Liquid chromatographic determination of hyoscine (scopolamine) in urine using solid phase extraction

Abstract

A sensitive method for the determination of hyoscine (scopolamine) in urine is described. After concentration and "clean-up" on C18 and CN solid phase extraction columns, hyoscine was quantified by high performance liquid chromatography with coulometric detection (oxidation at +0.9 V). The limit of detection was 5 ng per sample and the precision for 5 mL samples containing 2 ng/mL was 12.3%. The method was applied to urine samples collected from 12 volunteers wearing Scopoderm TTS patches. The mean excretion rate of unmetabolized hyoscine was 0.45 micrograms/h and 87% of the total hyoscine was present as conjugates. Apohyoscine (aposcopolamine) was identified as a urinary metabolite. The significance of this with regard to hyoscine assays is discussed.

Electrochemical Portable Method for on site Screening of Scopolamine in Beverage and Urine Samples

“…Various methods have been developed for the determination of SCP in pharmaceutical formulations, including high performance liquid chromatography (HPLC) , capillary electrophoresis spectrophotometry , potentiometry and voltammetry . On the other hand, only gas chromatography mass spectrometry (GC‐MS) , liquid chromatography electrospray ionization tandem mass spectrometry (LC‐ESI MS/MS) and radioreceptor assay procedures have been used for the determination of SCP in biological fluids. Many of these instrumental techniques are expensive and demands laborious and time‐consuming procedures, which are not appropriate for simple, rapid and portable screening of beverage and urine samples.…”

Potentiometric PVC Membrane Sensor for the Determination of Scopolamine in Some Pharmaceutical Formulations

“…Among these are high-performance liquid chromatography (HPLC), [3][4][5] capillary zone electrophoresis, 6 proton nuclear-magnetic resonance spectroscopy, 7 gas chromatography mass-spectrometry (GC-MS), 8 micellar electrokinetic chromatography, 9 enzymeimmunoassay, 10 and potentiometry. 11 Most of these methods involve several time-consuming manipulation steps and require sophisticated instruments.…”

Determinação de escopolamina em bebidas e urina empregando voltametria de onda quadrada e eletroforese capilar

“…Robinson sintetizou um produto de oxidação da atropina, a tropinona, através da síntese do sistema de anéis tropânicos (MAIRINK, 2013). A tropinona é um alvo sintético fundamental para numerosos alcaloides tropânicos como, por exemplo, da cocaína, um dos alcaloides com esqueleto tropânico mais conhecidos, tanto pelo seu efeito anestésico como pelo seu uso ilícito CRISOLOGO, 1975;CHEN et al, 2005;LUSTHOF et al, 2017;NIKOLAOU et al, 2012;PUTCHA et al, 1989;WHELPTON et al, 1992).…”

“…A determinação de SCP em amostras de urina, após administração através adesivos cutâneos, foi realizada por HPLC com detecção eletroquímica por Whelpton et al, (1992) O pré-tratamento da amostra consistiu no uso de um método semiautomatizado de extração em fase sólida utilizando colunas de sílica gel com posterior hidrólise da SCP com enzima beta glucunoridase por 10 horas. A elevada especificidade do ensaio radiorececptor possibilitou LDs de 0,00153 µmol L -1 para as amostras de urina e 0,0004 µmol L -1 para as amostras de soro sanguíneo.…”