离子色谱法测定护发和皂类产品中羟乙磷酸及其盐类

研究并建立了护发和皂类产品中羟乙磷酸及其盐类的离子色谱测定方法。将护发和皂类样品分散于3mmol/L盐酸中,于振荡器上振摇至完全溶解,护发和皂类样品提取液分别调节pH值至2.5和5.5,依次过尼龙滤膜和OnGuardⅡRP固相萃取柱。滤液采用离子色谱-抑制电导检测法分析测定,以IonPac AS11-HC阴离子交换色谱柱分离,40mmol/L氢氧化钾溶液为淋洗液等度洗脱,ASRS-400阴离子型抑制电导检测,外标法定量。方法的线性范围为0.5～8.0mg/L,相关系数为0.9999,对羟乙磷酸的定量限为0.025%,护发产品在低、中、高3种加标水平的回收率为84.0%～93.5%,相对标准偏差为1.3%～3.0%;皂类产品在低、中、高3种加标水平的回收率为81.4%～92.3%,相对标准偏差为1.8%～5.1%。该法准确、简便、快速,可用于护发和皂类产品的实际检测。     

Adsorptive removal of nitrogen-containing compounds from fuel by metal-organic frameworks

The adsorptive denitrogenation from fuels over three metal-organic frameworks(MIL-96(Al),MIL-53(Al)and MIL-101(Cr))was studied by batch adsorption experiments.Four nitrogen-containing compounds(NCCs)pyridine,pyrrole,quinoline and indole were used as model NCCs in fuels to study the adsorption mechanism.The physicochemical properties of the adsorbents were characterized by XRD,N2physical adsorption,FT-IR spectrum and Hammett indicator method.The metal-organic frameworks(MOFs),especially the MIL-101(Cr)containing Lewis acid sites as well as high specific surface area,can adsorb large quantities of NCCs from fuels.In addition,the adsorptive capacity over MIL-101(Cr)will be different for NCCs with different basicity.The stronger basicity of the NCC is,the more it can be absorbed over MIL-101(Cr).Furthermore,pore size and shape also affect the adsorption capacity for a given adsorbate,which can be proved by the adsorption over MIL-53(Al)and MIL-96(Al).The pseudo-second-order kinetic model and Langmuir equation can be used to describe kinetics and thermodynamics of the adsorption process,respectively.Finally,the regeneration of the used adsorbent has been conducted successfully by just washing it with ethanol.     

Combination of FASP and fully automated 2D‐LC‐MS/MS allows in‐depth proteomic characterization of mouse zymogen granules

Zymogen granule (ZG) constituents play important roles in pancreatic injury and disease. In previous studies, proteomic analyses with rat zymogen granules were separated by two‐dimensional gel electrophoresis or one‐dimensional SDS–PAGE, followed by in‐gel tryptic digestion. In order to overcome the disadvantage of in‐gel digestion and to carry out further in‐depth proteomic analysis of the zymogen granules, in this study, by combining a filter‐aided sample preparation method and fully automated 2D‐LC‐MS/MS technique, 800 ZG proteins were identified with at least two unique peptides for each protein, 75% of which have not been previously reported. The identified proteins revealed broad diversity in protein identity and function. This is the largest dataset of ZG proteome, and also the first dataset of the mouse ZG proteome, which may help elucidate on the molecular architecture of ZGs and their functions. Copyright © 2012 John Wiley & Sons, Ltd.     

Potential Applications of Cucurbit[n]urils and Their Derivatives in the Capture of Hazardous Chemicals

Cucurbit[n]urils (Q[n]s) are a relatively young family of macrocycles, consisting of glycoluril units bridged by methylene groups, and their unique structures have attracted extensive attention from chemists in recent decades. Due to the presence of a rigid hydrophobic inner cavity and two polar outer portals lined with carbonyl groups, Q[n]s not only encapsulate guest species into the cavity, but also coordinate with metal ions/clusters. Considerable achievements have been obtained in the fields of Q[n]s-based host–guest chemistry, coordination chemistry, as well as the combination of host–guest and coordination chemistry. Furthermore, the outer surface of Q[n]s has been demonstrated to be capable of interacting with definite species to generate supramolecular architectures in recent years. With more in-depth research into Q[n]s, their application studies have also emerged as a hot topic. This Minireview focuses on recent advances in the potential applications of solid-state materials based on Q[n]s and their derivatives for the capture and adsorption of hazardous chemicals from a solution or a gas mixture.     

Trends of Atmospheric CCl 3 F,CCl 2 F 2 and CCl 2 FCClF 2 in Shanghai (China)

Atmospheric concentrations of CCl 3 F (CFC-11), CCl 2 F 2 (CFC-12), and CCl 2 FCClF 2 (CFC-113) in troposphere in Shanghai, China (31°1N) have been routinely monitored by using gas chromatography with electron capture detector from November 1997 to December 2000. The observation shows that there is a slowly declining trend of the three compounds. On the other hand, a comparison has been drawn between the concentrations observed and the ones calculated by 2-box model on the basis of the global statistical data of CFCs production and emission. Our observation agrees with the calculations. It shows that production and emission of chlorofluorocarbons (CFCs) in China are still at a low level and gradually decreasing.     

Cyano terminated tolane compounds for polymer dispersed liquid crystal application: relationship between cyano terminated tolane based molecular structures and electro-optical properties

ABSTRACT

The structures of the liquid crystal (LC) molecules have a key role in impacting the electro-optical performance of a polymer dispersed liquid crystal (PDLC) film. In this paper, the relationship between the LC molecular structures and the electro-optical properties of PDLC films is investigated based on an unexplored cyano-terminated tolane compounds (CTTCs) doped E8 LCs/UV polymers system. Due to the high polarity of CTTCs, LCs doped with the cyano-terminated tolane (CTT) molecules exhibit high birefringence and large positive dielectric anisotropy. On the whole, PDLC films doped with the CTT molecules exhibit a lower driving voltage than that doped with the pure E8. More excitingly, PDLC films based on CTT molecules with larger length-to-width ratio and longer conjugated system show higher contrast ratio (CR) and faster response time. Eventually, the mechanism of the effects of CTT-based molecular structures and the relationship between the electro-optical performance of PDLC films and CTT molecules are illustrated. This work paves a new way for optimising the electro-optical properties of PDLC films.     

Homogeneous liquid crystal alignment on poly(vinylidene fluoride-trifluoroethylene) films subjected to ion-beam irradiation

We demonstrate homogeneous and uniform liquid crystal (LC) alignment on poly(vinylidene fluoride-trifluoroethylene) [PVDF-TrFE] films using ion-beam (IB) irradiation and a performance improvement of twisted nematic (TN) cells using IB-irradiated PVDF-TrFE films. Spontaneous ferroelectricity of the PVDF-TrFE films was modified by IB irradiation, which affected the LC alignment properties. The variation in the pre-tilt angles of the LC molecules on the IB-irradiated PVDF films is attributed to surface reformation, including defluorination and oxidation because the pre-tilt angles of LC molecules can be controlled by adjusting the fluorine content. The results of contact angle measurements supported this phenomenon. A 58% reduction in the switching voltage was observed for TN cells, indicating that the IB-irradiated PVDF-TrFE films are a promising candidate for use as an alignment layer.     

Evaluation of calcipotriol transdermal permeation through pig,rat and mouse skin using liquid chromatography–tandem mass spectrometry

A rapid and sensitive liquid chromatography–tandem mass spectrometric method to evaluate the permeation and retention of calcipotriol in excised samples of pig, rat and mouse skin after application of a calcipotriol ointment has been developed and validated. After sample preparation of ointment, skin homogenate and receptor medium by liquid–liquid extraction, chromatography was performed on an Extend‐C₁₈ column using isocratic elution. Detection was by electrospray ionization in the negative ion mode using multiple‐reaction monitoring of the precursor to product ion transitions of calcipotriol at m/z 411.1 → 393.5, and of lovastatin (internal standard) at m/z 403.2 → 101.2. The assay was linear in all matrices with LLOQs of 1, 0.5 and 40 ng/mL for skin homogenate, receptor medium and ointment samples respectively. In terms of the permeation profiles, it was found that calcipotriol permeated through all skins to only a limited extent over 20 h after application but was efficiently retained in all skins at a level at 20 h of between 40% (pig) and 60% (rat and mouse) of the applied dose. This indicates that calcipotriol ointment has the potential to provide sustained therapeutic benefit in the treatment of psoriasis with minimal systemic side effects. Copyright © 2013 John Wiley & Sons, Ltd.     

Metal complex with terpyrindine derivative ligand as highly selective colorimetric sensor for iron(Ⅲ)

A new metal complex[MnL₂]（NO₃）₂·CH₃CN（1） was synthesized by reaction of 4’-4-（l,2,4-triazol-l-yl）phenyl -2,2’:6’,2"-terpyridine（L） with manganese nitrate.The structure of the complex was determined by X-ray crystallography.The results of UV-vis studies showed that the complex exhibits colorimetric sensing ability for Fe³⁺,which can be observed by naked eye.