Validated liquid chromatographic-fluorescence method for the quantitation of darifenacin in mice plasma and its application to a pharmacokinetic study.

A highly selective, sensitive, and rapid high-performance liquid chromatography (HPLC) method has been developed and validated for the quantification of darifenacin in mouse plasma. Bisoprolol was used as an internal standard (IS). Darifenacin and the IS were extracted using the deproteinisation technique, followed by injection of an aliquot of the supernatant into the chromatographic system. The chromatographic separation was achieved on a reversed phase C18 column with a mobile phase of acetonitrile: 0.1% diethyl amine (pH 3.5) (60:40, v/v) pumped at a flow rate of 1.0 mL min(-1). The analytes were detected at 210 and 314 nm for excitation and emission, respectively. The assay exhibited a linear range of 100-3000 ng mL(-1), with a lower detection limit of 35 ng mL(-1). The method was statistically validated for linearity, accuracy, precision, selectivity and stability according to the FDA guidelines. The intra- and inter-assay coefficients of variation did not exceed 13.5% from the nominal concentration. The accuracy for darifenacin was within ±15% of the theoretical value. The assay was successfully applied in a pharmacokinetic study.

PVC membrane sensor for potentiometric determination of iron (II) in some pharmaceutical formulations based on a new neutral ionophore.

A novel poly (vinyl chloride) PVC membrane sensor for Fe(2+) ions is described. The sensor is based on the use of newly synthesized chiral 2,6-bis-(carboxamide methyl ester)pyridine derivative as neutral ionophore in plasticized PVC membrane. The sensor display a fast, stable and near-Nernstian response over a relative wide ferrous concentration range (1 × 10(-3) to 6 × 10(-6) M), with cationic slope of 31.5 ± 0.5, mV per concentration decade over a pH range of 5.0-9.0. The direct determination of 0.25-56.0 µg/ml of ferrous in aqueous solution shows an average recovery of 98.5% and a mean relative standard deviation of 1.5% at 20.0 µg/ml. The sensor displays long life-span, long-term stability, high reproducibility, and short response time. Selectivity coefficients for Fe(II) relative to a number of interfering substances were investigated. The sensor shows high significantly for Fe(2+) over Fe,(3+) Cu,(2+) Zn,(2+) Cd,(2+) Hg,(2+) Pb,(2+) Ni,(2+) Co,(2+) Mn,(2+) Al,(3+) alkaline earth and alkali metal ions. The sensor is successfully applied for measurement of ferrous in drug formulations. The results obtained for the determination of ferrous using the proposed sensor are comparable favourably with those obtained using the spectrophotometric method. Copyright © 2010 John Wiley & Sons, Ltd.

Development and characterization of ion selective electrode for the assay of antimony.

The construction and general performance characteristics of two novel potentiometric carbon paste electrodes (CPE) responsive to antimony are described. These sensors are based on the use of the ion associate complexes of tetraiodoantimonate (TIA) anion with cetylpyridinium (CP) and triphenyl tetrazolium (TPT) counter cations as ion exchange site in a carbon paste matrix. The two sensors exhibits fast, stable and near-Nernstian for the mono charged TIA anion over the concentration range 1x10(-3) to 10(-6)M at 25 degrees C in the pH range 4-10 with anionic slope of 58.0+/-0.5 and 55.0+/-0.7 per concentration decade for TIA-CP and TIA-TPT, respectively. The lower detection limits are 4 and 5x10(-6)M and response time are 20 and 30s in the same order of both electrodes. Selectivity coefficients for antimony relative to a number of different cations and anions were investigated. There is negligible interference from many inorganic cation and anion except for Hg(2+), Cd(2+), and Bi(3+); however, their effect were eliminated by EDTA. The determination of 1.0-120.0mug/ml of antimony in aqueous solutions shows an average recovery of 99.0 and 97.5% with relative standard deviation of 2.0% for both electrodes at 40mug/ml. The determination of antimony in wastewater and some antibilharzial compounds using the proposed electrodes gave results that compare favorably with those obtained by the atomic absorption spectrometric method. Precipitation titrations involving cetylpyridinium chloride as titrant are monitored with both electrodes with inflection point of 180 and 100mV for TIA-CP and TIA-TPT, respectively.

s-Benzylthiuronium PVC matrix membrane sensor for potentiometric determination of cationic surfactants in some pharmaceutical formulation.

The construction and characteristic performance of s-benzylthiuronium (s-BT)-PVC membrane sensor responsive for cetylpyridinium chloride (CPC) are described. The sensor is based on the use of s-BT-tetraphenylborate (TPB) ion pair as electroactive material in PVC matrix in presence of dioctylphthalate as solvent mediator. The membrane sensor shows a fast, stable and near Nernstian response for CPC over the concentration range of 6 x 10(-6)-1 x 10(-3)M at 25 degrees C and pH range 6-12 with cationic slope of 57.0+/-0.4. The lower detection limit is 4 x 0(-6)M and the response time is 10-30 s. Selectivity coefficients for CPC relative to a number of different species were investigated, which there is negligible intereferences are caused by most of investigated cations, anions, and some organic compounds. The determination of 2.0-350.0 microg/ml of CPC in aqueous solutions shows an average recovery of 98.8%and a mean relative standard deviation of 1.87% at 64.0 microg/ml. The determination of CPC in mouthwash pharmaceutical solution gave results that compare favorably with those obtained by the British pharmacopoeia method. The s-benzylthiuronium electrode has been utilized as an end point indicator electrode for some precipitation titration reactions involving CPC as titrant.

PVC matrix membrane sensor for potentiometric determination of metoclopramide hydrochloride in some pharmaceutical formulations.

The construction and characteristic performance of metoclopramide (MCP)-polyvinyl chloride (PVC) membrane sensor are described. The sensor is based on the use of MCP-tetraiodomercurate ion pair as electroactive material in PVC matrix in presence of dioctylphthalate (DOP) as solvent mediator. MCP membrane sensor shows a stable, near Nernstian response over the concentration range 1 x 10(-2)-6 x 10(-5) M of MCP at 25 degrees C in the pH range 3-7 with cationic slope of 53.0+/-0.5. The detection limit of 4 x 10(-5) M and the response time of 30-60 s have been attained. Selectivity coefficient data for some common ions show negligible intereferences. Direct potentiometric determination of 15-3540 microg/ml MCP show an average recovery of 98.5% and a mean relative standard deviation (R.S.D.) of 1.6% at 100.0 microg/ml. The determination of MCP in Primperan tablets, injection, and syrup gave results that compare favorably with those obtained by the British pharmacopoeia method. Precipitation titrations involving MCP as titrant are monitored with the MCP sensor for some potentiometric precipitation reaction, e.g. sodium tetraphenylborate (STPB) and phosphomolybdic acid (PMA).

Gallamine-tetraphenylborate-modified carbon paste electrode for the potentiometric determination of gallamine triethiodide (flaxedil).

The construction and general performance of a novel modified carbon paste electrode for the determination of gallamine triethiodide have been developed. The electrode shows a stable, potentiometric response for gallamine in the concentration range 1 x 10(-3)-2 x 10(-6) M at 25 degrees C independent of pH in the range 5-8. The electrode passes a near-Nernstian cationic slope of 17.0+/-0.7 mV and lower detection limit of 1 x 10(-6) M with a fast response time of 20-45 s. Selectivity coefficients for gallamine relative to a number of interfering substances were investigated. There is a negligible interference from the studied cations, anions, and pharmaceutical excipients. The determination of gallamine in aqueous solution shows an average recovery of 99.5% and a mean relative standard deviation (RSD) of 1.4% at 100 microg/ml. The direct determination of gallamine in injection solution gave results that compare favorably with those obtained by the British pharmacopoeia method. Potentiometric titration of gallamine with sodium tetraphenylborate and phosphotungstic acid as a titrant has been monitored with the modified carbon paste electrode as an end-point indicator electrode.

A novel tetrachlorothallate (III)-PVC membrane sensor for the potentiometric determination of thallium (III).

A novel tetrachlorothallate (III) (TCT)-selective membrane sensor consisting of tetrachlorothallate (III)-2,3,5-triphenyl-2-H-tetrazolium ion pair dispersed in a PVC matrix plasticized with dioctylphthalate is described. The electrode shows a stable, near-Nernstian response for 1x10(-3)-4x10(-6) M thallium (III) at 25 degrees C with an anionic slope of 56.5+/-0.5 over the pH range 3-6. The lower detection limit and the response time are 2x10(-6) M and 30-60 s, respectively. Selectivity coefficients for Tl(III) relative to a number of interfering substances were investigated. There is negligible interference from many cations and anions; however, iodide and bromide are significantly interfere. The determination of 0.5-200 mug ml(-1) of Tl(III) in aqueous solutions shows an average recovery of 99.0% and a mean relative standard deviation of 1.4% at 50.0 mug ml(-1). The direct determination of Tl(III) in spiked wastewater gave results that compare favorably with those obtained by the atomic absorption spectrometric method. The electrode was successfully applied for the determination of thallium in zinc concentrate. Also the tetrachlorothallate electrode has been utilized as an end point indicator electrode for the determination of thallium using potentiometric titration.