Development of monolith-based stir bar sorptive extraction and liquid chromatography tandem mass spectrometry method for sensitive determination of ten sulfonamides in pork and chicken samples

A highly sensitive method was developed for the simultaneous determination of ten sulfonamides in pork and chicken samples by monolith-based stir bar sorptive extraction (SBSE) coupled to high-performance liquid chromatography tandem mass spectrometry. The samples were freeze-dried and extracted by acetonitrile, then enriched and further extracted by SBSE which was based on poly(vinylphthalimide-co-N,N-methylenebisacrylamide) monolith (SBSE-VPMB) as coating. To achieve optimum extraction performance of SBSE for sulfonamides, several parameters, including pH value and ionic strength in the sample matrix and extraction and desorption time, were investigated in detail. Under the optimal conditions, the limits of detection (S/N?=?3) for target sulfonamides were 1.2–6.1 ng/kg in pork and 2.0–14.6 ng/kg in chicken, respectively. Real samples spiked at the concentration of 0.5 and 5.0 μg/kg showed recoveries above 55 % and relative standard deviations below 12 %. At the same time, the extraction performances of target sulfonamides on SBSE-VPMB were compared with other SBSE based on porous monolith and commercial SBSE.

A sensitive and specific ELISA for determining a residue marker of three quinoxaline antibiotics in swine liver

Methyl-3-quinoxaline-2-carboxylic acid (MQCA) is a possible residue marker for three quinoxaline veterinary medicines (olaquindox, mequindox, and quinocetone). The wide application of mequindox/quinocetone or the illegal use of olaquindox leads to MQCA residue in animal’s original food, thereby threatening the safety of human food. The indirect competitive enzyme-linked immunosorbent assay (IC-ELISA) with a specific coating antigen and monoclonal antibody (MAB) was established and optimized for detecting MQCA in swine liver. Samples were acidified with 2 mol?l^?1 hydrochloric acid, extracted with ethyl acetate–hexane–isopropanol (8?+?1?+?1, v/v/v) and then detected by IC-ELISA. The logarithm correlation of standards to OD values ranged from 0.2 to 200 μg?l^?1, with IC₅₀ of 6.46 μg?l^?1. Negligible cross-reactivity happened to five quinoxaline antibiotics (olaquindox, mequindox, quinocetone, carbadox, and cyadox) and the metabolite of carbadox and cyadox (quinoxaline-2-carboxylic acid). When spiked with 1 to 100 μg?kg^?1 of MQCA, the recoveries ranged from 85.44 to 100.02 %, with the intra-assay coefficient of variation (CV) of 6.64–10.57 % and inter-assay CV of 7.29–10.88 %. The limit of detection for MQCA was 1.0 μg?kg^?1 in swine liver. Furthermore, incurred samples were detected by the IC-ELISA and then conformed by a reported LC/MS/MS method, it shown that there was good correlation between the two methods. All these results indicated that the IC-ELISA method is appropriate for surveillance MQCA residue in animal tissues.

Sensitive monitoring of penicillin antibiotics in milk and honey treated by stir bar sorptive extraction based on monolith and LC‐electrospray MS detection

In the present study, a convenient and sensitive method for determination of six penicillin antibiotics (amoxicillin, ampicillin, penicillin G, oxacillin, cloxacillin, and dicloxacillin) in milk and honey samples was developed. Milk and honey samples were diluted with water, then directly treated by stir bar sorptive extraction based on poly (vinylimidazole‐divinylbenzene) monolithic material as coating. The analytes were analyzed by LC/ESI‐ MS/MS. Several extraction parameters including extraction and desorption time, pH value, and ionic strength in sample matrix were investigated in detail. Under the optimized extraction conditions, the calculated detection limits for the target compounds were as low as 0.23–2.66 ng/kg in milk and 0.18–1.42 ng/kg in honey, respectively. Good linearity was obtained for analytes with the correlation coefficients (R²) above 0.997. Excellent method reproducibility was achieved in terms of intraday and interday precisions, indicated by the RSDs of <5.0 and <10.0%, respectively. Finally, the proposed method was successfully applied to the determination of penicillin antibiotics residues in different milk and honey samples.     

Effect of Stress-Dependent Thermal Conductivity on Thermo-Mechanical Coupling Behavior in GaN-Based Nanofilm Under Pulse Heat Source

The thermal properties of a nanostructured semiconductor are affected by multi-physical fields,such as stress and electromagnetic fields,causing changes in temperature and strain distributions.In this work,the influence of stress-dependent thermal conductivity on the heat transfer behavior of a GaN-based nanofilm is investigated.The finite element method is adopted to simulate the temperature distribution in a prestressed nanofilm under heat pulses.Numerical results demonstrate the effect of stress field on the thermal conductivity of GaN-based nanofilm,namely,the prestress and the thermal stress lead to a change in the heat transfer behavior in the nanofilm.Under the same heat source,the peak temperature of the film with stress-dependent thermal conductivity is significantly lower than that of the film with a constant thermal conductivity and the maximum temperature difference can reach 8.2 K.These results could be useful for designing GaN-based semiconductor devices with higher reliability under multi-physical fields.     

Lutidine‐Based Chiral Pincer Manganese Catalysts for Enantioselective Hydrogenation of Ketones

A series of Mn^I complexes containing lutidine‐based chiral pincer ligands with modular and tunable structures has been developed. The complex shows unprecedentedly high activities (up to 9800 TON; TON=turnover number), broad substrate scope (81 examples), good functional‐group tolerance, and excellent enantioselectivities (85–98 % ee) in the hydrogenation of various ketones. These aspects are rare in earth‐abundant metal catalyzed hydrogenations. The utility of the protocol have been demonstrated in the asymmetric synthesis of a variety of key intermediates for chiral drugs. Preliminary mechanistic investigations indicate that an outer‐sphere mode of substrate–catalyst interactions probably dominates the catalysis.     

一种基于丹磺酰胺染料的高选择性汞(Ⅱ)离子荧光探针

对人类健康和社会环境而言,汞离子被认为是毒性最大的金属离子之一.本文设计、合成了一种新型基于丹磺酰胺染料的荧光探针,并研究了其对金属阳离子的识别性质.研究结果表明:该荧光探针在水溶液中,对汞离子具有高度的选择性和良好的灵敏度,且不受其它金属阳离子的干扰.该探针对汞离子的检测限可以达到2.1×10-8 mol/L.该探针极低的检测限和良好的水溶性表明其可用于活细胞中检测汞离子.生物成像实验证实该探针具有良好的细胞膜透性和生物相容性.     

Determination of Six Resorcylic Acid Lactones in Feed by GC–MS

A method was developed to simultaneously detect six resorcylic acid lactones in feed by GC–MS. Samples were extracted with methanol followed by a two step liquid–liquid extraction and an HLB SPE clean-up. The samples were derivatized with BSTFA + TMCS (99/1; v/v) and determined by GC–MS. For all analytes, the ranges of recoveries were 81.2–98.2%, with RSDs of 3.2–15.2%, and the LODs were 0.2–0.6 μg kg⁻¹.

     

Calculating critical relative humidity from solubility according to Pitzer ion interaction model

The solubility and the critical relative humidity (H(cr)) of 14 drugs and inorganic salts were determined, the relationship between the H(cr) and the solubility was explored theoretically, and the H(cr) was calculated in the light of Raoult's law and Pitzer ion interaction model from their solubility. The results indicate that the H(cr) values calculated by Raoult's law in high humidity (H(cr)>80%) and by Pitzer ion interaction model in low humidity (H(cr)<80%) are comparable to the measured ones.     

Achieving high strength and high ductility in nanostructured metals: Experiment and modelling

Engineering nanostructures in metallic materials such as nanograins and nanotwins can promote plastic performance significantly. Nano/ultrafine-grained metals embedded in coarse grains called bimodal metals and nanotwinned polycrystalline metals have been proved to possess extensively improved yield strength whilst keeping good ductility. This paper will present an experimental study on nanostructured stainless steel prepared by surface mechanical attrition treatment (SMAT) with surface impacts of lower strain rate (10 s^?1–10³ s^?1) and higher strain rate (10⁴ s^?1–10⁵ s^?1). Microstructure transition has been observed from the original γ-austenite coarse grains to α′-martensite nanograins with bimodal grain size distribution for lower strain rates to nanotwins in the ultrafine/coarse grained austenite phase for higher strain rates. Meanwhile, we will further address the mechanism-based plastic models to describe the yield strength, strain hardening and ductility in nanostructured metals with bimodal grain size distribution and nanotwinned polycrystalline metals. The proposed theoretical models can comprehensively describe the plastic deformation in these two kinds of nanostructured metals and excellent agreement is achieved between the numerical and experimental results. These models can be utilized to optimize the strength and ductility in nanostructured metals by controlling the size and distribution of nanostructures.     

局部上循环的3-Hom李双代数和3-李经典Hom-杨巴克斯方程

本文介绍了局部上循环的3-Hom李双代数,它的乘法和余乘两种运算的相容条件由局部上循环条件给出.作者研究了扭的3元版本的杨巴克斯方程,称为3-李Hom-杨巴克斯方程,它是文献[1]中3- 李杨巴克斯方程的一种广义化.文章证明由3-李Hom-杨巴克斯方程的解所诱导的双代数,可得到上边缘的局部上循环的3-Hom 李双代数.