Parallel ultra high pressure liquid chromatography–mass spectrometry for the quantification of HIV protease inhibitors using dried spot sample collection format

Watanabe, Kyoko; Varesio, Emmanuel; Hopfgartner, Gérard

doi:10.1016/j.jchromb.2014.05.008

Cited by 17 publications

(16 citation statements)

References 30 publications

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“…Alternatively, a faster technique is microwave irradiation. In a quantitative assay for 8 HIV protease inhibitors, drying time for 15 µL DBS was reduced to 5 min with 1,200 W irradiation in a commercial microwave (which also contained 100 mL of water) (Watanabe, Varesio, & Hopfgartner, ). Analyte stability was investigated and no degradation occurred during the irradiation/drying process.…”

Section: Blood Collectionmentioning

confidence: 99%

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The use of mass spectrometry to analyze dried blood spots

Wagner

Tonoli

Varesio

et al. 2014

Mass Spectrometry Reviews

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Dried blood spots (DBS) typically consist in the deposition of small volumes of capillary blood onto dedicated paper cards. Comparatively to whole blood or plasma samples, their benefits rely in the fact that sample collection is easier and that logistic aspects related to sample storage and shipment can be relatively limited, respectively, without the need of a refrigerator or dry ice. Originally, this approach has been developed in the sixties to support the analysis of phenylalanine for the detection of phenylketonuria in newborns using bacterial inhibition test. In the nineties tandem mass spectrometry was established as the detection technique for phenylalanine and tyrosine. DBS became rapidly recognized for their clinical value: they were widely implemented in pediatric settings with mass spectrometric detection, and were closely associated to the debut of newborn screening (NBS) programs, as a part of public health policies. Since then, sample collection on paper cards has been explored with various analytical techniques in other areas more or less successfully regarding large‐scale applications. Moreover, in the last 5 years a regain of interest for DBS was observed and originated from the bioanalytical community to support drug development (e.g., PK studies) or therapeutic drug monitoring mainly. Those recent applications were essentially driven by improved sensitivity of triple quadrupole mass spectrometers. This review presents an overall view of all instrumental and methodological developments for DBS analysis with mass spectrometric detection, with and without separation techniques. A general introduction to DBS will describe their advantages and historical aspects of their emergence. A second section will focus on blood collection, with a strong emphasis on specific parameters that can impact quantitative analysis, including chromatographic effects, hematocrit effects, blood effects, and analyte stability. A third part of the review is dedicated to sample preparation and will consider off‐line and on‐line extractions; in particular, instrumental designs that have been developed so far for DBS extraction will be detailed. Flow injection analysis and applications will be discussed in section IV. The application of surface analysis mass spectrometry (DESI, paper spray, DART, APTDCI, MALDI, LDTD‐APCI, and ICP) to DBS is described in section V, while applications based on separation techniques (e.g., liquid or gas chromatography) are presented in section VI. To conclude this review, the current status of DBS analysis is summarized, and future perspectives are provided. © 2014 Wiley Periodicals, Inc. Mass Spec Rev 35:361–438, 2016.

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Section: Blood Collectionmentioning

confidence: 99%

“…The aim was to provide a device that can combine sample collection and sample preparation; extraction is performed with an appropriate solvent in the tube. This device was demonstrated for quantitation of 8 HIV protease inhibitors (Watanabe, Varesio, & Hopfgartner, ).…”

Section: Blood Collectionmentioning

confidence: 99%

The use of mass spectrometry to analyze dried blood spots

Wagner

Tonoli

Varesio

et al. 2014

Mass Spectrometry Reviews

Self Cite

226

228

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“…The most commonly used technique to analyze ARVs in plasma is high‐performance liquid chromatography (HPLC) coupled with ultraviolet (UV), fluorescence or mass spectrometry (MS) detection systems. Several analytical methods have also been reported for quantifying ATV in dried blood spots (DBS) and plasma using HPLC coupled with UV, fluorescence (FL) and tandem mass spectrometry (MS/MS) techniques . The HPLC‐UV‐based method detects plasma concentrations of ATV between 0.09 and 4.38 μg/mL (retention time: 8.3 min, flow rate: 1.8 mL/min), and the HPLC‐FL‐based method detects plasma concentrations of ATV between 0.025 and 10 μg/mL (retention time: 11.8 min, flow rate: 1 mL/min) .…”

Section: Introductionmentioning

confidence: 99%

“…By comparison, MS detection, especially MS/MS, is highly sensitive, selective, and specific . HPLC‐coupled with MS/MS (LC/MS/MS) can detect ATV in DBS between 0.025 and 20 μg/mL (retention time: 3.0 min, flow rate: 0.6 mL/min), and in plasma between 1 and 1000 ng/mL (retention time: 4.96 min, flow rate: 0.35 mL/min) and between 19.53 and 5000 ng/mL (retention time: 2.9 min, flow rate: 0.6 mL/min) . In LC/MS/MS, the separation allows for differentiation between co‐eluting analytes, particularly deuterated internal standards, which eliminates overlapping analyte peak signals and miscalculation of drug levels.…”

Section: Introductionmentioning

confidence: 99%

Development and validation of an assay to analyze atazanavir in human hair via liquid chromatography/tandem mass spectrometry

Phung

Kuncze

Okochi

et al. 2018

Rapid Comm Mass Spectrometry

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Rationale Assays to quantify antiretrovirals in hair samples are increasingly used to monitor adherence and exposure in both HIV prevention and treatment studies. Atazanavir (ATV) is a protease inhibitor used in combination antiretroviral therapy (ART). We developed and validated a liquid chromatography/tandem mass spectrometry (LC/MS/MS)-based method to quantify ATV in human hair, per the NIH Division of AIDS Clinical Pharmacology Quality Assurance (CPQA) program and the FDA bioanalytical method validation guidelines. Methods ATV was extracted from hair using optimized methods and the extracts were injected onto a BDS C-18 column (5 μm, 4.6 × 100 mm), followed by isocratic elution via a mobile phase composed of 55% acetonitrile, 45% water, 0.15% acetic acid, and 4 mM ammonium acetate, at a flow rate of 0.8 mL/min prior to analysis by MS/MS. Levels were quantified using positive electrospray ionization by multiple reaction monitoring (MRM) for the transitions MH+ m/z 705.3 to m/z 168.0 and MH+ m/z 710.2 to m/z 168.0 for ATV and ATV-d5 (internal standard), respectively. Results Our assay demonstrated a linear standard curve (r = 0.99) over the concentration range of 0.0500 ng ATV/mg hair to 20.0 ng/mg hair. The inter- and intraday accuracy of ATV quality control (QC) samples was −1.33 to 4.00% and precision (% coefficient of variation (%CV)) was 1.75 to 6.31%. The %CV for ATV levels in hair samples from highly adherent patients (incurred samples) was less than 10%. No significant endogenous peaks or crosstalk were observed in the specificity test with other HIV drugs. The overall extraction efficiency of ATV from incurred hair samples was greater than 95%. Conclusions This highly sensitive, highly specific and validated assay can be considered for therapeutic drug monitoring for HIV-infected patients on ATV-based ART.

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“…Progresses in LC column technology and in particular the use of sub-2 µm particles result in sharper peaks and increased peak capacity and challenge the acquisition speed of the mass spectrometer in the MRM mode as well as for polarity switching in order to maintain at least twelve data points for accurate and precise quantification. In the present study, we adapted our previously validated dual-column LC-MS assay [3] to a single column assay for the quantification of eight PIs; nelfinavir, amprenavir, indinavir, saquinavir, atazanavir, darunavir, ritonavir and lopinavir in human plasma. The method takes advantage of 1.7 µm core-shell column operating at a flow rate of 0.6 mL/min at a pressure of 650 bar.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous Quantitative Analysis of HIV Protease Inhibitors in Human Plasma Using Core-Shell Column and Fast MRM Detection

et al. 2015

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To support therapeutic drug monitoring (TDM) a quantitative method for eight HIV protease inhibitors (PIs): nelfinavir, amprenavir, indinavir, saquinavir, atazanavir, darunavir, ritonavir and lopinavir in human plasma was developed. Separation of the analytes was achieved using core-shell column for UHPLC separation and mass spectrometric detection in fast multiple reaction monitoring (MRM) mode. Human plasma samples were collected on filter paper in the tube-based dried blood spot device and the analytes were extracted with methanol directly. Core-shell column and fast MRM allowed achieving an analysis time of six minutes. Using a plasma aliquot of 15 µL a dynamic linear range of 25-5000 ng/mL (ritonavir), 25-10000 ng/mL (nelfinavir and amprenavir) and 25-20000 ng/mL (indinavir, saquinavir, atazanavir, darunavir and lopinavir) could be achieved with precision and accuracies better than 15 %.

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Parallel ultra high pressure liquid chromatography–mass spectrometry for the quantification of HIV protease inhibitors using dried spot sample collection format

Cited by 17 publications

References 30 publications

The use of mass spectrometry to analyze dried blood spots

The use of mass spectrometry to analyze dried blood spots

Development and validation of an assay to analyze atazanavir in human hair via liquid chromatography/tandem mass spectrometry

Simultaneous Quantitative Analysis of HIV Protease Inhibitors in Human Plasma Using Core-Shell Column and Fast MRM Detection

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