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片剂中西酞普兰的柱高效液相色谱法和紫外分光光度法的开发与验证

Development and validation of column high-performance liquid chromatographic and ultraviolet spectrophotometric methods for citalopram in tablets.

作者信息

Menegola Júlia, Steppe Martin, Schapoval Elfrides E S

机构信息

Universidade Federal do Rio Grande do Sul, Faculdade de Farmácia, Programa de Pós-Graduação em Ciências Farmacêuticas, Av. Ipiranga, 2752, Lab. 402 Porto Alegre-RS, CEP 90610-000, Brazil.

出版信息

J AOAC Int. 2008 Jan-Feb;91(1):52-8.

Abstract

Column high-performance liquid chromatographic (LC) and UV spectrophotometric methods for the quantitative determination of citalopram, a potent and selective serotonin reuptake inhibitor, in tablets were developed. The parameters linearity, precision, accuracy, specificity, robustness, limit of detection, and limit of quantitation were studied according to International Conference on Harmonization guidelines. Chromatography was carried out by the reversed-phase technique on an ACE C18 column with a mobile phase composed of 0.30% triethylamine solution-acetonitrile (55 + 45, v/v) adjusted to pH 6.6 with 10% ortho-phosphoric acid at a flow rate of 1.0 mL/min and 25 degrees C. The UV spectrophotometric method was performed at 239 nm. The linearity of the LC method was in the range of 10.00-70.00 microg/mL, and 2.50-17.50 microg/mL for the UV spectrophotometric method. The interday and intraday assay precision was < 1.5% (relative standard deviation) for the LC and UV spectrophotometric methods. The recoveries were in the range 100.70-101.35% for the LC method and 98.48-98.65% for the UV spectrophotometric method. Statistical analysis by Student's t-test showed no significant difference between the results obtained by the 2 methods. The proposed methods are highly sensitive, precise, and accurate and can be used for the reliable quantitation of citalopram in tablets.

摘要

建立了柱高效液相色谱(LC)和紫外分光光度法,用于定量测定片剂中强效选择性5-羟色胺再摄取抑制剂西酞普兰。根据国际协调会议指南研究了线性、精密度、准确度、特异性、稳健性、检测限和定量限等参数。采用反相技术在ACE C18柱上进行色谱分析,流动相由0.30%三乙胺溶液-乙腈(55 + 45,v/v)组成,用10%正磷酸调至pH 6.6,流速为1.0 mL/min,柱温25℃。紫外分光光度法在239 nm处进行。LC法的线性范围为10.00 - 70.00 μg/mL,紫外分光光度法为2.50 - 17.50 μg/mL。LC法和紫外分光光度法的日间和日内测定精密度均<1.5%(相对标准偏差)。LC法的回收率在100.70 - 101.35%范围内,紫外分光光度法为98.48 - 98.65%。通过学生t检验的统计分析表明,两种方法所得结果之间无显著差异。所提出的方法具有高灵敏度、精密度和准确度,可用于可靠地定量片剂中的西酞普兰。

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