Study of cloud point extraction and high-performance liquid chromatographic determination of isoniazid based on the formation of isonicotinylhydrazone.

Isoniazid (INH) reacted with p-dimethylaminobenzaldehyde (DABD) in the presence of trichloroacetic acid to give isonicotinylhydrazone (INZ) having lambda(max) 365nm. Cloud point extraction (CPE) is carried out to extract INH and IHZ in aqueous solutions using surfactant poly(ethylene glycol) 4000 (PEG4000), respectively. Langmuir model is used to study the adsorption behaviors of the two solutes on micelles of PEG4000. A linear correlation is found between variation of PEG4000 concentration required for feed concentration of the two solutes and used to predict PEG4000 concentration required for extracting INH and IHZ in CPE procedure. The results calculated show that, for a desired recovery level of 90%, only can IHZ be sufficiently extracted by PEG4000. In this experiment, the feed concentration of PEG4000 is defined by above-mentioned correlation, and the effects of other operating parameters, e.g., concentration of salt, pH and centrifugation time on extraction of PEG4000-IHZ system have also been studied in detail. The proposed CPE method coupled with HPLC-UV system is successfully used for the determination of INH in urine sample.

Enhanced degradation of ortho-nitrochlorobenzene by the combined system of zero-valent iron reduction and persulfate oxidation in soils.

ortho-Nitrochlorobenzene (o-NCB) in soil poses significant health risks to human because of its persistence and high toxicity. The removal of o-NCB by both zero-valent iron (ZVI) and chemical oxidation (persulfate) was investigated by batch experiments. The o-NCB removal rate increases significantly from 15.1 to 97.3 % with an increase of iron dosage from 0.1 to 1.0 mmol g(-1). The o-NCB removal rate increases with the decrease of the initial solution pH, and a removal efficiency of 90.3 % is obtained at an initial pH value of 6.8 in this combined system. It is found that temperature and soil moisture could also increase the o-NCB removal rate. The o-NCB degradation rate increases from 83.9 to 96.2 % and from 41.5 to 82.4 % with an increase of temperature (15 to 35 °C) and soil moisture (0.25 to 1.50 mL g(-1)), respectively. Compared to the persulfate oxidation system and ZVI system, the persulfate-iron system shows high o-NCB removal capacity. o-NCB removal rates of 41.5 and 62.4 % are obtained in both the persulfate oxidation system and the ZVI system, while the removal rate of o-NCB is 90.3 % in the persulfate-iron system.

[Aluminum dissolution and changes of pH in soil solution during sorption of copper by aggregates of paddy soil].

Size fractions of soil aggregates in Lake Tai region were collected by the low-energy ultrasonic dispersion and the freeze-desiccation methods. The dissolution of aluminum and changes of pH in soil solution during sorption of Cu2+ and changes of the dissolution of aluminum at different pH in the solution of Cu2+ by aggregates were studied by the equilibrium sorption method. The results showed that in the process of Cu2+ sorption by aggregates, the aluminum was dissoluted and the pH decreased. The elution amount of aluminum and the decrease of pH changed with the sorption of Cu2+, both increasing with the increase of Cu2+ sorption. Under the same conditions, the dissolution of aluminum and the decrease of pH were in the order of coarse silt fraction > silt fraction > sand fraction > clay fraction, which was negatively correlated with the amount of iron oxide, aluminum and organic matter. It suggested that iron oxide, aluminum and organic matters had inhibitory and buffering effect on the aluminum dissolution and the decrease of pH during the sorption of Cu2+.

Determination of light-medium-heavy polycyclic aromatic hydrocarbons in vegetable oils by solid-phase extraction and high-performance liquid chromatography with diode array and fluorescence detection.

A new method for determination of 16 polycyclic aromatic hydrocarbons (PAHs)-naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene, benzo[g,h,i]perylene, and indeno[1,2,3-cd]pyrene-in vegetable oils was developed. Solid-phase extraction (SPE) prior to high-performance liquid chromatography with fluorescence detection could be used for all those PAHs except acenaphthylene. Acenaphthylene could be detected using a diode array detector at 228 nm. The parameters and variables that affect the extraction were investigated. Under optimum conditions: the extract reagent was centrifuged at 4 °C and evaporated. After that a SPE procedure was used for further cleanup. The limits of detection and limits of quantification were in the range of 0.01-2.35 and 0.04-7.00 µg kg(-1) in vegetable oil, respectively. The relative standard deviations were under 5%.

Determination of four carbamate pesticides in corn by cloud point extraction and high-performance liquid chromatography in the visible region based on their derivatization reaction.

A highly sensitive method for the determination of arprocarb (AC), carbofuran (CF), isoprocarb (IC), and fenobucarb (FC) is proposed. The method is based on alkaline hydrolysis of the four carbamate pesticides, and the resultant hydrolysis products are reacted with 4-aminoantipyrene (AP) to give four red color products. The colored compounds are enriched and separated by cloud point extraction (CPE) method, and the coacervate phase containing the compounds is determined with a high-performance liquid chromatography (HPLC) system in the visible region. AC, CF, IC, and FC were determined on the basis of a linear correlation between the signals of the colored compounds and the concentrations of the pesticides. The method is applied to determine the four pesticides in corn samples; the limits of detection are 2.0 x 10(-4) mg L(-1) for AC, CF, and IC and 5.0 x 10(-4) mg L(-1) for FC, with recoveries ranging between 84.8 and 93.0%, at spiking levels of 5 x 10(-3), 2 x 10(-2), and 0.2 mg kg(-1), respectively.