Novel spectrofluorimetric method for boldine alkaloid determination in herbal drugs and phytopharmaceuticals.

A new green on-line method for Boldine determination (BOL) in herbal drugs and phytopharmaceuticals, using its native fluorescence in acid media (λex=282nm; λem=373nm) has been developed. The presented methodology involves for the first time, a flow injection (FI) strategy using a mini-column of multiwalled carbon nanotubes as retention agent coupled with molecular fluorescence. Different parameters influence as sample pH and flow rate, eluent flow rate and composition; on BOL sensitivity and elution time was investigated by multifactorial techniques. Adequate dynamic calibration range (r2=0.9993) was obtained over a concentration interval of 0.029-27.0µgmL-1 BOL. The limits of detection (LOD) and quantification (LOQ) were 0.008 and 0.029µgmL-1, respectively. The average recoveries in explored samples ranged from 95% to 103%. Under optimized conditions, the throughput sample as high as 30h-1 was achieved with high repeatability performance (99%). The proposed development represents a useful and valuable tool emulating the analytical efficiency of the official methodologies for quality control of herbal and phytopharmaceutical drugs containing BOL. Moreover, this approach shows advantages respect to low cost, simplicity and environmental and analyst friendly.

A novel application of immobilization on membranes for the separation and spectrofluorimetric quantification of amiloride and furosemide in pharmaceutical samples.

A new, simple and highly sensitive method for spectrofluorimetric determination of amiloride (AMI) and furosemide (FUR) in pharmaceuticals is presented. The proposed method is based on the separation of AMI from FUR by solid-phase extraction using a nylon membrane, followed by spectrofluorimetric determination of both drugs, on the solid surface and the filtered aqueous solution, respectively. AMI shows low native fluorescence, but its separation-preconcentration by immobilization (solid-phase extraction) on nylon membrane surface provides a considerable enhancement in fluorescence intensity. The fluorescence determination is carried out at lambda(ex)=237, lambda(em)=415 nm for FUR; and lambda(ex)=365, lambda(em)=406 nm for AMI. The calibration graphs are linear in the range 3.20 x 10(-4) to 0.8 microg mL(-1) and 1.33 x 10(-3) to 4.0 microg mL(-1), for AMI and FUR, respectively, with a detection limit of 9.62 x 10(-5) and 4.01 x 10(-4) microg mL(-1) (S/N=3). The commonly found excipients in commercial pharmaceutical formulations do not interfere. The developed method is successfully applied to the determination of both drugs in pharmaceutical formulations.

Restless legs syndrome in Parkinson's disease.

We aimed to investigate the prevalence of restless legs syndrome (RLS) according to essential diagnostic criteria, and to explore potential associations with clinical features, especially motor fluctuations, in a cohort of 113 patients with idiopathic Parkinson's disease (PD). Twenty-eight (24%) fulfilled essential diagnostic criteria for RLS. They were younger (63.1 +/- 8.6 vs. 68.8 +/- 9.0 years; P = 0.004), had an earlier onset of PD (54.1 +/- 9.5 vs. 59.2 +/- 10.3 years; P = 0.018), and received lower levodopa equivalent doses (578.4 +/- 382.2 vs. 779.1 +/- 459.6 mg/day; P = 0.04) than patients with PD who scored negative for RLS. In 23 patients (82%), RLS symptom onset was after PD onset (mean interval, 4.5 +/- 3.7 years). The majority (n = 17, 61%) who scored positive for RLS reported that the urge to move the legs and unpleasant sensations were associated with wearing off, raising the possibility of RLS mimics in fluctuating patients with PD.

Video analysis of motor events in REM sleep behavior disorder.

In REM sleep behavior disorder (RBD), several studies focused on electromyographic characterization of motor activity, whereas video analysis has remained more general. The aim of this study was to undertake a detailed and systematic video analysis. Nine polysomnographic records from 5 Parkinson patients with RBD were analyzed and compared with sex- and age-matched controls. Each motor event in the video during REM sleep was classified according to duration, type of movement, and topographical distribution. In RBD, a mean of 54 +/- 23.2 events/10 minutes of REM sleep (total 1392) were identified and visually analyzed. Seventy-five percent of all motor events lasted <2 seconds. Of these events, 1,155 (83.0%) were classified as elementary, 188 (13.5%) as complex behaviors, 50 (3.6%) as violent, and 146 (10.5%) as vocalizations. In the control group, 3.6 +/- 2.3 events/10 minutes (total 264) of predominantly elementary simple character (n = 240, 90.9%) were identified. Number and types of motor events differed significantly between patients and controls (P < 0.05). This study shows a very high number and great variety of motor events during REM sleep in symptomatic RBD. However, most motor events are minor, and violent episodes represent only a small fraction.

Transcranial ultrasound shows nigral hypoechogenicity in restless legs syndrome.

In patients with Parkinson's disease, hyperechogenicity of the substantia nigra using transcranial ultrasound has been related to increased tissue concentrations of iron. Recently, deficient iron transport mechanisms in substantia nigra neurons have been described in postmortem tissue of patients with restless legs syndrome (RLS). This study was performed to study substantia nigra echogenicity in RLS patients compared with normal control subjects and Parkinson's disease patients. RLS patients had significantly reduced midbrain areas of hyperechogenicity compared with control subjects, and even more markedly reduced hyperechogenicity compared with Parkinson's disease patients. These findings lend further support to nigral iron deficiency as a pathogenetic factor in RLS.