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Highly sensitive determination of saquinavir in biological samples using liquid chromatography-tandem mass spectrometry

A selective and sensitive method for the determination of the HIV protease inhibitor saquinavir in human plasma, saliva, and urine using liquid-liquid extraction and LC-MS-MS has been developed, validated, and applied to samples of a healthy individual. After extraction with ethyl acetate, sample ex...

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Main Authors: Burhenne, Jürgen (Author) , Riedel, Klaus-Dieter (Author) , Martin-Facklam, Meret (Author) , Mikus, Gerd (Author) , Haefeli, Walter E. (Author)
Format: Article (Journal)
Language:English
Published: 2003
In: Journal of chromatography
Year: 2003, Volume: 784, Issue: 2, Pages: 233-242
ISSN:1873-376X
DOI:10.1016/S1570-0232(02)00803-6
Online Access:Verlag, lizenzpflichtig, Volltext: https://doi.org/10.1016/S1570-0232(02)00803-6
Verlag, lizenzpflichtig, Volltext: https://www.sciencedirect.com/science/article/pii/S1570023202008036
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Author Notes:Jürgen Burhenne, Klaus-Dieter Riedel, Meret Martin-Facklam, Gerd Mikus, Walter E. Haefeli

MARC

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520 |a A selective and sensitive method for the determination of the HIV protease inhibitor saquinavir in human plasma, saliva, and urine using liquid-liquid extraction and LC-MS-MS has been developed, validated, and applied to samples of a healthy individual. After extraction with ethyl acetate, sample extracts were chromatographed isocratically within 5 min on Kromasil RP-18. The drug was detected with tandem mass spectrometry in the selected reaction monitoring mode using an electrospray ion source and 2H5-saquinavir as internal standard. The limit of quantification was 0.05 ng/mL. The accuracy of the method varied between −1 and +10% (SD within-batch) and the precision ranged from +4 to +10% (SD batch-to-batch). The method is linear at least within 0.05 and 87.6 ng/mL. After a regular oral dose (600 mg) saquinavir concentrations were detectable for 48 h in plasma and were well correlated with saliva concentrations (r2=0.9348, mean saliva/plasma ratio 1:15.1). The method is well suited for low saquinavir concentrations in different matrices. 
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