pyridinedicarboxylic Acid Diethyl Ester to 2，6－Di（hydroxymethyl）pyridine

Reducing 2, 6-pyridinedicaboxylic acid diethyl ester to 2,6-di(hydroxymethyl)pyridine was carried out by using NaBH4/CaCl2 as reducing agent. It is an improved and efficient method. The yield is up to 91%.

A Novel Synthesis of Methyl 4, 6-O-Benzylidene-α-D-Glucopyranoside 2, 3-Cyclic Phosphite Ethyl Ester

A new compound. methyl 4. 6-O-benzylidene-a-D-glucopyranoside 2. 3-cyclicphosphite ethyl ester was synthesized via the reaction of methyl 4. 6-O-benzylidene-a-D-glucopyranoside and ethyl dichlorophosphite. Its structure was confirmed by NMR and MSspectral methods.

Synthesis and Crystal Structure of 4-(4,6-Dimethoxylpyrimidin-2-yl)-3-thiourea Carboxylic Acid Ethyl Ester

4-（4,6-Dimethoxyl-pyrimidin-2-yl）-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data： C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309（3）, b = 0.67682（6）, c = 1.74237（19） nm, β = 114.744（3）°, V= 2.7106（5） nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F（000） = 1200, Z= 8, R= 0.0514 and wR= 0.1529.

Synthesis and Characterization of Modified Epoxy Resins by Silicic Acid Tetraethyl Ester and Nano-SiO_2

A kind of modified epoxy resins was obtained by condensation of epoxy resin with silicic acid tetraethyl ester（TEOS） and nano-SiO2. The reactions were performed with hydrochloric acid as a catalyst at 63 ℃. The structure, thermal stability and morphological characteristics of the modified epoxy resins were studied through infrared spectra（FT-IR） analysis, thermogravimetric（TG） analysis and scanning electron microscopy respectively. It has been found from the IR and TG study that modified epoxy resins have greater thermal stability than epoxy resins, and its thermal stability has been improved by the formation of inter-crosslinked network structure. The modified epoxy resins exhibit heterogeneous morphology and heterogeneity increases with more TEOS feeding, which in turn confirms the formation of inter-crosslinked network structure in modified epoxy resins.

K_(2)CO_(3)/KOH协同醇解废弃涤纶纺织品及其制备再生DMT的研究

废弃涤纶纺织品囤积量逐年上升,而对废弃涤纶纺织品的综合利用回收率却较低。化学法回收中乙二醇醇解-甲醇酯交换法是一种回收废弃涤纶纺织品的方法,然而乙二醇醇解-甲醇酯交换工艺过程中存在对苯二甲酸双羟基乙酯(BHET)单体产率低、低聚物含量高的问题。文章采用K_(2)CO_(3)/KOH协同醇解废弃涤纶纺织品,并结合响应面法优化了醇解工艺参数,通过甲醇酯交换法制得再生对苯二甲酸二甲酯(DMT),研究了K_(2)CO_(3)/KOH协同醇解对乙二醇醇解-甲醇酯交换产物的影响。结果表明,随着KOH添加量的增加,醇解产物中BHET含量呈现先增加后下降的趋势。当KOH的添加量达到2%时,BHET含量达到最高70.2%。同时,优化后的醇解工艺参数为:反应温度210℃、反应时间120 min、K_(2)CO_(3)质量分数2.0%、KOH质量分数2.4%。此时BHET的收率为73.1%;醇解产物与甲醇酯交换得到再生DMT产率为80.1%,通过减压升华纯化后得到再生DMT含量高于99%以上。

Synthesis and Crystal Structure of 2-[(4-Methoxy- 6-methylthio-2-pyrimidinyl)aminocarbonyl- aminosulfonyl] Benzoic Acid Methyl Ester

The title compound 2-[(4-methoxy-6-methylthio-2-pyrimidinyl)aminocarbonyl- aminosulfonyl]benzoic acid methyl ester (C15H16N4O6S2, Mr = 412.44) was obtained by the reaction of (4-methoxy-6-methylthio-2-pyrimidinyl)amine with 2-methoxylcarbonylbenzene-sulfonylisocya- nate. The crystal is of monoclinic, space group P21/c with a =11.169(3), b = 9.508(3), c = 17.690(5) ? b = 91.593(5), Z = 4, V = 1877.9(10) 3, Dc = 1.459 g/cm3, F(000) = 856, m(MoKa) = 0.324 mm-1, R = 0.0690 and wR = 0.1368 for 3301 observed reflections (I > 2s(I)). The N(1)H…N(3) and N(2)H…O(4) hydrogen bonds can be observed. In the molecule the phenyl plane(I), pyrimi- din-2-yl-urea bridge plane(Ⅱ) and ester plane(Ⅲ) form three conjugated systems.

雪花状Fe_(2)O_(3)-AgNPs SERS基底在大豆基天然酯绝缘油-糠醛检测中的应用

本文通过一步水热合成了雪花状三氧化二铁(α-Fe_(2)O_(3))纳米材料,并通过化学还原法在其表面原位生长银纳米颗粒(AgNPs),并将其作为表面增强拉曼散射基底用于检测大豆基天然酯油中的糠醛浓度。根据扫面电子显微镜(SEM),透射电子显微镜(TEM),X射线衍射仪(XRD),电化学工作站以及拉曼光谱仪(Raman)分别进行表征。结果表明,以RhB作为探针分子,最低检测限为10-11 mol/L(M),而且相较于单一AgNPs基底,α-Fe_(2)O_(3)-AgNPs的SERS性能更优异。将α-Fe_(2)O_(3)-AgNPs基底进行功能化处理,使其表面修饰4-ATP分子,并用于检测大豆基天然酯绝缘油中的糠醛,最低检测限能达到0.05 mg/L。检测结果完全满足电力行业绝缘油的老化标准(重度老化,4mg/L;中度老化,0.5 mg/L;轻度老化,0.1 mg/L)。

A Highly Luminous LiCaPO₄:Eu²⁺Phosphor Synthesized by a Solution Method Employing a Water-Soluble Phosphate Ester

A LiCaPO4:Eu2+ phosphor with high photoluminescence was synthesized using a polymerizable complex (PC) method employing a water-soluble polyethylene glycol-conjugated phosphate ester (PEG-P). PEG-P could be obtained from a reaction among polyethylene glycol 300, phosphorus pentoxide, and pyrophosphoric acid. The PEG-P prepared was stable in an aqueous condition. A transparent solution and gel were obtained when the PEG-P was used as a source of P during the PC method, whereas the use of H3PO4 caused an undesirable precipitate. The LiCaPO4:Eu2+ obtained via the PC method employing the PEG-P showed higher emission intensity than those synthesized by a solid state reaction method and the PC method employing H3PO4. The high luminescence properties of the sample synthesized using the PEG-P may be attributed to high homogeneity of constituents in the sample.

Catalytic Synthesis of Salicylate Esters over Cordierite Honeycomb Coated with Mo (VI)/ZrO₂

Solid acids such as ZrO2 & Mo (VI)/ZrO2 were coated on a honeycomb monolith by impregnation method. These catalytic materials were characterized by NH3-TPD, PXRD and SEM techniques. Salicylate esters were synthesized via transesterification of methyl salicylate with different alcohols over these catalytic materials. An excellent yield of Salicylate esters was obtained under specific reaction conditions. A correlation between the surface acidity, PXRD phase and catalytic activity of Mo (VI)/ZrO2 was observed. The thermally regenerated catalytic material was reused repeatedly with a consistent high yield of salicylate esters. The honeycomb coated with zirconia catalysts were found to be economical, efficient and ecofriendly (3E concept).

超临界CO_(2)萃取石榴籽油及石榴酸甲酯富集

采用超临界CO_(2)萃取技术从石榴籽中提取石榴籽油,对其脂肪酸和甘三酯组成和含量进行分析;通过单因素和正交优化试验研究尿素包合法富集石榴酸甲酯。超临界CO_(2)萃取技术与有机溶剂萃取相比更有利于获得高石榴酸含量的石榴籽油,石榴籽油中检测出14种甘三酯。尿素包合法富集石榴酸甲酯的最佳工艺为尿素包合温度5℃、包合时间20 h、尿素与脂肪酸甲酯的质量比1∶1、尿素和95%乙醇的质量比1∶5,此最佳包合条件下获得的石榴酸甲酯的含量为78.82%。