Determination of Tetracyclines in Milk,Eggs and Honey Using in-situ Ionic Liquid Based Dispersive Liquid–Liquid Microextraction

In this study, in-situ ionic liquid based dispersive liquid?liquid microextraction method for enrichment of tetracyclines before liquid chromatographic analysis has been improved. A 1-benzyl-3- methylimidazolium chloride was used as an ionic liquid. To increase extraction efficiency, some optimization parameters (amount of ammonium hexafluorophoshate, extraction time, centrifugation time, ratio of ionic liquid/salt) were investigated. At optimized conditions, enrichment factors of four tetracycline antibiotics (tetracycline, chlortetracycline, methacycline, doxycycline) were between 25 and 98. The residues of tetracyclines were not found in the studied real samples. For the accuracy of the method, the concentration of 50 and 250 μg/L of standard tetracycline mixture solutions were spiked to the blank real milk, honey and egg samples and the percentage recoveries were obtained in the range of 75.8–109.7%.     

Densitometric HPTLC Analysis of the 5-Hydroxymethylfurfural Content of Turkish Fruit Wines and Vinegars

JPC – Journal of Planar Chromatography – Modern TLC - A thin-layer chromatographic method with densitometric UV detection at 286 nm after ethyl acetate extraction is described for...     

Preconcentration of uranium(VI) and thorium(IV) from aqueous solutions using low-cost abundantly available sorbent

Olive cake as low-cost abundantly available sorbent has been characterized by N₂ at 77 K adsorption, porosity analysis, elemental analysis and IR spectra and has been used for preconcentrating of uranium(VI) and thorium(IV) ions prior to their determination spectrophotometrically. The optimum pH values for quantitative sorption of U(VI) and Th(IV) are 4–7 and 3–7, respectively. The enrichment factor for the preconcentration of U(VI) and Th(IV) were found to be 125 and 75 in the given order. The sorption capacity of olive cake is in the range of 2,260–15,000 μg g⁻¹ for Th(IV) and in the range of 1,090–17,000 μg g⁻¹ for U(VI) at pH 3–7. The sorbent exhibits good reusability and the uptake and stripping of the studied ions were fairly rapid. The elution of U(VI) and Th(IV) was performed with 0.3–1 M HCl/1–2 M HNO₃ and 0.3–0.8 M HCl/1 M HNO₃, respectively. The precision of the method was 1.8 RSD% for U(VI) and 2.5 RSD% for Th(IV) in a concentration of 1.00 μg mL⁻¹ for 10 replicate analysis. The influence of some electrolytes and cations as interferents was discussed. Separation of U(VI) and Th(IV) from other metal ions in synthetic solution was achieved.     

A fluorescent chemical sensor for ethanol determination in alcoholic beverages

A sensor for ethanol is described that is based on the fluorescent probe 5,10,15,20-tetraphenyl porphyrin (TPP). Response is based on the quenching of the fluorescence of TPP by ethanol as a result of electrostatic attraction. The sensor linearly responds to ethanol in the concentration range from 1 to 75 vol.% and was applied to the determination of ethanol in various kinds of wines and whisky.     

Use of ionic liquid based chitosan as sorbent for preconcentration of fluoroquinolones in milk,egg, fish,bovine, and chicken meat samples by solid phase extraction prior to HPLC determination

The possibility of using ionic liquid based chitosan sorbent for the separation and preconcentration of fluoroquinolone antibiotics (marbofloxacin, enoxacin, ofloxacin, ciprofloxacin, and enrofloxacin) has been studied. For this reason, different ionic liquids were prepared and coated on the chitosan sorbent. The conditions of the preconcentration of fluoroquinolones on a microcolumn have been optimized and the extraction efficiencies of the prepared sorbents have been compared. The compounds were eluted with 5 mL of 20% NH₃ (v/v, MeOH) solution and determined by HPLC with diode array and fluorescence detector. The limits of detection were found as 4.23 µ g L^?1 for marbofloxacin, and 1.09 µg L^?1 for enoxacin; 3.23 × 10^?3 µg L^?1 for ofloxacin; 8.39 × 10^?3 µg L^?1 for ciprofloxacin; and 19.50 × 10^?3 µg L^?1 for enrofloxacin. The developed method was applied for the analysis of fluoroquinolone in milk, egg, fish, bovine, and chicken samples and the recoveries were obtained in the range 70–100%.     

Thermal behaviour of some metal complexes of N,N-diethyl-N′-benzoyl thiourea

The thermal behaviour of the complexes of N,N-diethyl-N-benzoylthiourea (DEBT) with Ni(II), Cu(II), Pt(II), Pd(II) and Ru(III) was studied using differential thermal analysis (DTA) and thermogravimetry (TG). These complexes undergo only a pyrolytic decomposition process. A gas chromatography-mass spectrometry combined system was used for the verification of the first decomposition product and X-ray diffraction method for the characterization of the final products of pyrolysis.This work was partially supported by Erciyes University Fund Project (AFP 94).     

Extraction of some transition metals with N,N-dibutyl-N'-benzoylthiourea into molten paraffin at 65 degrees C

The solid-liquid extraction behaviour of some transition metals (Cu(II), Co(II), Ni(II), Cd(II) and Pb(II)) by the use of N,N-dibutyl-N'-benzoylthiourea as an extractant in paraffin (58-60 degrees C) has been investigated at 65.0+/-0.5 degrees C. The effect of equilibration time, pH of the aqueous phase, concentration of extractant and solid solvent used on the extraction efficiency of these metals have been discussed. The interferences of various ions are examined. The method has been applied to the determination of these metals in synthetic samples, mushrooms and sediment.     

<Emphasis Type="Italic">p</Emphasis>-<Emphasis Type="Italic">tert</Emphasis>-Butylcalix[8]arene loaded silica gel for preconcentration of uranium(VI) via solid phase extraction

This paper reports silica gel loaded with p-tert-butylcalix[8]arene as a new solid phase extractor for determination of trace level of uranium. Effective extraction conditions were optimized in column methods prior to determination by spectrophotometry using arsenazo(III). The results showed that U(VI) ions can be sorbed at pH 6 in a mini-column and quantitative recovery of U(VI) (>95–98%) was achieved by stripping 0.4 mol L⁻¹ HCl. The sorption capacity of the functionalized sorbent is 0.072 mmol uranium(VI) g⁻¹ modified silica gel. The relative standard deviation and detection limit were 1.2% (n = 10) for 1 μg uranium(VI) mL⁻¹ solution and 0.038 μg L⁻¹, respectively. The method was employed to the preconcentration of U(VI) ions from spiked ground water samples.     

Polymer supported 5,10,15,20-tetrakis(phenoxy acetic acid)porphyrin derivative for separation and preconcentration of d- and f-electron metals

5,10,15,20-tetrakis(phenoxy acetic acid) porphyrin (PAAP) was covalently linked to Merrifield chloromethylated resin. Characterization of PAAP and the modified polymeric matrix were performed by ¹H NMR, FTIR and elemental analysis. The sorbent was used for the separation and enrichment of the d-electron metals (Mn(II), Co(II), Ni(II), Cu(II) and Zn(II)) at pH 6–8 and of the f-electron metals U(VI) and Th(IV) at pH 4–5. The metals ions were preconcentrated with a concentration factor range of 115–215 and then determined by flame atomic absorption spectrometry or visible spectrophotometry using Arsenazo(III). The retained metals were eluted with 2.0 mol L⁻¹ HNO₃ in the case of the d-electron metals and 0.1/0.25 mol L⁻¹ HCl in the case of the f-electron metals. The procedure was validated by analyzing the NIST standard reference material 2709 (San Joaquin Soil). Correspondence: Melek Merdivan, Chemistry Department, Faculty of Arts and Sciences, Dokuz Eylul University, 35160 Buca, Izmir, Turkey     

Sorption behaviour of uranium(VI) with N,N-dibutyl-N'-benzoylthiourea Impregnated in Amberlite XAD-16

The sorption of U(VI) by N, N-dibutyl, N'-benzoylthiourea (DBBT) impregnated resin has been studied. DBBT impregnated resin was prepared by direct adsorption of chelating ligand onto macroporous support, Amberlite XAD-16. The adsorption of DBBT on the macroporous support is shown by FTIR spectroscopy to be the result of only weak chelating ligand-support interactions. Parameters such as the pH effect on the sorption of uranium, the sorption capacity of the impregnated resin, the stripping of uranium and the effect of coexisting ions were investigated by batch experiments. The results demonstrated that uranium(VI) ions, at pH 4.5-7 could be sorbed completely using 0.1 g Amberlite XAD-16 resin loaded with DBBT. The sorption capacity of the impregnated resin is 0.90 mmol uranium(VI) g(-1). Quantitative recovery of U(VI) is achieved by stripping with 0.1 M HNO(3). The method was applied to the determination of uranium in synthetic samples. The precision of the method was 2.4 RSD% in a concentration of 1.20 mug ml(-1) for ten replicate analysis.