一种超高耐久混凝土——梯度结构混凝土

分析超高耐久混凝土的研究现状,提出了一种高耐久、低成本的超高耐久混凝土--梯度结构混凝土(Gradient Structural Concrete,简称GSC),采用电量法和氯离子扩散系数法来评价梯度结构混凝土的抗氯离子渗透性能,最后进行梯度结构混凝土的寿命预测与成本分析.结果表明,高性能混凝土(High Performance Concrete,简称HPC)、无细观界面过渡区水泥基复合材料(Meso-interfacial transition zone-free cement-based materials,简称 MIF)和梯度结构混凝土MIF-HPC的6 h导电量和氯离子扩散系数的排列顺序均为:HPC>MIF-HPC>MIF,其抗氯离子渗透性能排列顺序为:MIF>MIF-HPC>HPC.梯度结构混凝土的成本会有所增加,但由于其氯离子渗透性能大幅降低,其使用寿命得到大幅延长,使得其年损耗费用大幅下降.     

超高效液相色谱串联质谱法同时快速测定牛奶中不同类型的11种兽药残留

建立了超高效液相色谱串联质谱测定牛奶中四环素类、青霉素类、磺胺类和泰乐菌素等11种兽药残留的检测方法。样品经乙腈超声提取后离心分离,上层清液稀释10倍后过0.2μm滤膜上机测定。在优化条件下,11种兽药在其线性范围内的相关系数均在0.998以上,定量下限(LOQ,S/N=10)为0.3～15μg/kg,在低、中、高3个水平下的加标回收率为81%～117%,相对标准偏差为0.6%～10.2%。方法用于实际牛奶样品中兽药残留量的测定,结果满意。     

Ultra high performance liquid chromatography-quadrupole-time of flight analysis for the identification and the determination of resveratrol and its metabolites in mouse plasma

Resveratrol is a polyphenol that has numerous interesting biological properties, but, per os, it is quickly metabolized. Some of its metabolites are more concentrated than resveratrol, may have greater biological activities, and may act as a kind of store for resveratrol. Thus, to understand the biological impact of resveratrol on a physiological system, it is crucial to simultaneously analyze resveratrol and its metabolites in plasma. This study presents an analytical method based on UHPLC-Q-TOF mass spectrometry for the quantification of resveratrol and of its most common hydrophilic metabolites. The use of ¹³C- and D-labeled standards specific to each molecule led to a linear calibration curve on a larger concentration range than described previously. The use of high resolution mass spectrometry in the full scan mode enabled simultaneous identification and quantification of some hydrophilic metabolites not previously described in mice. In addition, UHPLC separation, allowing run times lower than 10 min, can be used in studies that requiring analysis of many samples.     

Effect of Ultra High Pressure Processing on the Particle Characteristics of Lotus-seed Starch

In this paper, the time dependent effects of various pressure treatments on the characteristics of lotus-seed starch which was modified by ultra-high pressure (UHP) were investigated. The results showed that the polarization cross of lotus-seed starch granules was weakening gradually with increasing the treatment time, which indicated the termination of their ordered crystallite structures. The morphologies of granules were collapsed once the UHP was kept at 500 MPa for 60 minutes. The particle size analysis demonstrated that the granule size and distribution of lotus-seed starches increased as the treatment time was prolonged. X-ray diffraction studies showed that the intensity of the feature diffraction peaks of starch decreased and eventually disappeared with increasing the treatment time, and B-type transformation pattern was observed. The Fourier transform infrared spectra (FTIR) analysis of starch showed that the UHP is a physical modification processing because no new groups formed. The research showed that UHP processing at certain degree is capable to achieve the modification of lotus-seed starch. It is of significance for the deep processing of lotus-seed products.     

A Hemi‐metallocene Chromium Catalyst with Trimethylaluminum‐Free Methylaluminoxane for the Synthesis of Disentangled Ultra‐High Molecular Weight Polyethylene

Recently, it has been shown that by using a single‐site catalytic system having titanium as a metallic center, it is possible to tailor the entanglement density in the amorphous region of a semi‐crystalline ultra‐high molecular weight polyethylene (UHMWPE). This route provides the possibility to make high‐modulus, high‐strength uniaxially and biaxially drawn tapes and films, without using any solvent during processing. In this publication, it is shown that a single‐site catalyst having chromium as metallic center, proposed by Enders and co‐workers, can also be tuned to provide control on the entanglement density during synthesis of the UHMWPE. However, to achieve the goal some modifications during the synthesis are required. The synthesized polymers can be processed in the solid state below the equilibrium melting temperature, resulting in uniaxially drawn tapes having tensile strength and modulus greater than 3.5 N/tex and 200 N/tex, respectively. Rheological studies have been performed to follow the increase in entanglement density in melt state with time.

     

免疫亲和柱净化-超高效液相色谱-三重四极杆质谱法高灵敏测定尿液和血浆中3种鹅膏毒肽

建立了超高效液相色谱-三重四极杆质谱高灵敏测定尿液和血浆中α-鹅膏毒肽、β-鹅膏毒肽和γ-鹅膏毒肽的方法。经过免疫亲和柱净化,尿液样品浓缩20倍、血浆样品浓缩10倍,以Kinetex Biphenyl色谱柱(100 mm×2.1 mm, 1.7 μm)作为分析柱,甲醇-0.005%(v/v)甲酸水溶液作为流动相进行梯度洗脱分离,电喷雾电离、负离子、多反应监测模式下检测,外标法定量。3种鹅膏毒肽的线性范围为0.1~200 ng/mL,相关系数(r)>0.999。尿液和血浆中3种鹅膏毒肽的基质效应和提取回收率分别为92%~108%和90%~103%,变异系数均小于13%。尿液中3种鹅膏毒肽的准确度为-9.4%~8.0%,重复性和中间精度分别为3.0%~14%和3.5%~18%,当取样量为2.00 mL时,方法的检出限均为0.002 ng/mL;血浆中3种鹅膏毒肽的准确度为-13%~8.0%,重复性和中间精度分别为3.9%~9.7%和5.5%~12%,当取样量为1.00 mL时,方法的检出限均为0.004 ng/mL。该法操作简单、灵敏、准确,已在中毒患者摄入野生蘑菇后138 h的尿液中检出0.0067 ng/mL α-鹅膏毒肽和0.0059 ng/mL β-鹅膏毒肽。该法已成功解决中毒患者尿液和血浆中超痕量鹅膏毒肽的检测难题,对于疑似中毒病人的早诊断、早治疗、降低死亡率都具有非常重要意义,也为今后开展此类毒素毒理作用及机体代谢规律的研究提供了可靠的技术支撑。     

Identification and quantification of anthocyanins,flavonoids, and phenolic acids in flowers of Rhododendron arboreum and evaluation of their antioxidant potential

The current study aimed to investigate the anthocyanins, non-anthocyanins (flavonoids and phenolic acids), and free radicals scavenging potential in the flowers of Rhododendron arboreum using ultra high performance liquid chromatography with ion mobility quadrupole time of flight tandem mass spectrometry. A total of 25 constituents including nine anthocyanins, six phenolic acids, and ten flavonoids were identified in the flower extract. The major anthocyanins identified were cyanidin-3-O-β-galactoside ( 1 ), cyanidin-3-O-α-arabinoside ( 4 ), and cyanidin-3-O-rhamnoside ( 8 ), while quercetin glycosides were the main identified flavonoids in R. arboreum flowers. Additionally, ultra high performance liquid chromatography methods were developed and validated for the quantification of nine compounds (anthocyanins, flavonoid glycosides, and phenolic acids); five of them were quantified using internal standards. The extracts were analyzed for total phenolics (123.6 mg GAE/g), anthocyanin content (1.76% w/w), and evaluated for antioxidant properties against 2,2-diphenyl-1-picrylhydrazyl radical (IC₅₀: 102.06 and 96.92 μg/mL) and 2,2′-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) radical cation (112.25 and 45.59 μM TE/g) assays. The profiling of R. arboreum for anthocyanins is reported for the first time. The findings suggest that the flowers are a promising source of bioactive constituents and could be used as functional food, antioxidants, and nutraceuticals.     

Determination of carbapenems in water samples by UHPLC–MS/MS

A rapid and reliable method for the detection of five carbapenems (biapenem, imipenem, doripenem, meropenem, and faropenem) in water was developed and validated. After acidification of water samples with acetic acid, carbapenems were isolated using a Bond Elut PPL cartridge. The target compounds were separated using ultra high performance liquid chromatography with a chromatographic run time of 5 min and detected on a triple quadrupole mass spectrometer operated in positive electrospray ionization and multiple reaction monitoring mode. Mean recoveries were in the range of 76.6–106.5%, with satisfactory intraday and interday relative standard deviations lower than 10.0 and 10.8%, respectively. The limits of detection and quantification were in the ranges of 0.05–0.2 µg/L and 0.1–0.5 µg/L, respectively, depending on the analyte. The proposed method was applied to the analysis of river samples and wastewater samples from swine farms, and no carbapenems were detected in the collected samples.     

一种新型温度自补偿高灵敏度折射率计

基于高频CO2激光脉冲写入的新型超长周期光纤光栅(ULPFG),提出了一种可实现温度自补偿的新型高灵敏度折射率计。理论与实验表明,新型超长周期光纤光栅不同闪耀阶次谐振峰对外界折射率与温度变化的灵敏度各自不同,特别的是,该光栅存在对外界折变不敏感的谐振峰,测量中除了可以利用该峰实现温度同时测量外,还可以补偿另一个测量折变的谐振峰因温度变化带来的测量误差。该折射率计具有制作简单、成本低、强度好,灵敏度高等优点,当外界折射率在1.43~1.45范围内变化时,其折射率测量灵敏度可达每单位折射率240 nm,在实际工业应用中具有较大的潜在实用价值。     

超高效液相色谱-串联四极杆质谱联用分析鸭蛋黄中的苏丹红Ⅰ～Ⅳ

建立了鸭蛋黄中苏丹红Ⅰ～Ⅳ号的超高效液相色谱-串联四极杆质谱联用（UPLC-MS/MS）的分析方法。采用乙腈提取样品中的苏丹红,加水反沉淀除去蛋白质和脂肪等杂质,冷冻后高速离心,取上层清液供UPLC-MS/MS分析。经Waters Acquity BHE C18超高效液相色谱柱分离,串联四极杆质谱多反应监测模式检测,4种物质的检出限均为0.05 μg/L,实际样品中4种物质的检出限为10 μg/kg。采用标准添加法测定苏丹红的回收率,100.0,200.0,300.0 μg/kg 3个不同添加水平的回收率为50.2%～101.3%。实验结果表明该方法灵敏度高,检出限低,确证能力强,分析时间短,可满足高通量食品样品中苏丹红的日常检测。