Flow injection chemiluminescence determination of acetochlor and cartap-HCl in freshwater samples using an acidic KMnO4 -rhodamine-B reaction system.

A flow injection (FI) methodology using the acidic potassium permanganate (KMnO4 )-rhodamine-B (Rh-B) reaction with chemiluminescence (CL) detection was established to determine acetochlor and cartap-HCl pesticides in freshwater samples. Experimental parameters were optimized, and Chelex-100 cationic exchanger mini column and solid-phase extraction (SPE) were used as phase separation techniques. Linear calibration curves were observed for the standard solutions of acetochlor and cartap-HCl over the ranges 0.005-2.0 mg L-1 [y = 1155.8x + 57.551, R2  = 0.9999 (n = 8)] and 0.005-1.0 mg L-1 [y = 979.76x + 14.491, R2  = 0.9998 (n = 8)] with LODs and LOQs of 7.5 × 10-4 and 8.0 × 10-4  mg L-1 (3σ blank) and 2.5 × 10-3 and 2.7 × 10-3  mg L-1 (10σ blank), respectively, with an injection throughput of 140 h-1 . These methods were used to estimate acetochlor and cartap-HCl with or without the SPE procedure, respectively, in spiked freshwater samples. Results obtained were not significantly different at a 95% confidence level to those of other reported methods. Recoveries for acetochlor and cartap-HCl were obtained over the ranges 93-112% (RSD = 1.9-3.6%) and 98-109% (RSD = 1.7-3.8%), respectively. The most probable CL reaction mechanism was explored.

Determination of pioglitazone hydrochloride by flow injection chemiluminescence tris(2,2'-bipyridyl)ruthenium(II)-silver(III) complex system.

A novel flow injection-chemiluminescence (FI-CL) approach is proposed for the assay of pioglitazone hydrochloride (PG-HCl) based on its enhancing influence on the tris(2,2'-bipyridyl)ruthenium(II)-silver(III) complex (Ru(bipy)3 2+ -DPA) CL system in sulfuric acid medium. The possible CL reaction mechanism is discussed with CL and ultraviolet (UV) spectra. The optimum experimental conditions were found as: Ru(bipy)3 2+ , 5.0 × 10-5  M; sulfuric acid, 1.0 × 10-3  M; diperiodatoargentate(III) (DPA), 1.0 × 10-4  M; potassium hydroxide, 1.0 × 10-3  M; flow rate 4.0 ml min-1 for each flow stream and sample loop volume, 180 µl. The CL intensity of PG-HCl was linear in the range of 1.0 × 10-3 to 5.0 mg L-1 (R2 = 0.9998, n = 10) with limit of detection [LOD, signal-to-noise ratio (S/N) = 3] of 2.2 × 10-4  mg L-1 , limit of quantification (LOQ, S/N = 10) of 6.7 × 10-4  mg L-1 , relative standard deviation (RSD) of 1.0 to 3.3% and sampling rate of 106 h-1 . The methodology was satisfactorily used to quantify PG-HCl in pharmaceutical tablets with recoveries ranging from 93.17 to 102.77 and RSD from 1.9 to 2.8%.

Daily Dose Standardization Based on Essential and Nonessential Trace Element Presence in Berberis baluchistanica Ahrendt Bark, Leaf, and Root.

Medicinal plants have great importance to the consumer health, as beside beneficial compounds, plants can accumulate essential and nonessential metals from soil and surrounding environments, leading to consumer health risks. Assuming this, the present study is aimed at evaluating the elemental composition and daily dose standardization based on essential and nonessential trace element presence in of bark, leaves, and roots of Berberis baluchistanica Ahrendt, a common medicinal plant used as a folk medicine in the region. Atomic absorption and flame emission spectroscopy were performed to analyze the presence of essential and nonessential elements manganese (Mn), copper (Cu), lead (Pb), nickel (Ni), iron (Fe), sodium (Na), and potassium (K). Among the essential elements, K was present at high concentrations in the bark (8926.98 ± 0.32 µg/g), leaves (7922.77 ± 0.42 µg/g), and roots (6668.5 ± 0.96 µg/g) of the plant. The estimated concentration of Na was higher in leaves (1782.56 ± 0.13 µg/g), followed by roots (1089.5 ± 0.71 µg/g) and bark (572.8 ± 0.62 µg/g). The Fe concentration varied in the range of 394.7 ± 0.3 µg/g in bark, 1298.3 ± 0.54 µg/g in leaves, and 1208.9 ± 0.7 µg/g in roots. The trace transition element Mn was highest in leaves (42.7 ± 0.99 µg/g), followed by roots (33.5 ± 0.94 µg/g) and bark (22 ± 1 µg/g). The Cu concentration was low, ranging from 20.1 ± 0.63 to 22.67 ± 0.7 µg/g in leaves, bark, and roots. The obtained concentration of nonessential element Pb was relatively lower than the permissible range (10 mgL-1) established by the World Health Organization. The elemental concentrations in all parts were within the set limits for provisional tolerable daily maximum intake (PTDMI) and provisional tolerable weekly intake (PTWI), and the hazard quotient index (HQ) was below 1 for all toxic metals. The micro and macroelemental distribution and the overall medicinal potential of any medicinal plant can be correlated for dose risk estimation, which will be useful in providing knowledge regarding the contraindication associated with folk medicines. In the present study, based on the elemental composition, it was calculated that the daily safe dose for Berberis baluchistanica is approximately 2-5 g/day of raw powder for an adult, which must not be exceeded to this safe range.