The comparison of two clean-up procedures, multifunctional column and immunoaffinity column, for HPLC determination of ochratoxin A in cereals, raisins and green coffee beans

To evaluate a clean-up method of detecting ochratoxin A (OTA) by HPLC, the performances of two different clean-up columns, an immunoaffinity column and a multifuntional column were compared in an inter-laboratory study. As samples, un-contaminated wheat, corn grits, green coffee beans and naturally contaminated raisins were used. The recovery test was performed at two different concentrations of OTA (0.5 and 5.0 μg/kg) except for naturally contaminated raisins. Using the immunoaffinity column, the recovery rates, and relative standard deviations for repeatability (R.S.D._r) and reproducibility (R.S.D._R) for wheat, corn grits and green coffee beans ranged 59.0-85.8, 4.2-7.8 and 22.9-29.2%, respectively. For naturally contaminated raisins, recovery, R.S.D._r and R.S.D._R were 84.1, 1.8 and 5.1%, respectively. Using the multifunctional column, the recovery rates, R.S.D._r and R.S.D._R for wheat, corn grits and green coffee beans ranged 80.8-185.0, 0.7-6.9 and 15.2-33.9%, respectively. For naturally contaminated raisins, the recovery, R.S.D._r and R.S.D._R were 128.7, 1.1 and 3.7%, respectively. The results suggest that a multifunctional column could be used to detect OTA in wheat and corn grits at a concentration as low as 0.5 μg/kg; however, it was difficult to detect OTA in green coffee beans and raisins at such a low level. Although an immunoaffinity column could be used for all the test samples in this study from a low level to a high level, the recovery rates were lower than with a multifunctional column.     

多功能柱净化-高效液相色谱法同时检测小麦中雪腐镰刀菌烯醇和脱氧雪腐镰刀菌烯醇

建立了小麦中雪腐镰刀菌烯醇（NIV）和脱氧雪腐镰刀菌烯醇（DON）的高效液相色谱同时检测方法。样品采用乙腈-水（体积比85：15）混合溶剂进行提取．通过多功能净化柱（MFC）进行一次性净化,以C18柱为分离柱,水-乙腈-甲醇（体积比90：5：5）混合溶剂为流动相进行高效液相色谱分离和检测。在小麦样品中,本方法在0．2～5μg／g添加范围内的凹收率为87％～99％;相对标准偏差为1．5％～8．3％;DON和NIV的检出限分别为0．12和0、16μg／g（5／N=3）。     

Application of sulfur microparticles for solid-phase extraction of polycyclic aromatic hydrocarbons from sea water and wastewater samples

The application of sulfur microparticles as efficient adsorbents for the solid-phase extraction (SPE) and determination of trace amounts of 10 polycyclic aromatic hydrocarbons (PAHs) was investigated in sea water and wastewater samples using high performance liquid chromatography coupled with an ultraviolet detector (HPLC–UV). Parameters influencing the preconcentration of PAHs such as the amount of sulfur, solution flow rate and volume, elution solvent, type and concentration of organic modifier, and salt effect were examined. The results showed that at a flow rate of 10 mL min⁻¹ for the sample solutions (100 mL), the PAHs could be adsorbed on the sulfur microparticles and then eluted by 2.0 mL of acetonitrile. For HPLC–UV analysis of extracted PAHs, the calibration curves were linear in the range of 0.05–80.0 μg L⁻¹; the coefficients of determinations (r²) were between 0.9934 and 0.9995. The relative standard deviations (RSDs) for eight replicates at two concentration levels (0.5 and 4.0 μg L⁻¹) of PAHs were lower than 7.3%, under optimized conditions. The limits of detection (LODs, <!-- no-mfc -->S/N<!-- /no-mfc --> = 3) of the proposed method for the studied PAHs were 0.007–0.048 μg L⁻¹. The recoveries of spiked PAHs (0.5 and 4 μg L⁻¹) in the wastewater and sea water samples ranged from 78% to 108%. The simplicity of experimental procedure, high extraction efficiency, short sample analysis, and using of low cost sorbent demonstrate the potential of this approach for routine trace PAH analysis in water and wastewater samples.     

One‐pot synthesis of organic–inorganic hybrid polyhedral oligomeric silsesquioxane microparticles in a double‐zone temperature controlled microfluidic reactor

Polyhedral oligomeric silsesquioxane (POSS) particles are one of the smallest organosilica nano‐cage structures with high multifunctionality that show both organic and inorganic properties. Until now poly(POSS) structures have been synthesized from beginning with a methacryl‐POSS monomer in free‐radical mechanism with batch‐wise methods that use sacrificial templates or additional multisteps. This study introduces a novel one‐pot synthesis inside a continuous flow, double temperature zone microfluidic reactor where the methodology is based on dispersion polymerization. As a result, spherical monodisperse POSS microparticles were obtained and characterized to determine their morphology, surface chemical structure, and thermal behavior by SEM, FTIR, and TGA, respectively. These results were also compared and reported with the outcomes of batch‐wise synthesis. © 2019 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2019, 57, 1396–1403     

Construction of multifunctional heterocycles bearing aza-quaternary carbons by titanocene-catalyzed umpolung reactions

The combined application of Grignard/Reformatsky addition and the titanocene-catalyzed umpolung α-amino carbon-carbon bond formations provided a flexible and versatile protocol for preparation of multifunctional pyrrolidinones/piperidinones/N-Boc-piperidines bearing aza-quaternary carbons (AQC) from cyclic imides and analogues. Based on these multifunctional single-ring motifs, several advanced AQC-bearing heterocycles, such as AQC-possessing indolizidines and 1-azaspirocycles, have been constructed efficiently.     

Deposition of non-spherical microparticles in the human upper respiratory tract

We investigated the deposition pattern of microparticles with different particle diameters, shape factors, and initial flow conditions in a realistic human upper respiratory tract model. We identified a close relationship between the deposition fraction and the particle shape factor. The deposition fraction of the particles decreased sharply with increasing particle shape factor because of the decreasing drag force. We also found that the deposition varied at different positions in the upper respiratory tract. At low shape factors, the highest fraction of particles deposited at the mouth and pharynx. However, with increasing shape factor, the deposition fraction in the trachea and lungs increased. Moreover, for a given shape factor, larger particles deposited at the mouth and pharynx, which indicates that the deposition fraction of microparticles in the human upper respiratory tract is affected first and foremost by particle inertia as well as by the drag force.