Glycolipid class profiling by packed-column subcritical fluid chromatography

The potential of packed-column subcritical fluid chromatography (SubFC) for the separation of lipid classes has been assessed in this study. Three polar stationary phases were checked: silica, diol, and poly(vinyl alcohol). Carbon dioxide (CO2) with methanol as modifier was used as mobile phase and detection performed by evaporative light scattering detection. The influence of methanol content, temperature, and pressure on the chromatographic behavior of sphingolipids and glycolipids were investigated. A complete separation of lipid classes from a crude wheat lipid extract was achieved using a modifier gradient from 10 to 40% methanol in carbon dioxide. Solute selectivity was improved using coupled silica and diol columns in series. Because the variation of eluotropic strength depending on the fluid density changes, a normalized separation factor product (NSP) was used to select the nature, the number and the order of the columns to reach the optimum glycolipid separation.     

亚临界1,1,1,2-四氟乙烷萃取-气相色谱-质谱法测定鱼肉中6种性激素残留

利用亚临界1,1,1,2-四氟乙烷(R134a)萃取技术,建立了鱼肉中6种性激素残留的气相色谱-质谱(GC-MS)分析方法。样品中的药物经过亚临界R134a萃取后,先进行冷冻过滤去脂,然后通过C18和NH2固相萃取小柱净化,最后经七氟丁酸酐衍生后,采用GC-MS进行定性与定量分析。本实验确定了亚临界R134a萃取6种性激素的最佳条件为:萃取压力4 MPa,萃取温度30℃,夹带剂用量6 mL。在此条件下,6种性激素在5~1000μg/L浓度范围内线性关系良好,相关系数均大于0.99;检出限为0.2~1μg/kg(S/N=3)。在3种浓度添加水平(1,5和10μg/kg)下,6种激素的平均回收率为70.5%~103.6%,相对标准偏差(RSD)为2.1%~12.5%。采用本方法进行实际样品检测时,在一份罗非鱼样品中检出己烯雌酚残留,残留量为14.6μg/kg。     

Determination of oxytetracycline, tetracycline and chloramphenicol antibiotics in animal feeds using subcritical water extraction and high performance liquid chromatography

A rapid analytical method for the determination of oxytetracycline (OTC), tetracycline (TC) and chloramphenicol (CAP) antibiotics in animal feeds has been developed based on subcritical water extraction (SWE) without further sample clean-up followed by high performance liquid chromatography (HPLC) with ultraviolet (UV) detection. On extracting target antibiotics from spiked samples, the efficiency of the water extraction device was evaluated in terms of pH and volume of the extractant, temperature and time of the static extraction. The best extraction conditions were obtained by using 5.5 mL of water adjusted to pH 2 with hydrochloric acid as the extractant at 100 °C with 5-min static extraction. After filtration, 20 μL of the aqueous extract was directly injected into the HPLC column. Recoveries between 82.1% and 90.0% with relative standard deviations ranging between 1.6% and 4.8% were achieved from spiked animal feed samples by using this method. Compared with the traditional ultrasonic extraction, this procedure was remarkably more efficient in extracting OTC, TC and CAP, simpler to perform, and there was no use of toxic organic solvents.     

Degradation of benzoic acid and its derivatives in subcritical water

In this research, the stability of benzoic acid and three of its derivatives (anthranilic acid, salicylic acid, and syringic acid) under subcritical water conditions was investigated. The stability studies were carried out at temperatures ranging from 50 to 350 °C with heating times of 10–630 min. The degradation of the benzoic acid derivatives increased with rising temperature and the acids became less stable with longer heating time. The three benzoic acid derivatives showed very mild degradation at 150 °C. Severe degradation of benzoic acid derivatives was observed at 200 °C while their complete degradation occurred at 250 °C. However, benzoic acid remained stable at temperatures up to 300 °C. The degradation products of benzoic acid and the three derivatives were identified and quantified by HPLC and confirmed by GC/MS. Anthranilic acid, salicylic acid, syringic acid, and benzoic acid in high-temperature water underwent decarboxylation to form aniline, phenol, syringol, and benzene, respectively.     

Chlorination of various substrates in subcritical carbon tetrachloride

Various aliphatic hydrocarbons and the side chains of aromatic hydrocarbons were chlorinated in subcritical carbon tetrachloride. Chlorination of aromatic compounds including 1,4-disubstituted benzenes was investigated. Ketones and sulfones were stable under the employed conditions. Sulfoxides were converted into sulfides in a low to modest yields. The coupling adducts between olefins and carbon tetrachloride were obtained from the reactions of olefins.     

Experiment of subcritical water (Fenton) oxidation treatment of methyl vanillin wastewater

In this paper the oxidative degradation process of methyl vanillin wastewater was studied by the subcritical water oxidation (HCWO) technology. A subcritical Fenton oxidation (HCFO) system formed while Fe²⁺ was added as a catalyst. The oxidation degradation kinetics of methyl vanillin wastewater was also studied. The results showed that the suitable process conditions for degradation of methyl vanillin wastewater by HCWO were as follows: temperature of 340 ​°C, pressure of 24 ​MPa, oxidant multiple of 1.5, residence time of 217.3 ​s (flow rate of 2.0 ​mL ​min^-1). For methyl vanillin wastewater, the HCFO system has no obvious advantages compared to the HCWO system. The activation energy (Ea) of HCWO oxidized methyl vanillin wastewater reaction was 32.6 ​kJ ​mol^-1, and the pre-exponential factor A was 5.64 s^-1.     

Fractional Schrödinger equation; solvability and connection with classical Schrödinger equation

We consider the Dirichlet boundary problem for semilinear fractional Schrödinger equation with subcritical nonlinear term. Local and global in time solvability and regularity properties of solutions are discussed. But our main task is to describe the connections of the fractional equation with the classical nonlinear Schrödinger equation, including convergence of the linear semigroups and continuity of the nonlinear semigroups when the fractional exponent α approaches 1.     

Tensile strength of ostrich carotid artery decellularized with liquefied dimethyl ether and DNase: An effort in addressing religious and cultural concerns

In a previous report, we proposed a method for decellularizing ostrich carotid arteries by removing lipids from the arteries using liquefied dimethyl ether (DME) instead of the conventional sodium dodecyl sulfate (SDS). This is followed by DNA fragmentation with DNase. In the present study, the physical properties of ostrich carotid arteries decellularized using the DME method were evaluated via tensile tests. Results showed that the tissue with SDS broke under less than half the stress of the original ostrich carotid artery. In contrast, the tissue treated with liquefied DME withstood the same level of the original tissue. Both decellularized tissues by liquefied DME showed flexibility comparable to that of the original tissue. We attributed this to the no CN bonds temporarily generated by dehydration through the Schiff-base reaction when lipids were removed by liquefied DME.