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采用高效液相色谱串联质谱法测定人血浆中阿莫曲坦的方法开发与验证:应用于药代动力学研究

Method development and validation of almotriptan in human plasma by HPLC tandem mass spectrometry: application to pharmacokinetic study.

作者信息

Ravikumar Konda, Chandu Babu Rao, Challa Balasekhara Reddy, Chandrasekhar Kottapalli B

机构信息

Hindu college of Pharmacy, Amaravathi Road, Guntur, Andhrapradesh, 522002, India.

出版信息

Sci Pharm. 2012 Apr-Jun;80(2):367-78. doi: 10.3797/scipharm.1112-01. Epub 2012 Feb 27.

Abstract

A simple, sensitive and selective method has been developed for quantification of Almotriptan (AL) in human plasma using Almotriptan-d(6) (ALD6) as an internal standard. Almotriptan and Almotriptan-d(6) were detected with proton adducts at m/z 336.1→201.1 and 342.2→207.2 in multiple reaction monitoring (MRM) positive mode, respectively. The method was linear over a concentration range of 0.5-150.0 ng/mL. The limit of detection (LOD) and limit of quantification (LOQ) for Almotriptan were 0.2 pg/mL and 0.5 ng/mL, respectively. Liquid-liquid extraction was used followed by MS/MS (ion spray). The method was shown to be precise with an average within-run and between-run variation of 0.68 to 2.78% and 0.57 to 0.86%, respectively. The average within-run and between-run accuracy of the method throughout its linear range was 98.94 to 102.64% and 99.43 to 101.44%, respectively. The mean recovery of drug and internal standard from human plasma was 92.12 ± 4.32% and 89.62 ± 6.32%. It can be applied for clinical and pharmacokinetic studies.

摘要

已开发出一种简单、灵敏且具选择性的方法,以Almotriptan-d(6)(ALD6)作为内标物,用于定量测定人血浆中的阿莫曲坦(AL)。在多反应监测(MRM)正模式下,分别以质荷比m/z 336.1→201.1和342.2→207.2的质子加合物检测到阿莫曲坦和Almotriptan-d(6)。该方法在0.5 - 150.0 ng/mL的浓度范围内呈线性。阿莫曲坦的检测限(LOD)和定量限(LOQ)分别为0.2 pg/mL和0.5 ng/mL。采用液 - 液萃取,随后进行MS/MS(离子喷雾)。该方法显示出良好的精密度,批内平均变异和批间平均变异分别为0.68%至2.78%和0.57%至0.86%。在整个线性范围内,该方法的批内平均准确度和批间平均准确度分别为98.94%至102.64%和99.43%至101.44%。药物和内标物从人血浆中的平均回收率分别为92.12 ± 4.32%和89.62 ± 6.32%。该方法可应用于临床和药代动力学研究。

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