A novel pollution index based on the bioavailability of elements: a study on Anzali wetland bed sediments.

In this research, we study on the distribution of several elements in bed sediments of Anzali wetland. Anzali, one of the most important international wetlands, is located on the southern coast of the Caspian Sea in Iran. This wetland receives discharges of domestic, agricultural, and industrial wastewater, which affect the distribution of elements. Our contribution in this study is threefold. First, we measured the total concentration of metals as well as their chemical partitioning and bioavailability in the sediments. Second, we calculated anthropogenic portions of metals in the sediment of this area. The results reveal anthropogenic portion of metals as Mo > Mn > Cd > As > Zn > Hg > Co > Sn > Cu > V > Ag > Ni > Pb > Fe > Cr > Al, respectively. We evaluated the intensity of pollution by using an enrichment factor, the geo-accumulation index and the pollution index. All these indices do not take into consideration the bioavailability of the elements. As our third and most important contribution, we introduced a new formula that takes into account the bioavailability of different elements. In comparison with aforementioned pollution indices, our newly introduced pollution index has a higher Pearson correlation with anthropogenic portion of metals. This high-correlation coefficient shows that our proposed pollution index is an effective indicator for determining the level of pollution, while other indices preserve their own merits.

Extraction and Determination of Cyproheptadine in Human Urine by DLLME-HPLC Method.

Novel dispersive liquid-liquid microextraction (DLLME), coupled with high performance liquid chromatography with photodiode array detection (HPLC-DAD) has been applied for the extraction and determination of cyproheptadine (CPH), an antihistamine, in human urine samples. In this method, 0.6 mL of acetonitrile (disperser solvent) containing 30 µL of carbon tetrachloride (extraction solvent) was rapidly injected by a syringe into 5 mL urine sample. After centrifugation, the sedimented phase containing enriched analyte was dissolved in acetonitrile and an aliquot of this solution injected into the HPLC system for analysis. Development of DLLME procedure includes optimization of some important parameters such as kind and volume of extraction and disperser solvent, pH and salt addition. The proposed method has good linearity in the range of 0.02-4.5 µg mL(-1) and low detection limit (13.1 ng mL(-1)). The repeatability of the method, expressed as relative standard deviation was 4.9% (n = 3). This method has also been applied to the analysis of real urine samples with satisfactory relative recoveries in the range of 91.6-101.0%.

A rapid, simple, liquid chromatographic-electrospray ionization, ion trap mass spectrometry method for the determination of finasteride in human plasma and its application to pharmacokinetic study.

A fast, accurate, sensitive, selective and reliable method using reversed-phase high performance liquid chromatography coupled to electrospray ionization ion trap mass spectrometry was developed and validated for the determination of finasteride in human plasma. After protein precipitation with perchloric acid, satisfactory separation was achieved on a Zorbax Eclipse(®) C8 analytical column using a mobile phase consisted of acetonitrile, 2 mM ammonium formate buffer (58:42, pH adjusted at 2.5 using formic acid); the flow rate was 0.25 mLmin(-1) and the column oven was set to 50°C. Tamoxifen citrate was used as internal standard. This method involved the use of [M +H](+) ions of finasteride and IS at m/z 373 and 372 respectively with the selected ion monitoring (SIM) mode. The calibration curve was linear over the range of 0.1-60 ng mL(-1). The limit of quantification for finasteride in plasma was 0.1 ng mL(-1). The intra-day and inter-day repeatability (precision) were 2.68-13.87% and 2.14-14.69% respectively. Intra-day and inter-day accuracy were 98-101.57% and 99.7-110%. The assay method has been successfully used to estimate the pharmacokinetics of finasteride after oral administration of a 5 mg tablet of finasteride in 12 healthy volunteers.

Methylmercury determination in biological samples using electrothermal atomic absorption spectrometry after acid leaching extraction.

An efficient and sensitive method for the determination of methylmercury in biological samples was developed based on acid leaching extraction of methylmercury into toluene. Methylmercury in the organic phase was determined by electrothermal atomic absorption spectrometry (ETAAS). The methylmercury signal was enhanced and the reproducibility increased by formation of certain complexes and addition of Pd-DDC modifier. The complex of methylmercury with DDC produced the optimum analytical signal in terms of sensitivity and reproducibility compared to complexes with dithizone, cysteine, 1,10-phenanthroline, and diethyldithiocarbamate. Method performance was optimized by modifying parameters such as temperature of mineralization, atomization, and gas flow rate. The limit of detection for methylmercury determination was 0.015 mug g(-1) and the RSD of the whole procedure was 12% for human teeth samples (n=5) and 15.8% for hair samples (n=5). The method's accuracy was investigated by using NIES-13 and by spiking the samples with different amounts of methylmercury. The results were in good agreement with the certified values and the recoveries were 88-95%.