Analysis of risperidone and its metabolite in plasma and saliva by LC with coulometric detection and a novel MEPS procedure

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• 作者：Maria Addolorata Saracino ; Anna de Palma ; Giancarlo Boncompagni ; Maria Augusta Raggi
• 关键词：Risperidone ; 9-Hydroxyrisperidone ; Liquid chromatography ; Microextraction by packed sorbent ; Saliva ; Plasma
• 刊名：Talanta
• 出版年：2010
• 出版时间：15 June 2010
• 年：2010
• 卷：81
• 期：4-5
• 页码：1547-1553
• 全文大小：546 K

文摘

A new analytical method, based on the use of liquid chromatography with coulometric detection, has been developed and applied to quantify risperidone and its main active metabolite 9-hydroxyrisperidone in human plasma and saliva. The analytes were separated on a reversed phase C18 column, using a mobile phase composed of acetonitrile (26 % ) and a pH 6.5 phosphate buffer (74 % ). Pipamperone was used as the internal standard. A high sensitivity coulometric detection analytical cell containing two flow-through working electrodes was used: electrode 1 was set at +0.500 V and electrode 2 at +0.700 V. The detector response was linear over a plasma and saliva concentration range of 0.5–50.0 ng mL⁻¹ for risperidone and 0.5–100.0 ng mL⁻¹ for 9-hydroxyrisperidone. The limit of quantitation and the limit of detection for risperidone and 9-hydroxyrisperidone were 0.5 ng mL⁻¹ and 0.17 ng mL⁻¹, respectively. A novel clean-up procedure of biological samples was developed using the microextraction by packed sorbent technique, which gave good extraction yield for both the analytes, with absolute recovery values higher than 90.1 % . The intra-day and the inter-day precision results, expressed by relative standard deviation values, were lower than 5.8 % . Accuracy and selectivity assays were also satisfactory. The validated method has been successfully applied to the analysis of risperidone and 9-hydroxyrisperidone in plasma and saliva of psychiatric patients undergoing therapy with risperidone.